# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_NiC4DCsty
_database_code_depnum_ccdc_archive 'CCDC 1524563'
_audit_update_record             
;
2016-12-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 N2 Ni O5'
_chemical_formula_sum            'C32 H32 N2 Ni O5'
_chemical_formula_weight         583.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0021 0.0012 '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 0.0044 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0047 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3389 0.8999 '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                   18.788(4)
_cell_length_b                   8.4300(17)
_cell_length_c                   18.868(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.53(3)
_cell_angle_gamma                90
_cell_volume                     2696.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    67052
_cell_measurement_theta_min      1.797
_cell_measurement_theta_max      33.355

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.630
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40553
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.797
_diffrn_reflns_theta_max         33.355
_diffrn_reflns_theta_full        22.210
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12624
_reflns_number_gt                8878
_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       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.0632P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12624
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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 0.33660(2) 0.73173(2) 0.28373(2) 0.00625(4) Uani 1 1 d . . . . .
O1 O 0.35984(6) 0.96933(11) 0.28848(5) 0.01088(16) Uani 1 1 d . . . . .
H1 H 0.3297(15) 1.044(3) 0.2948(14) 0.056(8) Uiso 1 1 d . . . . .
H2 H 0.4104(16) 0.983(3) 0.3240(15) 0.056(8) Uiso 1 1 d . . . . .
O2 O 0.30996(5) 0.49260(10) 0.26961(5) 0.01079(16) Uani 1 1 d . . . . .
O3 O 0.28308(5) 0.24663(10) 0.29043(5) 0.00863(15) Uani 1 1 d . . . . .
O4 O 0.54313(5) 0.30176(11) 0.64478(5) 0.01229(17) Uani 1 1 d . . . . .
O5 O 0.48887(6) 0.05977(13) 0.62636(7) 0.0221(2) Uani 1 1 d . . . . .
C1 C 0.32982(7) 0.36348(13) 0.30480(6) 0.00717(18) Uani 1 1 d . . . . .
C2 C 0.41350(7) 0.33515(16) 0.36499(7) 0.0123(2) Uani 1 1 d . . . . .
H2A H 0.4411 0.4385 0.3793 0.015 Uiso 1 1 calc R U . . .
H2B H 0.4408 0.2697 0.3407 0.015 Uiso 1 1 calc R U . . .
C3 C 0.42099(8) 0.25229(15) 0.44071(7) 0.0139(2) Uani 1 1 d . . . . .
H3A H 0.3847 0.1603 0.4266 0.017 Uiso 1 1 calc R U . . .
H3B H 0.4755 0.2119 0.4698 0.017 Uiso 1 1 calc R U . . .
C4 C 0.40184(8) 0.36362(16) 0.49369(8) 0.0164(2) Uani 1 1 d . . . . .
H4A H 0.3484 0.4082 0.4637 0.020 Uiso 1 1 calc R U . . .
H4B H 0.4398 0.4529 0.5098 0.020 Uiso 1 1 calc R U . . .
C5 C 0.40517(8) 0.28028(18) 0.56741(8) 0.0161(2) Uani 1 1 d . . . . .
H5A H 0.3926 0.3581 0.5997 0.019 Uiso 1 1 calc R U . . .
H5B H 0.3645 0.1961 0.5514 0.019 Uiso 1 1 calc R U . . .
C6 C 0.48505(7) 0.20731(16) 0.61674(7) 0.0123(2) Uani 1 1 d . . . . .
N1 N 0.35506(6) 0.71786(12) 0.18168(6) 0.00918(17) Uani 1 1 d . . . . .
C7 C 0.41709(8) 0.78479(16) 0.17565(7) 0.0130(2) Uani 1 1 d . . . . .
H7 H 0.4524 0.8471 0.2182 0.016 Uiso 1 1 calc R U . . .
C8 C 0.30496(8) 0.63326(16) 0.12029(7) 0.0130(2) Uani 1 1 d . . . . .
H8 H 0.2605 0.5861 0.1234 0.016 Uiso 1 1 calc R U . . .
C9 C 0.43194(8) 0.76713(17) 0.11028(7) 0.0144(2) Uani 1 1 d . . . . .
H9 H 0.4767 0.8164 0.1087 0.017 Uiso 1 1 calc R U . . .
C10 C 0.31533(8) 0.61169(17) 0.05254(8) 0.0153(2) Uani 1 1 d . . . . .
H10 H 0.2777 0.5526 0.0100 0.018 Uiso 1 1 calc R U . . .
C11 C 0.38097(7) 0.67674(16) 0.04669(7) 0.0122(2) Uani 1 1 d . . . . .
C12 C 0.39284(8) 0.64424(17) -0.02355(7) 0.0154(2) Uani 1 1 d . . . . .
H12 H 0.3503 0.5957 -0.0663 0.018 Uiso 1 1 calc R U . . .
C13 C 0.45769(8) 0.67607(17) -0.03359(7) 0.0152(2) Uani 1 1 d . . . . .
H13 H 0.5004 0.7253 0.0088 0.018 Uiso 1 1 calc R U . . .
C14 C 0.46837(8) 0.64128(16) -0.10451(7) 0.0145(2) Uani 1 1 d . . . . .
C15 C 0.53596(9) 0.6949(2) -0.11008(8) 0.0215(3) Uani 1 1 d . . . . .
H15 H 0.5746 0.7524 -0.0676 0.026 Uiso 1 1 calc R U . . .
C16 C 0.41360(9) 0.55375(18) -0.16726(8) 0.0185(3) Uani 1 1 d . . . . .
H16 H 0.3677 0.5136 -0.1644 0.022 Uiso 1 1 calc R U . . .
C17 C 0.54787(9) 0.6654(2) -0.17706(9) 0.0247(3) Uani 1 1 d . . . . .
H17 H 0.5939 0.7043 -0.1802 0.030 Uiso 1 1 calc R U . . .
C18 C 0.42556(10) 0.5249(2) -0.23369(9) 0.0234(3) Uani 1 1 d . . . . .
H18 H 0.3874 0.4668 -0.2762 0.028 Uiso 1 1 calc R U . . .
C19 C 0.49290(10) 0.5801(2) -0.23854(9) 0.0227(3) Uani 1 1 d . . . . .
H19 H 0.5010 0.5592 -0.2840 0.027 Uiso 1 1 calc R U . . .
N2 N 0.31212(6) 0.73238(12) 0.38288(6) 0.00937(17) Uani 1 1 d . . . . .
C20 C 0.25127(7) 0.64682(15) 0.38214(7) 0.0112(2) Uani 1 1 d . . . . .
H20 H 0.2186 0.5922 0.3353 0.013 Uiso 1 1 calc R U . . .
C21 C 0.35700(7) 0.80901(15) 0.44947(7) 0.0112(2) Uani 1 1 d . . . . .
H21 H 0.4000 0.8705 0.4509 0.013 Uiso 1 1 calc R U . . .
C22 C 0.23406(7) 0.63453(15) 0.44619(7) 0.0119(2) Uani 1 1 d . . . . .
H22 H 0.1905 0.5722 0.4427 0.014 Uiso 1 1 calc R U . . .
C23 C 0.34398(8) 0.80319(15) 0.51674(7) 0.0124(2) Uani 1 1 d . . . . .
H23 H 0.3777 0.8593 0.5626 0.015 Uiso 1 1 calc R U . . .
C24 C 0.28074(8) 0.71388(15) 0.51624(7) 0.0114(2) Uani 1 1 d . . . . .
C25 C 0.26535(8) 0.70910(16) 0.58617(7) 0.0140(2) Uani 1 1 d . . . . .
H25 H 0.2990 0.7696 0.6304 0.017 Uiso 1 1 calc R U . . .
C26 C 0.20761(8) 0.62623(16) 0.59248(7) 0.0140(2) Uani 1 1 d . . . . .
H26 H 0.1751 0.5645 0.5482 0.017 Uiso 1 1 calc R U . . .
C27 C 0.18899(8) 0.62033(16) 0.66063(7) 0.0136(2) Uani 1 1 d . . . . .
C28 C 0.12931(9) 0.51716(17) 0.65768(8) 0.0169(2) Uani 1 1 d . . . . .
H28 H 0.1020 0.4547 0.6120 0.020 Uiso 1 1 calc R U . . .
C29 C 0.22750(9) 0.71312(18) 0.72771(8) 0.0187(3) Uani 1 1 d . . . . .
H29 H 0.2674 0.7854 0.7305 0.022 Uiso 1 1 calc R U . . .
C30 C 0.10923(9) 0.50444(18) 0.72066(9) 0.0192(3) Uani 1 1 d . . . . .
H30 H 0.0689 0.4334 0.7179 0.023 Uiso 1 1 calc R U . . .
C31 C 0.20776(10) 0.7003(2) 0.79058(8) 0.0221(3) Uani 1 1 d . . . . .
H31 H 0.2348 0.7630 0.8363 0.027 Uiso 1 1 calc R U . . .
C32 C 0.14855(9) 0.59620(19) 0.78713(8) 0.0205(3) Uani 1 1 d . . . . .
H32 H 0.1353 0.5883 0.8302 0.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0438(10) . ?
Ni1 O2 2.0664(10) . ?
Ni1 O3 2.0779(12) 2 ?
Ni1 O4 2.0923(12) 3_666 ?
Ni1 N1 2.1017(11) . ?
Ni1 N2 2.1103(11) . ?
O1 H1 0.89(3) . ?
O1 H2 0.90(3) . ?
O2 C1 1.2455(14) . ?
O3 C1 1.2687(14) . ?
O3 Ni1 2.0779(12) 2_545 ?
O4 C6 1.2677(16) . ?
O4 Ni1 2.0923(12) 3_666 ?
O5 C6 1.2545(17) . ?
C1 C2 1.5099(18) . ?
C2 C3 1.5413(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.5230(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.5352(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5143(19) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N1 C8 1.3403(16) . ?
N1 C7 1.3431(16) . ?
C7 C9 1.3849(17) . ?
C7 H7 0.9500 . ?
C8 C10 1.3854(17) . ?
C8 H8 0.9500 . ?
C9 C11 1.3952(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.3969(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.4615(17) . ?
C12 C13 1.3384(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.4657(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.3939(19) . ?
C14 C16 1.398(2) . ?
C15 C17 1.397(2) . ?
C15 H15 0.9500 . ?
C16 C18 1.3870(19) . ?
C16 H16 0.9500 . ?
C17 C19 1.377(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
N2 C21 1.3393(16) . ?
N2 C20 1.3467(16) . ?
C20 C22 1.3831(17) . ?
C20 H20 0.9500 . ?
C21 C23 1.3931(17) . ?
C21 H21 0.9500 . ?
C22 C24 1.4016(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.4032(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.4679(17) . ?
C25 C26 1.3380(18) . ?
C25 H25 0.9500 . ?
C26 C27 1.4718(17) . ?
C26 H26 0.9500 . ?
C27 C29 1.3957(19) . ?
C27 C28 1.4010(19) . ?
C28 C30 1.3973(19) . ?
C28 H28 0.9500 . ?
C29 C31 1.3913(19) . ?
C29 H29 0.9500 . ?
C30 C32 1.385(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.396(2) . ?
C31 H31 0.9500 . ?
C32 H32 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
O1 Ni1 O2 175.57(4) . . ?
O1 Ni1 O3 96.83(4) . 2 ?
O2 Ni1 O3 80.82(4) . 2 ?
O1 Ni1 O4 87.31(4) . 3_666 ?
O2 Ni1 O4 94.92(4) . 3_666 ?
O3 Ni1 O4 175.44(4) 2 3_666 ?
O1 Ni1 N1 88.75(4) . . ?
O2 Ni1 N1 87.37(4) . . ?
O3 Ni1 N1 86.81(5) 2 . ?
O4 Ni1 N1 91.40(5) 3_666 . ?
O1 Ni1 N2 94.74(4) . . ?
O2 Ni1 N2 89.06(4) . . ?
O3 Ni1 N2 90.62(5) 2 . ?
O4 Ni1 N2 90.93(5) 3_666 . ?
N1 Ni1 N2 175.89(4) . . ?
Ni1 O1 H1 124.3(17) . . ?
Ni1 O1 H2 107.1(17) . . ?
H1 O1 H2 110(2) . . ?
C1 O2 Ni1 141.59(8) . . ?
C1 O3 Ni1 129.74(8) . 2_545 ?
C6 O4 Ni1 132.88(9) . 3_666 ?
O2 C1 O3 122.95(11) . . ?
O2 C1 C2 120.98(11) . . ?
O3 C1 C2 116.00(10) . . ?
C1 C2 C3 114.73(10) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 C2 112.09(11) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 112.56(11) . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 112.67(11) . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
O5 C6 O4 125.24(12) . . ?
O5 C6 C5 118.13(12) . . ?
O4 C6 C5 116.63(12) . . ?
C8 N1 C7 117.53(11) . . ?
C8 N1 Ni1 119.32(8) . . ?
C7 N1 Ni1 123.10(9) . . ?
N1 C7 C9 123.05(12) . . ?
N1 C7 H7 118.5 . . ?
C9 C7 H7 118.5 . . ?
N1 C8 C10 122.79(12) . . ?
N1 C8 H8 118.6 . . ?
C10 C8 H8 118.6 . . ?
C7 C9 C11 119.84(12) . . ?
C7 C9 H9 120.1 . . ?
C11 C9 H9 120.1 . . ?
C8 C10 C11 120.09(12) . . ?
C8 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C11 C10 116.65(11) . . ?
C9 C11 C12 124.46(12) . . ?
C10 C11 C12 118.88(12) . . ?
C13 C12 C11 126.49(13) . . ?
C13 C12 H12 116.8 . . ?
C11 C12 H12 116.8 . . ?
C12 C13 C14 125.47(13) . . ?
C12 C13 H13 117.3 . . ?
C14 C13 H13 117.3 . . ?
C15 C14 C16 117.98(12) . . ?
C15 C14 C13 119.45(13) . . ?
C16 C14 C13 122.56(12) . . ?
C14 C15 C17 121.11(14) . . ?
C14 C15 H15 119.4 . . ?
C17 C15 H15 119.4 . . ?
C18 C16 C14 120.73(13) . . ?
C18 C16 H16 119.6 . . ?
C14 C16 H16 119.6 . . ?
C19 C17 C15 120.02(14) . . ?
C19 C17 H17 120.0 . . ?
C15 C17 H17 120.0 . . ?
C16 C18 C19 120.54(14) . . ?
C16 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C17 C19 C18 119.59(13) . . ?
C17 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 N2 C20 117.17(11) . . ?
C21 N2 Ni1 122.90(8) . . ?
C20 N2 Ni1 119.85(8) . . ?
N2 C20 C22 123.24(11) . . ?
N2 C20 H20 118.4 . . ?
C22 C20 H20 118.4 . . ?
N2 C21 C23 123.43(12) . . ?
N2 C21 H21 118.3 . . ?
C23 C21 H21 118.3 . . ?
C20 C22 C24 120.09(12) . . ?
C20 C22 H22 120.0 . . ?
C24 C22 H22 120.0 . . ?
C21 C23 C24 119.57(11) . . ?
C21 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C22 C24 C23 116.50(11) . . ?
C22 C24 C25 123.29(12) . . ?
C23 C24 C25 120.20(11) . . ?
C26 C25 C24 125.15(12) . . ?
C26 C25 H25 117.4 . . ?
C24 C25 H25 117.4 . . ?
C25 C26 C27 127.06(12) . . ?
C25 C26 H26 116.5 . . ?
C27 C26 H26 116.5 . . ?
C29 C27 C28 118.51(12) . . ?
C29 C27 C26 123.21(12) . . ?
C28 C27 C26 118.28(12) . . ?
C30 C28 C27 121.24(13) . . ?
C30 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C31 C29 C27 120.34(14) . . ?
C31 C29 H29 119.8 . . ?
C27 C29 H29 119.8 . . ?
C32 C30 C28 119.54(14) . . ?
C32 C30 H30 120.2 . . ?
C28 C30 H30 120.2 . . ?
C29 C31 C32 120.58(14) . . ?
C29 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C30 C32 C31 119.78(13) . . ?
C30 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2 0.89(3) 2.41(3) 2.8988(15) 115(2) 2
O1 H1 O3 0.89(3) 1.91(3) 2.7552(13) 160(2) 1_565
O1 H2 O5 0.90(3) 1.75(3) 2.6048(17) 157(2) 3_666

_refine_diff_density_max         0.677
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.106

####################################################################### 
# 
# 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_NiC4DCsty_UV_24h
_database_code_depnum_ccdc_archive 'CCDC 1524564'
_audit_update_record             
;
2016-12-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H64 N4 Ni2 O10'
_chemical_formula_weight         1166.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 '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                   21.313(4)
_cell_length_b                   8.5080(17)
_cell_length_c                   30.830(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.27(3)
_cell_angle_gamma                90
_cell_volume                     5575(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    99643
_cell_measurement_theta_min      1.552
_cell_measurement_theta_max      33.270

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34671
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         1.552
_diffrn_reflns_theta_max         33.270
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             18478
_reflns_number_gt                8870
_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       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.1424P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0176(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         18478
_refine_ls_number_parameters     851
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.1578
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2500
_refine_ls_wR_factor_gt          0.2061
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.004
_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 0.28629(2) 0.80166(4) 0.98204(2) 0.03528(14) Uani 1 1 d . . . . .
O1 O 0.29390(12) 0.5655(3) 0.96874(9) 0.0398(5) Uani 1 1 d . . . . .
H1W H 0.332(2) 0.545(4) 0.9622(13) 0.048 Uiso 1 1 d . U . . .
H2W H 0.2853(19) 0.510(5) 0.9897(13) 0.048 Uiso 1 1 d . U . . .
Ni2 Ni 0.18213(2) 0.30304(4) 1.03652(2) 0.03426(14) Uani 1 1 d . . . . .
O2 O 0.17528(12) 0.0687(3) 1.05131(9) 0.0380(5) Uani 1 1 d . . . . .
H3W H 0.1865(19) 0.014(5) 1.0334(13) 0.046 Uiso 1 1 d . U . . .
H4W H 0.1344(19) 0.055(4) 1.0559(12) 0.046 Uiso 1 1 d . U . . .
O3 O 0.37393(11) 0.8329(3) 0.95974(8) 0.0412(6) Uani 1 1 d . . . . .
O4 O 0.40646(12) 0.5915(3) 0.94246(9) 0.0522(7) Uani 1 1 d . . . . .
O5 O 0.72914(11) 0.9636(2) 1.00594(7) 0.0376(5) Uani 1 1 d . . . . .
O6 O 0.72872(11) 0.7135(2) 0.98506(7) 0.0354(5) Uani 1 1 d . . . . .
C1 C 0.41465(18) 0.7376(4) 0.94769(12) 0.0449(8) Uani 1 1 d . . . . .
C2 C 0.47915(17) 0.8032(4) 0.94153(13) 0.0471(9) Uani 1 1 d . . . . .
H2A H 0.4756 0.9166 0.9347 0.057 Uiso 1 1 calc R U . . .
H2B H 0.4969 0.7498 0.9167 0.057 Uiso 1 1 calc R U . . .
C3 C 0.52306(17) 0.7807(4) 0.98206(12) 0.0420(8) Uani 1 1 d . . . . .
H3A H 0.5223 0.6691 0.9912 0.050 Uiso 1 1 calc R U . . .
H3B H 0.5083 0.8454 1.0060 0.050 Uiso 1 1 calc R U . . .
C4 C 0.59022(16) 0.8276(4) 0.97381(12) 0.0428(8) Uani 1 1 d . . . . .
H4A H 0.6049 0.7612 0.9502 0.051 Uiso 1 1 calc R U . . .
H4B H 0.5903 0.9381 0.9638 0.051 Uiso 1 1 calc R U . . .
C5 C 0.63595(17) 0.8111(4) 1.01371(11) 0.0388(8) Uani 1 1 d . . . . .
H5A H 0.6265 0.8913 1.0356 0.047 Uiso 1 1 calc R U . . .
H5B H 0.6313 0.7060 1.0269 0.047 Uiso 1 1 calc R U . . .
C6 C 0.70243(17) 0.8319(3) 1.00122(11) 0.0366(7) Uani 1 1 d . . . . .
O7 O 0.19958(11) 0.7879(2) 1.00594(8) 0.0400(5) Uani 1 1 d . . . . .
O8 O 0.19826(11) 0.5370(2) 1.02494(8) 0.0382(5) Uani 1 1 d . . . . .
O9 O -0.09266(12) 0.6658(3) 0.94292(9) 0.0466(6) Uani 1 1 d . . . . .
O10 O -0.05927(12) 0.9051(3) 0.92726(9) 0.0527(7) Uani 1 1 d . . . . .
C7 C 0.17283(16) 0.6695(3) 1.02040(12) 0.0375(7) Uani 1 1 d D . . . .
C8A C 0.1070(5) 0.6968(15) 1.0349(4) 0.038(3) Uani 0.615(9) 1 d D . P A 1
H8A1 H 0.1011 0.8094 1.0416 0.046 Uiso 0.615(9) 1 calc R U P A 1
H8A2 H 0.1009 0.6349 1.0614 0.046 Uiso 0.615(9) 1 calc R U P A 1
C9A C 0.0590(3) 0.6452(8) 0.9976(2) 0.052(2) Uani 0.615(9) 1 d D . P A 1
H9A1 H 0.0160 0.6622 1.0068 0.062 Uiso 0.615(9) 1 calc R U P A 1
H9A2 H 0.0641 0.5311 0.9925 0.062 Uiso 0.615(9) 1 calc R U P A 1
C10A C 0.0655(3) 0.7347(9) 0.9533(3) 0.065(3) Uani 0.615(9) 1 d D . P A 1
H10A H 0.0638 0.8498 0.9578 0.079 Uiso 0.615(9) 1 calc R U P A 1
H10B H 0.1060 0.7082 0.9413 0.079 Uiso 0.615(9) 1 calc R U P A 1
C11A C 0.0108(6) 0.681(2) 0.9226(5) 0.054(4) Uani 0.615(9) 1 d D U P A 1
H11A H 0.0061 0.5659 0.9252 0.065 Uiso 0.615(9) 1 calc R U P A 1
H11B H 0.0204 0.7044 0.8923 0.065 Uiso 0.615(9) 1 calc R U P A 1
C8B C 0.1047(7) 0.678(3) 1.0286(8) 0.073(9) Uani 0.385(9) 1 d D . P A 2
H8B1 H 0.0884 0.5691 1.0301 0.087 Uiso 0.385(9) 1 calc R U P A 2
H8B2 H 0.1010 0.7268 1.0574 0.087 Uiso 0.385(9) 1 calc R U P A 2
C9B C 0.0641(4) 0.7660(12) 0.9959(3) 0.045(3) Uani 0.385(9) 1 d D . P A 2
H9B1 H 0.0865 0.8579 0.9848 0.054 Uiso 0.385(9) 1 calc R U P A 2
H9B2 H 0.0249 0.8019 1.0081 0.054 Uiso 0.385(9) 1 calc R U P A 2
C10B C 0.0503(6) 0.6433(17) 0.9601(4) 0.063(4) Uani 0.385(9) 1 d D U P A 2
H10C H 0.0907 0.6007 0.9514 0.076 Uiso 0.385(9) 1 calc R U P A 2
H10D H 0.0267 0.5554 0.9722 0.076 Uiso 0.385(9) 1 calc R U P A 2
C11B C 0.0133(9) 0.705(4) 0.9203(8) 0.060(9) Uani 0.385(9) 1 d D U P A 2
H11C H 0.0089 0.6213 0.8980 0.073 Uiso 0.385(9) 1 calc R U P A 2
H11D H 0.0362 0.7940 0.9081 0.073 Uiso 0.385(9) 1 calc R U P A 2
C12 C -0.05174(18) 0.7596(4) 0.93134(12) 0.0446(8) Uani 1 1 d D . . . .
N1 N 0.24842(15) 0.8356(3) 0.91656(10) 0.0425(7) Uani 1 1 d . . . . .
C13 C 0.2641(2) 0.7407(4) 0.88561(13) 0.0549(10) Uani 1 1 d . . . . .
H13 H 0.2811 0.6411 0.8941 0.066 Uiso 1 1 calc R U . . .
C14 C 0.21911(18) 0.9684(4) 0.90289(13) 0.0493(9) Uani 1 1 d . . . . .
H14 H 0.2035 1.0362 0.9241 0.059 Uiso 1 1 calc R U . . .
C15 C 0.2579(2) 0.7742(4) 0.84195(13) 0.0589(11) Uani 1 1 d . . . . .
H15 H 0.2717 0.7005 0.8216 0.071 Uiso 1 1 calc R U . . .
C16 C 0.21056(19) 1.0113(5) 0.85991(12) 0.0524(10) Uani 1 1 d . . . . .
H16 H 0.1901 1.1076 0.8523 0.063 Uiso 1 1 calc R U . . .
C17 C 0.23141(17) 0.9159(4) 0.82754(12) 0.0435(8) Uani 1 1 d . . . . .
C18 C 0.22970(19) 0.9704(4) 0.78098(12) 0.0481(9) Uani 1 1 d . . . . .
H18 H 0.1850 0.9883 0.7699 0.058 Uiso 1 1 calc R U . . .
C19 C 0.2629(2) 0.8720(5) 0.74764(13) 0.0580(11) Uani 1 1 d . . . . .
H19 H 0.296(2) 0.807(5) 0.7625(14) 0.070 Uiso 1 1 d . U . . .
C21A C 0.2599(3) 0.6106(7) 0.7184(2) 0.061(3) Uani 0.461(6) 1 d G . P B 1
H21A H 0.2932 0.5807 0.7390 0.073 Uiso 0.461(6) 1 calc R U P B 1
C20A C 0.2366(4) 0.7633(6) 0.7184(2) 0.047(3) Uani 0.461(6) 1 d G . P B 1
C22A C 0.1879(4) 0.8070(7) 0.6883(3) 0.071(4) Uani 0.461(6) 1 d G . P B 1
H22A H 0.1720 0.9114 0.6883 0.085 Uiso 0.461(6) 1 calc R U P B 1
C24A C 0.1625(4) 0.6982(11) 0.6583(3) 0.29(3) Uani 0.461(6) 1 d G . P B 1
H24A H 0.1292 0.7281 0.6378 0.347 Uiso 0.461(6) 1 calc R U P B 1
C25A C 0.1857(5) 0.5456(10) 0.6584(3) 0.088(5) Uani 0.461(6) 1 d G . P B 1
H25A H 0.1683 0.4712 0.6379 0.105 Uiso 0.461(6) 1 calc R U P B 1
C23A C 0.2345(4) 0.5018(6) 0.6885(3) 0.089(4) Uani 0.461(6) 1 d G . P B 1
H23A H 0.2504 0.3975 0.6885 0.107 Uiso 0.461(6) 1 calc R U P B 1
C20B C 0.2136(7) 0.7620(17) 0.7183(5) 0.084(4) Uani 0.539(6) 1 d . . P B 2
C21B C 0.1634(6) 0.6916(15) 0.7353(4) 0.116(5) Uani 0.539(6) 1 d . . P B 2
H21B H 0.1572 0.6998 0.7654 0.139 Uiso 0.539(6) 1 calc R U P B 2
C22B C 0.2269(5) 0.7157(9) 0.6789(3) 0.065(3) Uani 0.539(6) 1 d . . P B 2
H22B H 0.2682 0.7299 0.6699 0.078 Uiso 0.539(6) 1 calc R U P B 2
C23B C 0.1213(5) 0.6067(17) 0.7070(5) 0.145(7) Uani 0.539(6) 1 d . . P B 2
H23B H 0.0848 0.5607 0.7176 0.174 Uiso 0.539(6) 1 calc R U P B 2
C24B C 0.1818(7) 0.6478(17) 0.6512(4) 0.077(4) Uani 0.539(6) 1 d . . P B 2
H24B H 0.1884 0.6455 0.6211 0.092 Uiso 0.539(6) 1 calc R U P B 2
C25B C 0.1333(6) 0.5899(18) 0.6629(5) 0.135(7) Uani 0.539(6) 1 d . . P B 2
H25B H 0.1049 0.5357 0.6430 0.162 Uiso 0.539(6) 1 calc R U P B 2
N2 N 0.22042(15) 1.1574(3) 0.60049(9) 0.0413(7) Uani 1 1 d . . . . .
C26 C 0.1891(3) 1.1845(11) 0.63428(17) 0.159(4) Uani 1 1 d . . . . .
H26 H 0.1491 1.2335 0.6296 0.191 Uiso 1 1 calc R U . . .
C27 C 0.27624(18) 1.0956(5) 0.60938(13) 0.0558(10) Uani 1 1 d . . . . .
H27 H 0.3014 1.0750 0.5859 0.067 Uiso 1 1 calc R U . . .
C28 C 0.2097(4) 1.1473(14) 0.67621(18) 0.204(6) Uani 1 1 d . . . . .
H28 H 0.1832 1.1668 0.6991 0.245 Uiso 1 1 calc R U . . .
C29 C 0.30066(19) 1.0585(5) 0.65112(12) 0.0521(10) Uani 1 1 d . . . . .
H29 H 0.3417 1.0150 0.6553 0.063 Uiso 1 1 calc R U . . .
C30 C 0.2674(2) 1.0830(5) 0.68562(13) 0.0543(10) Uani 1 1 d . . . . .
C31 C 0.2920(2) 1.0276(5) 0.72996(12) 0.0553(10) Uani 1 1 d . . . . .
H31 H 0.3390 1.0203 0.7317 0.066 Uiso 1 1 calc R U . . .
C32 C 0.26977(19) 1.1178(4) 0.77050(12) 0.0502(9) Uani 1 1 d . . . . .
H32 H 0.2422 1.2088 0.7614 0.060 Uiso 1 1 calc R U . . .
C33 C 0.3201(2) 1.1656(4) 0.80484(13) 0.0489(9) Uani 1 1 d . . . . .
C34 C 0.3149(2) 1.3055(5) 0.82650(16) 0.0642(12) Uani 1 1 d . . . . .
H34 H 0.2812 1.3749 0.8180 0.077 Uiso 1 1 calc R U . . .
C35 C 0.3698(2) 1.0679(5) 0.81768(13) 0.0574(11) Uani 1 1 d . . . . .
H35 H 0.3748 0.9715 0.8028 0.069 Uiso 1 1 calc R U . . .
C36 C 0.3577(3) 1.3472(6) 0.86036(18) 0.0802(16) Uani 1 1 d . . . . .
H36 H 0.3534 1.4454 0.8745 0.096 Uiso 1 1 calc R U . . .
C37 C 0.4127(2) 1.1084(6) 0.85216(14) 0.0672(12) Uani 1 1 d . . . . .
H37 H 0.4465 1.0396 0.8608 0.081 Uiso 1 1 calc R U . . .
C38 C 0.4060(2) 1.2497(7) 0.87378(15) 0.0720(13) Uani 1 1 d . . . . .
H38 H 0.4346 1.2780 0.8976 0.086 Uiso 1 1 calc R U . . .
N3 N 0.33317(14) 0.7762(3) 1.04450(10) 0.0390(6) Uani 1 1 d . . . . .
C39 C 0.31788(18) 0.8633(4) 1.07826(12) 0.0455(8) Uani 1 1 d . . . . .
H39 H 0.2823 0.9306 1.0744 0.055 Uiso 1 1 calc R U . . .
C40 C 0.38239(18) 0.6793(4) 1.05140(13) 0.0451(9) Uani 1 1 d . . . . .
H40 H 0.3936 0.6152 1.0280 0.054 Uiso 1 1 calc R U . . .
C41 C 0.35117(19) 0.8605(4) 1.11833(12) 0.0470(9) Uani 1 1 d . . . . .
H41 H 0.3394 0.9280 1.1409 0.056 Uiso 1 1 calc R U . . .
C42 C 0.41787(19) 0.6672(4) 1.09060(13) 0.0489(9) Uani 1 1 d . . . . .
H42 H 0.4526 0.5971 1.0935 0.059 Uiso 1 1 calc R U . . .
C43 C 0.40266(18) 0.7579(4) 1.12593(12) 0.0440(8) Uani 1 1 d . . . . .
C44 C 0.4388(2) 0.7420(4) 1.16777(13) 0.0491(9) Uani 1 1 d . . . . .
H44 H 0.4757 0.6790 1.1684 0.059 Uiso 1 1 calc R U . . .
C45 C 0.4251(2) 0.8070(4) 1.20521(13) 0.0521(10) Uani 1 1 d . . . . .
H45 H 0.3876 0.8675 1.2049 0.063 Uiso 1 1 calc R U . . .
C46 C 0.4631(2) 0.7938(4) 1.24713(13) 0.0511(10) Uani 1 1 d . . . . .
C47 C 0.4378(2) 0.8449(5) 1.28486(13) 0.0574(11) Uani 1 1 d . . . . .
H47 H 0.3965 0.8877 1.2830 0.069 Uiso 1 1 calc R U . . .
C48 C 0.5235(2) 0.7348(5) 1.25086(14) 0.0555(10) Uani 1 1 d . . . . .
H48 H 0.5422 0.6995 1.2255 0.067 Uiso 1 1 calc R U . . .
C49 C 0.4714(2) 0.8354(5) 1.32543(14) 0.0600(11) Uani 1 1 d . . . . .
H49 H 0.4530 0.8686 1.3510 0.072 Uiso 1 1 calc R U . . .
C50 C 0.5575(2) 0.7260(5) 1.29072(14) 0.0612(11) Uani 1 1 d . . . . .
H50 H 0.5990 0.6846 1.2925 0.073 Uiso 1 1 calc R U . . .
C51 C 0.5320(2) 0.7763(5) 1.32747(14) 0.0606(11) Uani 1 1 d . . . . .
H51 H 0.5560 0.7708 1.3547 0.073 Uiso 1 1 calc R U . . .
N4 N 0.14206(14) 0.2772(3) 0.97224(9) 0.0379(6) Uani 1 1 d . . . . .
C52 C 0.16180(18) 0.3633(4) 0.93986(12) 0.0456(9) Uani 1 1 d . . . . .
H52 H 0.1972 0.4298 0.9459 0.055 Uiso 1 1 calc R U . . .
C53 C 0.09196(17) 0.1862(4) 0.96281(13) 0.0451(8) Uani 1 1 d . . . . .
H53 H 0.0773 0.1227 0.9853 0.054 Uiso 1 1 calc R U . . .
C54 C 0.1340(2) 0.3614(4) 0.89826(13) 0.0539(10) Uani 1 1 d . . . . .
H54 H 0.1506 0.4238 0.8762 0.065 Uiso 1 1 calc R U . . .
C55 C 0.0604(2) 0.1791(5) 0.92245(13) 0.0555(10) Uani 1 1 d . . . . .
H55 H 0.0244 0.1139 0.9177 0.067 Uiso 1 1 calc R U . . .
C56 C 0.0814(2) 0.2677(5) 0.88859(13) 0.0555(10) Uani 1 1 d . . . . .
C57 C 0.0484(3) 0.2578(8) 0.84532(18) 0.0921(18) Uani 1 1 d . . . . .
H57 H 0.0130 0.1896 0.8426 0.111 Uiso 1 1 calc R U . . .
C58 C 0.0616(5) 0.3305(11) 0.8106(3) 0.147(4) Uani 1 1 d D . . . .
H58 H 0.103(2) 0.389(9) 0.815(3) 0.176 Uiso 1 1 d D U . . .
C60A C 0.0584(3) 0.3494(11) 0.7280(3) 0.119(4) Uani 0.665(6) 1 d G U P C 1
H60A H 0.1020 0.3734 0.7297 0.143 Uiso 0.665(6) 1 calc R U P C 1
C59A C 0.0288(4) 0.3170(11) 0.7657(3) 0.175(8) Uani 0.665(6) 1 d G U P C 1
C61A C -0.0351(4) 0.2819(9) 0.7632(2) 0.112(4) Uani 0.665(6) 1 d G U P C 1
H61A H -0.0553 0.2597 0.7890 0.135 Uiso 0.665(6) 1 calc R U P C 1
C63A C -0.0693(3) 0.2793(10) 0.7231(3) 0.134(4) Uani 0.665(6) 1 d G U P C 1
H63A H -0.1130 0.2554 0.7214 0.161 Uiso 0.665(6) 1 calc R U P C 1
C64A C -0.0398(5) 0.3118(12) 0.6854(2) 0.317(16) Uani 0.665(6) 1 d G U P C 1
H64A H -0.0632 0.3100 0.6580 0.380 Uiso 0.665(6) 1 calc R U P C 1
C62A C 0.0241(5) 0.3468(11) 0.6879(3) 0.145(5) Uani 0.665(6) 1 d G U P C 1
H62A H 0.0443 0.3690 0.6621 0.174 Uiso 0.665(6) 1 calc R U P C 1
C60B C 0.0263(6) 0.2064(13) 0.7440(4) 0.109(7) Uani 0.335(6) 1 d G U P C 2
H60B H 0.0533 0.1235 0.7542 0.130 Uiso 0.335(6) 1 calc R U P C 2
C59B C 0.0168(6) 0.3348(14) 0.7706(3) 0.069(5) Uani 0.335(6) 1 d G U P C 2
C61B C -0.0229(6) 0.4562(12) 0.7556(3) 0.090(5) Uani 0.335(6) 1 d G U P C 2
H61B H -0.0294 0.5439 0.7738 0.109 Uiso 0.335(6) 1 calc R U P C 2
C63B C -0.0530(5) 0.4490(10) 0.7141(3) 0.084(5) Uani 0.335(6) 1 d G U P C 2
H63B H -0.0800 0.5320 0.7039 0.101 Uiso 0.335(6) 1 calc R U P C 2
C64B C -0.0435(5) 0.3206(11) 0.6875(2) 0.049(3) Uani 0.335(6) 1 d G U P C 2
H64B H -0.0640 0.3157 0.6591 0.059 Uiso 0.335(6) 1 calc R U P C 2
C62B C -0.0038(6) 0.1993(11) 0.7024(4) 0.160(11) Uani 0.335(6) 1 d G U P C 2
H62B H 0.0027 0.1115 0.6843 0.192 Uiso 0.335(6) 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
Ni1 O7 2.043(2) . ?
Ni1 O3 2.055(3) . ?
Ni1 O1 2.059(2) . ?
Ni1 O5 2.062(2) 3_677 ?
Ni1 N3 2.113(3) . ?
Ni1 N1 2.137(3) . ?
Ni2 O2 2.053(2) . ?
Ni2 O8 2.056(2) . ?
Ni2 O6 2.064(2) 3_667 ?
Ni2 O9 2.071(3) 3_567 ?
Ni2 N2 2.105(3) 4_576 ?
Ni2 N4 2.110(3) . ?
O3 C1 1.264(4) . ?
O4 C1 1.264(4) . ?
O5 C6 1.260(4) . ?
O5 Ni1 2.062(2) 3_677 ?
O6 C6 1.273(4) . ?
O6 Ni2 2.064(2) 3_667 ?
C1 C2 1.509(5) . ?
C2 C3 1.517(5) . ?
C3 C4 1.526(5) . ?
C4 C5 1.518(5) . ?
C5 C6 1.506(5) . ?
O7 C7 1.256(4) . ?
O8 C7 1.253(4) . ?
O9 C12 1.253(4) . ?
O9 Ni2 2.071(3) 3_567 ?
O10 C12 1.254(4) . ?
C7 C8B 1.493(16) . ?
C7 C8A 1.521(11) . ?
C8A C9A 1.545(12) . ?
C9A C10A 1.578(11) . ?
C10A C11A 1.517(14) . ?
C11A C12 1.531(11) . ?
C8B C9B 1.484(17) . ?
C9B C10B 1.531(13) . ?
C10B C11B 1.502(18) . ?
C11B C12 1.525(17) . ?
N1 C13 1.312(5) . ?
N1 C14 1.344(4) . ?
C13 C15 1.373(5) . ?
C14 C16 1.373(5) . ?
C15 C17 1.390(5) . ?
C16 C17 1.385(5) . ?
C17 C18 1.506(5) . ?
C18 C19 1.538(6) . ?
C18 C32 1.564(5) . ?
C19 C20A 1.381(6) . ?
C19 C31 1.576(6) . ?
C19 C20B 1.630(13) . ?
C21A C20A 1.3900 . ?
C21A C23A 1.3900 . ?
C20A C22A 1.3900 . ?
C22A C24A 1.3900 . ?
C24A C25A 1.3900 . ?
C25A C23A 1.3900 . ?
C20B C22B 1.327(15) . ?
C20B C21B 1.36(2) . ?
C21B C23B 1.403(14) . ?
C22B C24B 1.366(14) . ?
C23B C25B 1.41(2) . ?
C24B C25B 1.22(2) . ?
N2 C26 1.299(6) . ?
N2 C27 1.311(5) . ?
N2 Ni2 2.105(3) 4_575 ?
C26 C28 1.371(7) . ?
C27 C29 1.388(5) . ?
C28 C30 1.356(7) . ?
C29 C30 1.338(6) . ?
C30 C31 1.503(5) . ?
C31 C32 1.569(5) . ?
C32 C33 1.505(5) . ?
C33 C34 1.374(5) . ?
C33 C35 1.381(6) . ?
C34 C36 1.381(7) . ?
C35 C37 1.393(6) . ?
C36 C38 1.362(7) . ?
C37 C38 1.387(7) . ?
N3 C39 1.338(5) . ?
N3 C40 1.339(4) . ?
C39 C41 1.378(5) . ?
C40 C42 1.381(5) . ?
C41 C43 1.408(5) . ?
C42 C43 1.392(5) . ?
C43 C44 1.459(5) . ?
C44 C45 1.332(6) . ?
C45 C46 1.477(5) . ?
C46 C48 1.380(6) . ?
C46 C47 1.387(6) . ?
C47 C49 1.396(5) . ?
C48 C50 1.381(5) . ?
C49 C51 1.384(7) . ?
C50 C51 1.361(6) . ?
N4 C52 1.331(5) . ?
N4 C53 1.334(4) . ?
C52 C54 1.372(5) . ?
C53 C55 1.371(5) . ?
C54 C56 1.390(6) . ?
C55 C56 1.388(6) . ?
C56 C57 1.464(6) . ?
C57 C58 1.285(10) . ?
C58 C59B 1.504(10) . ?
C58 C59A 1.508(9) . ?
C60A C59A 1.3900 . ?
C60A C62A 1.3900 . ?
C59A C61A 1.3900 . ?
C61A C63A 1.3900 . ?
C63A C64A 1.3900 . ?
C64A C62A 1.3900 . ?
C60B C59B 1.3900 . ?
C60B C62B 1.3900 . ?
C59B C61B 1.3900 . ?
C61B C63B 1.3900 . ?
C63B C64B 1.3900 . ?
C64B C62B 1.3900 . ?

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
O7 Ni1 O3 175.61(9) . . ?
O7 Ni1 O1 95.88(10) . . ?
O3 Ni1 O1 88.43(10) . . ?
O7 Ni1 O5 80.22(9) . 3_677 ?
O3 Ni1 O5 95.50(9) . 3_677 ?
O1 Ni1 O5 175.30(10) . 3_677 ?
O7 Ni1 N3 92.55(11) . . ?
O3 Ni1 N3 86.46(11) . . ?
O1 Ni1 N3 92.44(10) . . ?
O5 Ni1 N3 90.37(9) 3_677 . ?
O7 Ni1 N1 93.45(11) . . ?
O3 Ni1 N1 87.44(11) . . ?
O1 Ni1 N1 88.49(10) . . ?
O5 Ni1 N1 89.12(10) 3_677 . ?
N3 Ni1 N1 173.80(12) . . ?
O2 Ni2 O8 174.01(10) . . ?
O2 Ni2 O6 95.04(10) . 3_667 ?
O8 Ni2 O6 80.79(9) . 3_667 ?
O2 Ni2 O9 88.51(10) . 3_567 ?
O8 Ni2 O9 95.68(9) . 3_567 ?
O6 Ni2 O9 176.44(9) 3_667 3_567 ?
O2 Ni2 N2 88.62(10) . 4_576 ?
O8 Ni2 N2 87.12(10) . 4_576 ?
O6 Ni2 N2 90.62(11) 3_667 4_576 ?
O9 Ni2 N2 89.68(12) 3_567 4_576 ?
O2 Ni2 N4 94.41(10) . . ?
O8 Ni2 N4 89.95(9) . . ?
O6 Ni2 N4 90.47(11) 3_667 . ?
O9 Ni2 N4 89.04(11) 3_567 . ?
N2 Ni2 N4 176.67(10) 4_576 . ?
C1 O3 Ni1 132.6(2) . . ?
C6 O5 Ni1 143.6(2) . 3_677 ?
C6 O6 Ni2 128.5(2) . 3_667 ?
O4 C1 O3 125.3(3) . . ?
O4 C1 C2 117.8(3) . . ?
O3 C1 C2 116.8(3) . . ?
C1 C2 C3 111.2(3) . . ?
C2 C3 C4 111.0(3) . . ?
C5 C4 C3 113.2(3) . . ?
C6 C5 C4 110.0(3) . . ?
O5 C6 O6 122.8(3) . . ?
O5 C6 C5 120.0(3) . . ?
O6 C6 C5 117.2(3) . . ?
C7 O7 Ni1 128.4(2) . . ?
C7 O8 Ni2 144.4(2) . . ?
C12 O9 Ni2 133.0(2) . 3_567 ?
O8 C7 O7 123.8(3) . . ?
O8 C7 C8B 116.2(10) . . ?
O7 C7 C8B 119.7(9) . . ?
O8 C7 C8A 120.3(6) . . ?
O7 C7 C8A 115.7(5) . . ?
C7 C8A C9A 108.2(8) . . ?
C8A C9A C10A 114.2(7) . . ?
C11A C10A C9A 106.4(10) . . ?
C10A C11A C12 113.5(10) . . ?
C9B C8B C7 115.7(14) . . ?
C8B C9B C10B 102.5(14) . . ?
C11B C10B C9B 114.3(16) . . ?
C10B C11B C12 110.8(15) . . ?
O9 C12 O10 124.8(4) . . ?
O9 C12 C11B 122.2(14) . . ?
O10 C12 C11B 113.0(14) . . ?
O9 C12 C11A 113.9(9) . . ?
O10 C12 C11A 121.3(9) . . ?
C13 N1 C14 115.3(3) . . ?
C13 N1 Ni1 120.3(3) . . ?
C14 N1 Ni1 123.0(2) . . ?
N1 C13 C15 125.0(4) . . ?
N1 C14 C16 123.4(4) . . ?
C13 C15 C17 120.1(4) . . ?
C14 C16 C17 120.9(4) . . ?
C16 C17 C15 115.0(4) . . ?
C16 C17 C18 121.3(3) . . ?
C15 C17 C18 123.5(3) . . ?
C17 C18 C19 119.3(3) . . ?
C17 C18 C32 117.9(3) . . ?
C19 C18 C32 90.7(3) . . ?
C20A C19 C18 128.1(5) . . ?
C20A C19 C31 119.2(5) . . ?
C18 C19 C31 89.2(3) . . ?
C18 C19 C20B 112.0(6) . . ?
C31 C19 C20B 123.0(7) . . ?
C20A C21A C23A 120.0 . . ?
C19 C20A C22A 120.1(5) . . ?
C19 C20A C21A 119.9(5) . . ?
C22A C20A C21A 120.0 . . ?
C20A C22A C24A 120.0 . . ?
C25A C24A C22A 120.0 . . ?
C23A C25A C24A 120.0 . . ?
C25A C23A C21A 120.0 . . ?
C22B C20B C21B 116.7(11) . . ?
C22B C20B C19 120.3(13) . . ?
C21B C20B C19 122.0(11) . . ?
C20B C21B C23B 118.0(13) . . ?
C20B C22B C24B 120.5(13) . . ?
C21B C23B C25B 119.8(13) . . ?
C25B C24B C22B 124.0(13) . . ?
C24B C25B C23B 117.4(11) . . ?
C26 N2 C27 114.6(4) . . ?
C26 N2 Ni2 122.5(3) . 4_575 ?
C27 N2 Ni2 122.9(3) . 4_575 ?
N2 C26 C28 124.5(5) . . ?
N2 C27 C29 123.8(4) . . ?
C30 C28 C26 121.1(5) . . ?
C30 C29 C27 121.2(4) . . ?
C29 C30 C28 114.7(4) . . ?
C29 C30 C31 120.3(4) . . ?
C28 C30 C31 124.8(4) . . ?
C30 C31 C32 117.7(3) . . ?
C30 C31 C19 117.3(4) . . ?
C32 C31 C19 89.2(3) . . ?
C33 C32 C18 116.3(3) . . ?
C33 C32 C31 116.8(3) . . ?
C18 C32 C31 88.5(3) . . ?
C34 C33 C35 118.0(4) . . ?
C34 C33 C32 119.8(4) . . ?
C35 C33 C32 122.0(3) . . ?
C33 C34 C36 121.2(5) . . ?
C33 C35 C37 121.1(4) . . ?
C38 C36 C34 121.0(5) . . ?
C38 C37 C35 119.7(5) . . ?
C36 C38 C37 119.0(5) . . ?
C39 N3 C40 116.8(3) . . ?
C39 N3 Ni1 121.7(2) . . ?
C40 N3 Ni1 121.3(3) . . ?
N3 C39 C41 123.3(3) . . ?
N3 C40 C42 123.8(4) . . ?
C39 C41 C43 120.2(4) . . ?
C40 C42 C43 119.9(3) . . ?
C42 C43 C41 115.9(3) . . ?
C42 C43 C44 120.1(3) . . ?
C41 C43 C44 123.9(4) . . ?
C45 C44 C43 126.4(4) . . ?
C44 C45 C46 125.9(4) . . ?
C48 C46 C47 117.5(4) . . ?
C48 C46 C45 123.2(4) . . ?
C47 C46 C45 119.3(4) . . ?
C46 C47 C49 121.9(5) . . ?
C50 C48 C46 121.2(4) . . ?
C51 C49 C47 118.4(5) . . ?
C51 C50 C48 120.6(5) . . ?
C50 C51 C49 120.4(4) . . ?
C52 N4 C53 116.6(3) . . ?
C52 N4 Ni2 121.2(2) . . ?
C53 N4 Ni2 121.8(3) . . ?
N4 C52 C54 123.8(3) . . ?
N4 C53 C55 123.7(4) . . ?
C52 C54 C56 119.5(4) . . ?
C53 C55 C56 119.7(4) . . ?
C55 C56 C54 116.8(4) . . ?
C55 C56 C57 119.6(4) . . ?
C54 C56 C57 123.6(4) . . ?
C58 C57 C56 127.6(6) . . ?
C57 C58 C59B 122.0(9) . . ?
C57 C58 C59A 127.8(8) . . ?
C59A C60A C62A 120.0 . . ?
C61A C59A C60A 120.0 . . ?
C61A C59A C58 116.8(8) . . ?
C60A C59A C58 123.0(8) . . ?
C59A C61A C63A 120.0 . . ?
C64A C63A C61A 120.0 . . ?
C63A C64A C62A 120.0 . . ?
C64A C62A C60A 120.0 . . ?
C59B C60B C62B 120.0 . . ?
C61B C59B C60B 120.0 . . ?
C61B C59B C58 128.5(9) . . ?
C60B C59B C58 110.7(9) . . ?
C63B C61B C59B 120.0 . . ?
C61B C63B C64B 120.0 . . ?
C63B C64B C62B 120.0 . . ?
C64B C62B C60B 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1W O4 0.87(4) 1.79(4) 2.598(4) 155(4) .
O1 H2W O6 0.83(4) 2.08(4) 2.828(3) 149(4) 3_667
O1 H2W O8 0.83(4) 2.23(4) 2.782(4) 124(3) .
O2 H3W O5 0.77(4) 2.25(4) 2.807(4) 130(4) 3_667
O2 H3W O7 0.77(4) 2.13(4) 2.835(3) 152(4) 1_545
O2 H4W O10 0.90(4) 1.75(4) 2.616(4) 159(4) 3_567

_refine_diff_density_max         1.459
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.117

####################################################################### 
# 
# 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_NiC4DCsty_UV_6h
_database_code_depnum_ccdc_archive 'CCDC 1524565'
_audit_update_record             
;
2016-12-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 N2 Ni O5'
_chemical_formula_sum            'C32 H32 N2 Ni O5'
_chemical_formula_weight         583.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 '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 0.0048 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0087 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3417 0.9522 '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                   18.732(4)
_cell_length_b                   8.4040(17)
_cell_length_c                   18.827(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.03(3)
_cell_angle_gamma                90
_cell_volume                     2685.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    67052
_cell_measurement_theta_min      1.847
_cell_measurement_theta_max      33.341

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.650
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37046
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.847
_diffrn_reflns_theta_max         33.341
_diffrn_reflns_theta_full        22.955
_diffrn_measured_fraction_theta_max 0.745
_diffrn_measured_fraction_theta_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.745
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_point_group_measured_fraction_full 0.947
_reflns_number_total             10138
_reflns_number_gt                5330
_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       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.0919P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0165(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         10138
_refine_ls_number_parameters     497
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1917
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   1.076
_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 0.33799(2) 0.22624(4) 0.28054(2) 0.02307(12) Uani 1 1 d . . . . .
O1 O 0.35995(13) 0.4655(2) 0.28472(13) 0.0277(5) Uani 1 1 d D . . . .
H1W H 0.4123(11) 0.477(5) 0.307(2) 0.057(13) Uiso 1 1 d D . . . .
H2W H 0.3289(17) 0.534(4) 0.288(2) 0.033(10) Uiso 1 1 d D . . . .
O2 O 0.21927(12) 0.2441(2) 0.20729(12) 0.0266(4) Uani 1 1 d . . . . .
O3 O 0.19047(12) 0.4860(2) 0.23221(11) 0.0246(4) Uani 1 1 d . . . . .
O4 O -0.04251(11) 0.3051(2) -0.14803(12) 0.0250(4) Uani 1 1 d . . . . .
O5 O 0.01018(12) 0.0616(2) -0.12767(13) 0.0315(5) Uani 1 1 d . . . . .
C1 C 0.17163(16) 0.3588(3) 0.19435(16) 0.0205(5) Uani 1 1 d . . . . .
C2 C 0.08765(17) 0.3316(3) 0.13389(16) 0.0243(6) Uani 1 1 d . . . . .
H2A H 0.0603 0.4355 0.1203 0.029 Uiso 1 1 calc R U . . .
H2B H 0.0600 0.2650 0.1578 0.029 Uiso 1 1 calc R U . . .
C3 C 0.08109(18) 0.2512(3) 0.05837(17) 0.0261(6) Uani 1 1 d . . . . .
H3A H 0.1184 0.1608 0.0721 0.031 Uiso 1 1 calc R U . . .
H3B H 0.0272 0.2078 0.0300 0.031 Uiso 1 1 calc R U . . .
C4 C 0.09828(18) 0.3632(3) 0.00459(17) 0.0273(6) Uani 1 1 d . . . . .
H4A H 0.1513 0.4098 0.0336 0.033 Uiso 1 1 calc R U . . .
H4B H 0.0596 0.4513 -0.0108 0.033 Uiso 1 1 calc R U . . .
C5 C 0.09487(17) 0.2815(4) -0.06947(18) 0.0276(6) Uani 1 1 d . . . . .
H5A H 0.1078 0.3603 -0.1014 0.033 Uiso 1 1 calc R U . . .
H5B H 0.1352 0.1966 -0.0542 0.033 Uiso 1 1 calc R U . . .
C6 C 0.01500(16) 0.2097(3) -0.11876(16) 0.0231(5) Uani 1 1 d . . . . .
N1A N 0.3537(6) 0.2127(19) 0.1826(9) 0.0227(19) Uani 0.602(5) 1 d . U P A 1
C7A C 0.4158(7) 0.2811(15) 0.1755(9) 0.0237(18) Uani 0.602(5) 1 d . . P A 1
H7A H 0.4512 0.3430 0.2180 0.028 Uiso 0.602(5) 1 calc R U P A 1
C8A C 0.3038(6) 0.1264(15) 0.1203(8) 0.0208(16) Uani 0.602(5) 1 d . . P A 1
H8A H 0.2605 0.0745 0.1241 0.025 Uiso 0.602(5) 1 calc R U P A 1
C9A C 0.4304(3) 0.2662(7) 0.1103(3) 0.0208(10) Uani 0.602(5) 1 d . . P A 1
H9A H 0.4751 0.3167 0.1087 0.025 Uiso 0.602(5) 1 calc R U P A 1
C10A C 0.3132(4) 0.1108(8) 0.0521(5) 0.0228(13) Uani 0.602(5) 1 d . . P A 1
H10A H 0.2747 0.0555 0.0089 0.027 Uiso 0.602(5) 1 calc R U P A 1
C11A C 0.3794(3) 0.1762(6) 0.0459(3) 0.0204(10) Uani 0.602(5) 1 d . . P A 1
C12A C 0.3917(3) 0.1433(5) -0.0243(3) 0.0199(10) Uani 0.602(5) 1 d . . P A 1
H12A H 0.3491 0.0949 -0.0669 0.024 Uiso 0.602(5) 1 calc R U P A 1
C13A C 0.4565(3) 0.1739(6) -0.0352(3) 0.0211(10) Uani 0.602(5) 1 d . . P A 1
H13A H 0.4999 0.2213 0.0069 0.025 Uiso 0.602(5) 1 calc R U P A 1
C14A C 0.4652(7) 0.139(2) -0.1074(10) 0.024(2) Uani 0.602(5) 1 d . U P A 1
C15A C 0.5362(6) 0.1914(10) -0.1114(5) 0.0267(16) Uani 0.602(5) 1 d . U P A 1
H15A H 0.5755 0.2453 -0.0682 0.032 Uiso 0.602(5) 1 calc R U P A 1
C16A C 0.4157(13) 0.053(2) -0.1669(12) 0.027(2) Uani 0.602(5) 1 d . U P A 1
H16A H 0.3716 0.0071 -0.1621 0.033 Uiso 0.602(5) 1 calc R U P A 1
C17A C 0.5474(3) 0.1626(7) -0.1787(4) 0.0275(12) Uani 0.602(5) 1 d . U P A 1
H17A H 0.5936 0.2007 -0.1822 0.033 Uiso 0.602(5) 1 calc R U P A 1
C18A C 0.4240(4) 0.0260(8) -0.2351(4) 0.0299(13) Uani 0.602(5) 1 d . U P A 1
H18A H 0.3840 -0.0281 -0.2777 0.036 Uiso 0.602(5) 1 calc R U P A 1
C19A C 0.4913(3) 0.0783(6) -0.2410(3) 0.0276(11) Uani 0.602(5) 1 d . U P A 1
H19A H 0.4992 0.0570 -0.2868 0.033 Uiso 0.602(5) 1 calc R U P A 1
N1B N 0.3676(9) 0.204(3) 0.1749(11) 0.020(3) Uani 0.398(5) 1 d . U P A 2
C7B C 0.4337(10) 0.251(2) 0.1722(15) 0.032(3) Uani 0.398(5) 1 d . . P A 2
H7B H 0.4672 0.3194 0.2130 0.039 Uiso 0.398(5) 1 calc R U P A 2
C8B C 0.3195(12) 0.123(3) 0.1101(17) 0.039(5) Uani 0.398(5) 1 d . . P A 2
H8B H 0.2682 0.0978 0.1053 0.047 Uiso 0.398(5) 1 calc R U P A 2
C9B C 0.4583(6) 0.2094(13) 0.1142(6) 0.037(2) Uani 0.398(5) 1 d . . P A 2
H9B H 0.5068 0.2489 0.1168 0.044 Uiso 0.398(5) 1 calc R U P A 2
C10B C 0.3388(7) 0.0722(15) 0.0499(7) 0.036(2) Uani 0.398(5) 1 d . . P A 2
H10B H 0.3018 0.0124 0.0075 0.043 Uiso 0.398(5) 1 calc R U P A 2
C11B C 0.4113(6) 0.1086(12) 0.0514(5) 0.033(2) Uani 0.398(5) 1 d . . P A 2
C12B C 0.4404(5) 0.0300(10) -0.0046(5) 0.0334(19) Uani 0.398(5) 1 d . . P A 2
H12B H 0.3939 -0.0065 -0.0524 0.040 Uiso 0.398(5) 1 calc R U P A 2
C13B C 0.5000(5) 0.1149(10) -0.0301(5) 0.034(2) Uani 0.398(5) 1 d . . P A 2
H13B H 0.5216 0.2126 0.0022 0.041 Uiso 0.398(5) 1 calc R U P A 2
C15B C 0.5327(11) 0.225(2) -0.1331(9) 0.048(4) Uani 0.398(5) 1 d . U P A 2
H15B H 0.5761 0.2766 -0.0929 0.057 Uiso 0.398(5) 1 calc R U P A 2
C14B C 0.4819(10) 0.146(3) -0.1099(15) 0.025(4) Uani 0.398(5) 1 d . U P A 2
C16B C 0.409(2) 0.078(3) -0.1770(19) 0.031(5) Uani 0.398(5) 1 d . U P A 2
H16B H 0.3665 0.0319 -0.1688 0.037 Uiso 0.398(5) 1 calc R U P A 2
C18B C 0.4081(8) 0.0898(16) -0.2507(8) 0.050(3) Uani 0.398(5) 1 d . U P A 2
H18B H 0.3645 0.0440 -0.2932 0.060 Uiso 0.398(5) 1 calc R U P A 2
C19B C 0.4647(7) 0.1612(15) -0.2679(7) 0.050(3) Uani 0.398(5) 1 d . U P A 2
H19B H 0.4617 0.1606 -0.3195 0.060 Uiso 0.398(5) 1 calc R U P A 2
C17B C 0.5284(7) 0.2366(15) -0.2046(7) 0.048(3) Uani 0.398(5) 1 d . U P A 2
H17B H 0.5672 0.2944 -0.2140 0.058 Uiso 0.398(5) 1 calc R U P A 2
N2 N 0.31326(14) 0.2318(3) 0.37984(14) 0.0243(5) Uani 1 1 d . . . . .
C20 C 0.25221(17) 0.1483(3) 0.38021(18) 0.0264(6) Uani 1 1 d . . . . .
H20 H 0.2194 0.0925 0.3340 0.032 Uiso 1 1 calc R U . . .
C21 C 0.35816(17) 0.3083(3) 0.44569(17) 0.0261(6) Uani 1 1 d . . . . .
H21 H 0.4017 0.3677 0.4467 0.031 Uiso 1 1 calc R U . . .
C22 C 0.23489(18) 0.1395(4) 0.44382(19) 0.0297(6) Uani 1 1 d . . . . .
H22 H 0.1909 0.0786 0.4406 0.036 Uiso 1 1 calc R U . . .
C23 C 0.34492(18) 0.3062(3) 0.51307(18) 0.0301(7) Uani 1 1 d . . . . .
H23 H 0.3787 0.3632 0.5585 0.036 Uiso 1 1 calc R U . . .
C24 C 0.28092(18) 0.2188(4) 0.51322(18) 0.0288(6) Uani 1 1 d . . . . .
C25 C 0.2654(2) 0.2177(4) 0.5825(2) 0.0358(7) Uani 1 1 d . . . . .
H25 H 0.2988 0.2801 0.6260 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2071(2) 0.1348(4) 0.58995(19) 0.0333(7) Uani 1 1 d . . . . .
H26 H 0.1745 0.0730 0.5459 0.040 Uiso 1 1 calc R U . . .
C27 C 0.1882(2) 0.1290(4) 0.6576(2) 0.0328(7) Uani 1 1 d . . . . .
C28 C 0.1295(2) 0.0253(4) 0.6561(2) 0.0375(8) Uani 1 1 d . . . . .
H28 H 0.1023 -0.0380 0.6108 0.045 Uiso 1 1 calc R U . . .
C29 C 0.2271(2) 0.2217(4) 0.7253(2) 0.0384(8) Uani 1 1 d . . . . .
H29 H 0.2668 0.2948 0.7279 0.046 Uiso 1 1 calc R U . . .
C30 C 0.1100(2) 0.0126(4) 0.7192(2) 0.0412(8) Uani 1 1 d . . . . .
H30 H 0.0694 -0.0582 0.7167 0.049 Uiso 1 1 calc R U . . .
C31 C 0.2077(2) 0.2067(4) 0.7883(2) 0.0428(9) Uani 1 1 d . . . . .
H31 H 0.2348 0.2688 0.8341 0.051 Uiso 1 1 calc R U . . .
C32 C 0.1492(2) 0.1020(4) 0.7851(2) 0.0406(8) Uani 1 1 d . . . . .
H32 H 0.1364 0.0924 0.8286 0.049 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 N1A 1.990(12) . ?
Ni1 O1 2.047(2) . ?
Ni1 O2 2.068(2) . ?
Ni1 O3 2.0763(19) 2_545 ?
Ni1 O4 2.084(2) 4_666 ?
Ni1 N2 2.108(3) . ?
Ni1 N1B 2.286(16) . ?
O2 C1 1.265(3) . ?
O3 C1 1.250(3) . ?
O3 Ni1 2.0763(19) 2 ?
O4 C6 1.266(3) . ?
O4 Ni1 2.084(2) 4_565 ?
O5 C6 1.254(3) . ?
C1 C2 1.519(4) . ?
C2 C3 1.532(4) . ?
C3 C4 1.513(4) . ?
C4 C5 1.531(4) . ?
C5 C6 1.513(4) . ?
N1A C7A 1.354(16) . ?
N1A C8A 1.36(2) . ?
C7A C9A 1.371(14) . ?
C8A C10A 1.374(13) . ?
C9A C11A 1.405(7) . ?
C10A C11A 1.407(8) . ?
C11A C12A 1.461(6) . ?
C12A C13A 1.338(7) . ?
C13A C14A 1.465(17) . ?
C14A C16A 1.33(3) . ?
C14A C15A 1.432(14) . ?
C15A C17A 1.391(12) . ?
C16A C18A 1.38(3) . ?
C17A C19A 1.392(8) . ?
C18A C19A 1.384(9) . ?
N1B C7B 1.32(2) . ?
N1B C8B 1.36(4) . ?
C7B C9B 1.40(2) . ?
C8B C10B 1.39(2) . ?
C9B C11B 1.417(12) . ?
C10B C11B 1.381(14) . ?
C11B C12B 1.526(13) . ?
C12B C13B 1.562(12) . ?
C12B C13B 1.593(13) 3_655 ?
C13B C14B 1.42(3) . ?
C13B C12B 1.593(13) 3_655 ?
C15B C17B 1.32(2) . ?
C15B C14B 1.37(3) . ?
C14B C16B 1.53(4) . ?
C16B C18B 1.39(4) . ?
C18B C19B 1.371(17) . ?
C19B C17B 1.428(15) . ?
N2 C21 1.332(4) . ?
N2 C20 1.344(4) . ?
C20 C22 1.369(5) . ?
C21 C23 1.392(4) . ?
C22 C24 1.393(4) . ?
C23 C24 1.407(4) . ?
C24 C25 1.453(5) . ?
C25 C26 1.351(5) . ?
C26 C27 1.459(5) . ?
C27 C28 1.393(5) . ?
C27 C29 1.407(5) . ?
C28 C30 1.388(5) . ?
C29 C31 1.384(5) . ?
C30 C32 1.369(5) . ?
C31 C32 1.387(5) . ?

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
N1A Ni1 O1 89.2(5) . . ?
N1A Ni1 O2 85.7(3) . . ?
O1 Ni1 O2 95.52(8) . . ?
N1A Ni1 O3 88.2(5) . 2_545 ?
O1 Ni1 O3 175.74(8) . 2_545 ?
O2 Ni1 O3 80.93(8) . 2_545 ?
N1A Ni1 O4 92.9(3) . 4_666 ?
O1 Ni1 O4 87.46(8) . 4_666 ?
O2 Ni1 O4 176.69(8) . 4_666 ?
O3 Ni1 O4 96.02(8) 2_545 4_666 ?
N1A Ni1 N2 175.7(4) . . ?
O1 Ni1 N2 93.44(9) . . ?
O2 Ni1 N2 90.69(9) . . ?
O3 Ni1 N2 88.97(8) 2_545 . ?
O4 Ni1 N2 90.55(9) 4_666 . ?
O1 Ni1 N1B 89.7(6) . . ?
O2 Ni1 N1B 90.8(4) . . ?
O3 Ni1 N1B 88.0(6) 2_545 . ?
O4 Ni1 N1B 87.8(4) 4_666 . ?
N2 Ni1 N1B 176.3(5) . . ?
C1 O2 Ni1 130.96(18) . . ?
C1 O3 Ni1 140.25(18) . 2 ?
C6 O4 Ni1 133.21(18) . 4_565 ?
O3 C1 O2 122.4(3) . . ?
O3 C1 C2 120.6(2) . . ?
O2 C1 C2 116.9(2) . . ?
C1 C2 C3 114.4(2) . . ?
C4 C3 C2 113.0(2) . . ?
C3 C4 C5 113.1(2) . . ?
C6 C5 C4 112.8(2) . . ?
O5 C6 O4 124.7(3) . . ?
O5 C6 C5 118.3(3) . . ?
O4 C6 C5 116.9(2) . . ?
C7A N1A C8A 116.6(11) . . ?
C7A N1A Ni1 122.5(11) . . ?
C8A N1A Ni1 120.8(8) . . ?
N1A C7A C9A 123.7(12) . . ?
N1A C8A C10A 122.9(8) . . ?
C7A C9A C11A 120.1(7) . . ?
C8A C10A C11A 120.5(7) . . ?
C9A C11A C10A 116.0(5) . . ?
C9A C11A C12A 125.0(5) . . ?
C10A C11A C12A 119.0(5) . . ?
C13A C12A C11A 127.0(4) . . ?
C12A C13A C14A 124.6(6) . . ?
C16A C14A C15A 117.2(17) . . ?
C16A C14A C13A 125.4(14) . . ?
C15A C14A C13A 117.2(12) . . ?
C17A C15A C14A 119.7(10) . . ?
C14A C16A C18A 124(2) . . ?
C15A C17A C19A 120.3(6) . . ?
C16A C18A C19A 119.3(11) . . ?
C18A C19A C17A 118.9(5) . . ?
C7B N1B C8B 113.1(17) . . ?
C7B N1B Ni1 125.8(16) . . ?
C8B N1B Ni1 120.8(11) . . ?
N1B C7B C9B 125.3(18) . . ?
N1B C8B C10B 125.7(14) . . ?
C7B C9B C11B 120.6(11) . . ?
C11B C10B C8B 120.5(13) . . ?
C10B C11B C9B 114.1(9) . . ?
C10B C11B C12B 121.7(8) . . ?
C9B C11B C12B 123.9(8) . . ?
C11B C12B C13B 121.7(7) . . ?
C11B C12B C13B 116.1(7) . 3_655 ?
C13B C12B C13B 90.4(6) . 3_655 ?
C14B C13B C12B 122.0(10) . . ?
C14B C13B C12B 112.8(11) . 3_655 ?
C12B C13B C12B 89.6(6) . 3_655 ?
C17B C15B C14B 127.6(17) . . ?
C15B C14B C13B 122.6(16) . . ?
C15B C14B C16B 115(2) . . ?
C13B C14B C16B 122(2) . . ?
C18B C16B C14B 115(3) . . ?
C19B C18B C16B 125.9(19) . . ?
C18B C19B C17B 117.1(11) . . ?
C15B C17B C19B 119.1(12) . . ?
C21 N2 C20 116.8(3) . . ?
C21 N2 Ni1 123.1(2) . . ?
C20 N2 Ni1 120.0(2) . . ?
N2 C20 C22 123.3(3) . . ?
N2 C21 C23 123.8(3) . . ?
C20 C22 C24 120.9(3) . . ?
C21 C23 C24 119.3(3) . . ?
C22 C24 C23 115.9(3) . . ?
C22 C24 C25 124.0(3) . . ?
C23 C24 C25 120.0(3) . . ?
C26 C25 C24 125.0(3) . . ?
C25 C26 C27 127.7(3) . . ?
C28 C27 C29 117.8(3) . . ?
C28 C27 C26 118.9(3) . . ?
C29 C27 C26 123.3(3) . . ?
C30 C28 C27 121.5(3) . . ?
C31 C29 C27 120.2(3) . . ?
C32 C30 C28 119.9(4) . . ?
C29 C31 C32 120.6(4) . . ?
C30 C32 C31 119.9(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H2W O3 0.840(18) 2.38(3) 2.903(3) 121(3) .
O1 H2W O2 0.840(18) 2.00(2) 2.810(3) 161(3) 2
O1 H1W O5 0.894(19) 1.75(2) 2.601(3) 157(4) 4_666

_refine_diff_density_max         0.877
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.115

