# 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_Ni_mononuclear
_database_code_depnum_ccdc_archive 'CCDC 1535434'
_audit_update_record             
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C16 H15 N3 Ni O5'
_chemical_formula_moiety         'C16 H15 N3 Ni O5'
_chemical_formula_weight         388.01
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   6.85643(16)
_cell_length_b                   15.3741(4)
_cell_length_c                   14.9966(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.5363(8)
_cell_angle_gamma                90.0000
_cell_volume                     1573.43(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17210
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.50
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.150
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800.00
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_type   none

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            25006
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_reflns_number_total             3592
_reflns_number_gt                3229
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0973
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3592
_refine_ls_number_parameters     226
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0435P)²+1.8335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.32187(4) 0.431592(17) 0.541930(17) 0.01305(10) Uani 1.0 4 d . . .
O1 O 0.3080(3) 0.43917(9) 0.42072(10) 0.0146(3) Uani 1.0 4 d . . .
O2 O 0.4989(3) 0.18473(10) 0.50552(11) 0.0189(4) Uani 1.0 4 d . . .
O3 O 0.2525(3) 0.47514(10) 0.25176(10) 0.0187(4) Uani 1.0 4 d . . .
O4 O -0.1674(3) 0.09844(12) 0.45455(13) 0.0309(5) Uani 1.0 4 d . . .
O5 O -0.1996(3) -0.08083(12) 0.44011(13) 0.0313(5) Uani 1.0 4 d . . .
N1 N 0.4132(3) 0.31939(12) 0.55261(12) 0.0151(4) Uani 1.0 4 d . . .
N2 N 0.3341(3) 0.43267(12) 0.66443(12) 0.0158(4) Uani 1.0 4 d . . .
N3 N 0.2125(3) 0.54461(12) 0.55344(12) 0.0141(4) Uani 1.0 4 d . . .
C1 C 0.3559(3) 0.37636(14) 0.36689(14) 0.0145(4) Uani 1.0 4 d . . .
C2 C 0.3292(3) 0.39429(14) 0.27301(14) 0.0158(5) Uani 1.0 4 d . . .
C3 C 0.3742(4) 0.33343(15) 0.21022(14) 0.0175(5) Uani 1.0 4 d . . .
C4 C 0.4461(4) 0.25147(15) 0.23887(15) 0.0184(5) Uani 1.0 4 d . . .
C5 C 0.4708(3) 0.23246(14) 0.32855(15) 0.0167(5) Uani 1.0 4 d . . .
C6 C 0.4258(3) 0.29319(14) 0.39364(14) 0.0144(4) Uani 1.0 4 d . . .
C7 C 0.4492(3) 0.26349(14) 0.48847(14) 0.0154(5) Uani 1.0 4 d . . .
C8 C 0.4187(4) 0.28323(14) 0.64411(14) 0.0176(5) Uani 1.0 4 d . . .
C9 C 0.4358(4) 0.35894(15) 0.70982(15) 0.0200(5) Uani 1.0 4 d . . .
C10 C 0.2669(4) 0.49918(15) 0.70286(14) 0.0177(5) Uani 1.0 4 d . . .
C11 C 0.1921(3) 0.56683(14) 0.64044(14) 0.0160(5) Uani 1.0 4 d . . .
C12 C 0.1144(3) 0.64541(15) 0.66380(15) 0.0175(5) Uani 1.0 4 d . . .
C13 C 0.0575(3) 0.70459(14) 0.59623(15) 0.0179(5) Uani 1.0 4 d . . .
C14 C 0.0794(3) 0.68270(14) 0.50800(15) 0.0169(5) Uani 1.0 4 d . . .
C15 C 0.1571(3) 0.60171(14) 0.48875(14) 0.0154(4) Uani 1.0 4 d . . .
C16 C 0.2230(4) 0.49578(16) 0.15822(15) 0.0260(6) Uani 1.0 4 d . . .
H3 H 0.3565 0.3469 0.1482 0.0211 Uiso 1.0 4 calc R . .
H4 H 0.4776 0.2093 0.1962 0.0220 Uiso 1.0 4 calc R . .
H5 H 0.5196 0.1769 0.3472 0.0200 Uiso 1.0 4 calc R . .
H8A H 0.2977 0.2497 0.6509 0.0211 Uiso 1.0 4 calc R . .
H8B H 0.5324 0.2438 0.6558 0.0211 Uiso 1.0 4 calc R . .
H9A H 0.5752 0.3734 0.7265 0.0240 Uiso 1.0 4 calc R . .
H9B H 0.3745 0.3438 0.7649 0.0240 Uiso 1.0 4 calc R . .
H10 H 0.2658 0.5040 0.7660 0.0213 Uiso 1.0 4 calc R . .
H12 H 0.1002 0.6588 0.7247 0.0210 Uiso 1.0 4 calc R . .
H13 H 0.0042 0.7594 0.6103 0.0215 Uiso 1.0 4 calc R . .
H14 H 0.0418 0.7226 0.4610 0.0202 Uiso 1.0 4 calc R . .
H15 H 0.1709 0.5868 0.4282 0.0184 Uiso 1.0 4 calc R . .
H16A H 0.3353 0.4752 0.1283 0.0312 Uiso 1.0 4 calc R . .
H16B H 0.1034 0.4673 0.1316 0.0312 Uiso 1.0 4 calc R . .
H16C H 0.2102 0.5589 0.1508 0.0312 Uiso 1.0 4 calc R . .



#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_molecular_graphics    'CrystalStructure 4.0'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni1 O1 1.8148(16) yes . .
Ni1 N1 1.8370(19) yes . .
Ni1 N2 1.8310(19) yes . .
Ni1 N3 1.9069(19) yes . .
O1 C1 1.320(3) yes . .
O2 C7 1.277(3) yes . .
O3 C2 1.375(3) yes . .
O3 C16 1.433(3) yes . .
N1 C7 1.331(3) yes . .
N1 C8 1.478(3) yes . .
N2 C9 1.464(3) yes . .
N2 C10 1.281(3) yes . .
N3 C11 1.369(3) yes . .
N3 C15 1.336(3) yes . .
C1 C2 1.429(3) yes . .
C1 C6 1.410(3) yes . .
C2 C3 1.383(4) yes . .
C3 C4 1.405(4) yes . .
C4 C5 1.371(4) yes . .
C5 C6 1.406(3) yes . .
C6 C7 1.488(3) yes . .
C8 C9 1.522(4) yes . .
C10 C11 1.459(3) yes . .
C11 C12 1.379(4) yes . .
C12 C13 1.389(3) yes . .
C13 C14 1.387(4) yes . .
C14 C15 1.395(3) yes . .
C3 H3 0.950 no . .
C4 H4 0.950 no . .
C5 H5 0.950 no . .
C8 H8A 0.990 no . .
C8 H8B 0.990 no . .
C9 H9A 0.990 no . .
C9 H9B 0.990 no . .
C10 H10 0.950 no . .
C12 H12 0.950 no . .
C13 H13 0.950 no . .
C14 H14 0.950 no . .
C15 H15 0.950 no . .
C16 H16A 0.980 no . .
C16 H16B 0.980 no . .
C16 H16C 0.980 no . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O1 Ni1 N1 97.59(8) yes . . .
O1 Ni1 N2 175.78(8) yes . . .
O1 Ni1 N3 92.82(7) yes . . .
N1 Ni1 N2 86.49(9) yes . . .
N1 Ni1 N3 168.98(9) yes . . .
N2 Ni1 N3 83.18(8) yes . . .
Ni1 O1 C1 124.99(13) yes . . .
C2 O3 C16 116.21(18) yes . . .
Ni1 N1 C7 128.97(15) yes . . .
Ni1 N1 C8 114.34(14) yes . . .
C7 N1 C8 116.00(18) yes . . .
Ni1 N2 C9 115.67(15) yes . . .
Ni1 N2 C10 118.35(15) yes . . .
C9 N2 C10 125.79(19) yes . . .
Ni1 N3 C11 113.02(14) yes . . .
Ni1 N3 C15 128.30(16) yes . . .
C11 N3 C15 118.69(19) yes . . .
O1 C1 C2 116.46(19) yes . . .
O1 C1 C6 125.94(19) yes . . .
C2 C1 C6 117.6(2) yes . . .
O3 C2 C1 114.36(19) yes . . .
O3 C2 C3 123.99(19) yes . . .
C1 C2 C3 121.6(2) yes . . .
C2 C3 C4 119.5(2) yes . . .
C3 C4 C5 119.8(2) yes . . .
C4 C5 C6 121.7(2) yes . . .
C1 C6 C5 119.7(2) yes . . .
C1 C6 C7 123.6(2) yes . . .
C5 C6 C7 116.68(19) yes . . .
O2 C7 N1 122.2(2) yes . . .
O2 C7 C6 118.99(19) yes . . .
N1 C7 C6 118.84(19) yes . . .
N1 C8 C9 107.88(18) yes . . .
N2 C9 C8 106.72(17) yes . . .
N2 C10 C11 113.57(19) yes . . .
N3 C11 C10 111.82(19) yes . . .
N3 C11 C12 122.6(2) yes . . .
C10 C11 C12 125.6(2) yes . . .
C11 C12 C13 118.5(2) yes . . .
C12 C13 C14 119.2(2) yes . . .
C13 C14 C15 119.5(2) yes . . .
N3 C15 C14 121.6(2) yes . . .
C2 C3 H3 120.230 no . . .
C4 C3 H3 120.223 no . . .
C3 C4 H4 120.072 no . . .
C5 C4 H4 120.081 no . . .
C4 C5 H5 119.167 no . . .
C6 C5 H5 119.180 no . . .
N1 C8 H8A 110.128 no . . .
N1 C8 H8B 110.124 no . . .
C9 C8 H8A 110.139 no . . .
C9 C8 H8B 110.135 no . . .
H8A C8 H8B 108.441 no . . .
N2 C9 H9A 110.379 no . . .
N2 C9 H9B 110.380 no . . .
C8 C9 H9A 110.382 no . . .
C8 C9 H9B 110.382 no . . .
H9A C9 H9B 108.601 no . . .
N2 C10 H10 123.221 no . . .
C11 C10 H10 123.212 no . . .
C11 C12 H12 120.763 no . . .
C13 C12 H12 120.775 no . . .
C12 C13 H13 120.386 no . . .
C14 C13 H13 120.402 no . . .
C13 C14 H14 120.250 no . . .
C15 C14 H14 120.255 no . . .
N3 C15 H15 119.208 no . . .
C14 C15 H15 119.219 no . . .
O3 C16 H16A 109.479 no . . .
O3 C16 H16B 109.472 no . . .
O3 C16 H16C 109.470 no . . .
H16A C16 H16B 109.467 no . . .
H16A C16 H16C 109.470 no . . .
H16B C16 H16C 109.470 no . . .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 Ni1 N1 C7 -1.82(16) no . . . .
O1 Ni1 N1 C8 -171.88(11) no . . . .
N1 Ni1 O1 C1 -0.18(14) no . . . .
O1 Ni1 N3 C11 179.02(11) no . . . .
O1 Ni1 N3 C15 -1.23(15) no . . . .
N3 Ni1 O1 C1 -176.55(13) no . . . .
N1 Ni1 N2 C9 10.57(12) no . . . .
N1 Ni1 N2 C10 -174.14(14) no . . . .
N2 Ni1 N1 C7 179.25(16) no . . . .
N2 Ni1 N1 C8 9.20(12) no . . . .
N2 Ni1 N3 C11 -2.32(12) no . . . .
N2 Ni1 N3 C15 177.43(16) no . . . .
N3 Ni1 N2 C9 -173.28(13) no . . . .
N3 Ni1 N2 C10 2.01(13) no . . . .
Ni1 O1 C1 C2 178.23(11) no . . . .
Ni1 O1 C1 C6 -0.1(3) no . . . .
C16 O3 C2 C1 -179.91(17) no . . . .
C16 O3 C2 C3 -1.2(3) no . . . .
Ni1 N1 C7 O2 -174.60(13) no . . . .
Ni1 N1 C7 C6 3.8(3) no . . . .
Ni1 N1 C8 C9 -25.32(19) no . . . .
C7 N1 C8 C9 163.28(16) no . . . .
C8 N1 C7 O2 -4.7(3) no . . . .
C8 N1 C7 C6 173.71(15) no . . . .
Ni1 N2 C9 C8 -26.2(2) no . . . .
Ni1 N2 C10 C11 -1.2(3) no . . . .
C9 N2 C10 C11 173.53(18) no . . . .
C10 N2 C9 C8 158.9(2) no . . . .
Ni1 N3 C11 C10 2.2(2) no . . . .
Ni1 N3 C11 C12 -179.45(13) no . . . .
Ni1 N3 C15 C14 -179.80(12) no . . . .
C11 N3 C15 C14 -0.1(3) no . . . .
C15 N3 C11 C10 -177.53(16) no . . . .
C15 N3 C11 C12 0.8(3) no . . . .
O1 C1 C2 O3 -1.2(3) no . . . .
O1 C1 C2 C3 -179.95(16) no . . . .
O1 C1 C6 C5 179.88(17) no . . . .
O1 C1 C6 C7 2.1(4) no . . . .
C2 C1 C6 C5 1.6(3) no . . . .
C2 C1 C6 C7 -176.19(17) no . . . .
C6 C1 C2 O3 177.21(17) no . . . .
C6 C1 C2 C3 -1.5(3) no . . . .
O3 C2 C3 C4 -177.93(17) no . . . .
C1 C2 C3 C4 0.7(3) no . . . .
C2 C3 C4 C5 0.1(4) no . . . .
C3 C4 C5 C6 0.0(4) no . . . .
C4 C5 C6 C1 -0.9(3) no . . . .
C4 C5 C6 C7 177.02(18) no . . . .
C1 C6 C7 O2 174.55(18) no . . . .
C1 C6 C7 N1 -3.9(3) no . . . .
C5 C6 C7 O2 -3.3(3) no . . . .
C5 C6 C7 N1 178.27(17) no . . . .
N1 C8 C9 N2 31.2(3) no . . . .
N2 C10 C11 N3 -0.7(3) no . . . .
N2 C10 C11 C12 -178.98(18) no . . . .
N3 C11 C12 C13 -0.9(3) no . . . .
C10 C11 C12 C13 177.15(18) no . . . .
C11 C12 C13 C14 0.4(3) no . . . .
C12 C13 C14 C15 0.3(3) no . . . .
C13 C14 C15 N3 -0.5(3) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
Ni1 C6 3.207(3) no . .
O1 O3 2.586(2) no . .
O1 C7 3.012(3) no . .
O1 C15 2.926(3) no . .
O2 C5 2.742(3) no . .
O2 C8 2.671(3) no . .
N1 C1 2.910(3) no . .
N3 C13 2.779(3) no . .
C1 C4 2.826(4) no . .
C2 C5 2.770(3) no . .
C3 C6 2.808(3) no . .
C3 C16 2.785(4) no . .
C10 C15 3.591(3) no . .
C11 C14 2.724(3) no . .
C12 C15 2.753(4) no . .
Ni1 Ni1 3.5448(4) no . 3_666
Ni1 O1 3.2290(15) no . 3_666
Ni1 C14 3.289(2) no . 3_566
Ni1 C15 3.312(2) no . 3_566
O1 Ni1 3.2290(15) no . 3_666
O1 N2 3.484(3) no . 3_666
O1 N3 3.282(3) no . 3_666
O1 C11 3.464(3) no . 3_566
O1 C12 3.314(3) no . 3_566
O1 C13 3.333(3) no . 3_566
O1 C14 3.501(3) no . 3_566
O2 O4 2.813(3) no . 1_655
O2 O5 2.784(3) no . 3_556
O2 C14 3.559(3) no . 3_666
O3 N2 3.307(3) no . 3_666
O3 C9 3.342(3) no . 3_666
O3 C10 3.324(3) no . 3_666
O3 C12 3.462(3) no . 3_566
O4 O2 2.813(3) no . 1_455
O4 O5 2.772(3) no . .
O4 O5 2.852(3) no . 3_556
O4 C13 3.229(3) no . 3_566
O4 C14 3.455(3) no . 3_566
O4 C16 3.526(3) no . 4_455
O5 O2 2.784(3) no . 3_556
O5 O4 2.772(3) no . .
O5 O4 2.852(3) no . 3_556
O5 C3 3.574(3) no . 2_545
O5 C7 3.509(3) no . 3_556
N1 C14 3.412(3) no . 3_566
N1 C15 3.300(3) no . 3_666
N2 O1 3.484(3) no . 3_666
N2 O3 3.307(3) no . 3_666
N2 C2 3.587(3) no . 3_666
N3 O1 3.282(3) no . 3_666
N3 N3 3.470(3) no . 3_566
N3 C1 3.313(3) no . 3_666
N3 C6 3.552(3) no . 3_666
N3 C15 3.402(3) no . 3_566
C1 N3 3.313(3) no . 3_666
C1 C10 3.459(3) no . 3_666
C1 C11 3.232(3) no . 3_666
C1 C12 3.231(3) no . 3_566
C1 C13 3.193(3) no . 3_566
C2 N2 3.587(3) no . 3_666
C2 C10 3.208(3) no . 3_666
C2 C11 3.463(3) no . 3_666
C2 C12 3.329(3) no . 3_566
C3 O5 3.574(3) no . 2_555
C4 C12 3.588(3) no . 3_666
C5 C12 3.400(3) no . 3_666
C5 C13 3.459(3) no . 3_666
C6 N3 3.552(3) no . 3_666
C6 C11 3.467(3) no . 3_666
C6 C12 3.478(3) no . 3_666
C6 C13 3.332(3) no . 3_566
C6 C13 3.532(3) no . 3_666
C6 C14 3.586(3) no . 3_666
C6 C15 3.596(3) no . 3_666
C7 O5 3.509(3) no . 3_556
C7 C14 3.332(3) no . 3_666
C7 C15 3.394(3) no . 3_666
C9 O3 3.342(3) no . 3_666
C10 O3 3.324(3) no . 3_666
C10 C1 3.459(3) no . 3_666
C10 C2 3.208(3) no . 3_666
C11 O1 3.464(3) no . 3_566
C11 C1 3.232(3) no . 3_666
C11 C2 3.463(3) no . 3_666
C11 C6 3.467(3) no . 3_666
C12 O1 3.314(3) no . 3_566
C12 O3 3.462(3) no . 3_566
C12 C1 3.231(3) no . 3_566
C12 C2 3.329(3) no . 3_566
C12 C4 3.588(3) no . 3_666
C12 C5 3.400(3) no . 3_666
C12 C6 3.478(3) no . 3_666
C13 O1 3.333(3) no . 3_566
C13 O4 3.229(3) no . 3_566
C13 C1 3.193(3) no . 3_566
C13 C5 3.459(3) no . 3_666
C13 C6 3.332(3) no . 3_566
C13 C6 3.532(3) no . 3_666
C14 Ni1 3.289(2) no . 3_566
C14 O1 3.501(3) no . 3_566
C14 O2 3.559(3) no . 3_666
C14 O4 3.455(3) no . 3_566
C14 N1 3.412(3) no . 3_566
C14 C6 3.586(3) no . 3_666
C14 C7 3.332(3) no . 3_666
C15 Ni1 3.312(2) no . 3_566
C15 N1 3.300(3) no . 3_666
C15 N3 3.402(3) no . 3_566
C15 C6 3.596(3) no . 3_666
C15 C7 3.394(3) no . 3_666
C16 O4 3.526(3) no . 4_554
Ni1 H8A 3.2503 no . .
Ni1 H8B 3.5866 no . .
Ni1 H9A 3.2485 no . .
Ni1 H9B 3.5915 no . .
Ni1 H10 3.5950 no . .
Ni1 H15 3.0552 no . .
O1 H15 2.4636 no . .
O2 H5 2.3952 no . .
O2 H8A 2.8693 no . .
O2 H8B 2.4196 no . .
O3 H3 2.6498 no . .
O3 H15 3.2477 no . .
N1 H9A 2.8581 no . .
N1 H9B 3.2420 no . .
N2 H8A 2.8290 no . .
N2 H8B 3.2149 no . .
N3 H10 3.2338 no . .
N3 H12 3.2633 no . .
N3 H14 3.2343 no . .
C1 H3 3.3118 no . .
C1 H5 3.2889 no . .
C2 H4 3.2670 no . .
C2 H16A 2.5050 no . .
C2 H16B 2.7426 no . .
C2 H16C 3.1847 no . .
C3 H5 3.2577 no . .
C3 H16A 2.5035 no . .
C3 H16B 2.9415 no . .
C5 H3 3.2591 no . .
C6 H4 3.2802 no . .
C7 H5 2.5869 no . .
C7 H8A 2.7464 no . .
C7 H8B 2.5372 no . .
C9 H10 2.6888 no . .
C10 H9A 2.8613 no . .
C10 H9B 2.6425 no . .
C10 H12 2.7394 no . .
C11 H13 3.2427 no . .
C11 H15 3.1870 no . .
C12 H10 2.8009 no . .
C12 H14 3.2569 no . .
C13 H15 3.2575 no . .
C14 H12 3.2596 no . .
C15 H13 3.2659 no . .
C16 H3 2.4746 no . .
H3 H4 2.3595 no . .
H3 H16A 1.9975 no . .
H3 H16B 2.5332 no . .
H3 H16C 3.4111 no . .
H4 H5 2.3099 no . .
H8A H9A 2.8476 no . .
H8A H9B 2.2628 no . .
H8B H9A 2.2645 no . .
H8B H9B 2.5610 no . .
H9A H10 3.0198 no . .
H9B H10 2.5732 no . .
H10 H12 2.6831 no . .
H12 H13 2.3561 no . .
H13 H14 2.3468 no . .
H14 H15 2.3379 no . .
Ni1 H14 3.4370 no . 3_566
Ni1 H15 3.4624 no . 3_566
Ni1 H15 3.4749 no . 3_666
O2 H3 3.1324 no . 4_555
O2 H14 3.4491 no . 3_666
O2 H16B 3.0483 no . 4_555
O2 H16C 3.2624 no . 2_545
O3 H9A 2.6165 no . 3_666
O3 H10 3.5525 no . 3_566
O3 H10 3.3542 no . 3_666
O3 H12 3.2214 no . 3_566
O4 H3 3.0116 no . 4_455
O4 H5 2.8255 no . 1_455
O4 H9B 3.0195 no . 4_454
O4 H10 3.2307 no . 4_454
O4 H13 2.6805 no . 3_566
O4 H14 3.1158 no . 3_566
O4 H16A 3.2963 no . 2_545
O4 H16A 2.8397 no . 4_455
O4 H16B 3.3685 no . 4_455
O5 H3 3.0199 no . 2_545
O5 H8A 2.9799 no . 3_556
O5 H8B 3.5937 no . 3_556
O5 H10 2.8552 no . 4_454
O5 H12 3.5918 no . 4_454
O5 H14 3.4461 no . 1_545
O5 H16A 2.9206 no . 2_545
O5 H16A 3.2450 no . 4_455
O5 H16B 2.9654 no . 2_445
O5 H16C 3.2946 no . 4_455
N1 H14 3.1730 no . 3_566
N1 H15 3.1834 no . 3_666
N2 H4 3.3458 no . 4_455
N3 H15 3.3478 no . 3_566
C1 H12 3.3362 no . 3_566
C1 H13 3.2762 no . 3_566
C2 H8B 3.3234 no . 4_454
C2 H10 3.2880 no . 3_666
C2 H12 3.0587 no . 3_566
C3 H8A 3.3704 no . 4_554
C3 H8B 2.6825 no . 4_454
C3 H10 3.5069 no . 3_666
C3 H12 3.4871 no . 3_566
C3 H14 3.1813 no . 2_545
C4 H8A 2.8579 no . 4_554
C4 H8B 2.9870 no . 4_454
C4 H9A 3.1779 no . 4_454
C4 H9B 3.2716 no . 4_554
C4 H12 3.3986 no . 3_666
C4 H14 3.0400 no . 2_545
C4 H15 3.5975 no . 2_545
C5 H9A 3.3983 no . 4_454
C5 H9B 3.2335 no . 4_554
C5 H12 3.5407 no . 3_666
C5 H13 3.4701 no . 3_566
C5 H16C 2.9715 no . 2_545
C6 H13 3.0521 no . 3_566
C7 H13 3.3309 no . 3_566
C7 H14 3.5277 no . 3_566
C7 H14 3.5055 no . 3_666
C8 H4 3.1982 no . 4_455
C8 H12 2.7567 no . 2_546
C8 H14 3.3917 no . 3_566
C9 H4 3.3002 no . 4_455
C9 H12 3.2470 no . 2_546
C9 H13 3.0944 no . 2_546
C9 H16C 3.2982 no . 3_666
C10 H16A 3.5599 no . 3_666
C11 H15 3.5125 no . 3_566
C12 H8A 3.2153 no . 2_556
C12 H8B 3.3384 no . 2_556
C12 H9B 3.2308 no . 2_556
C13 H5 3.4603 no . 3_666
C13 H9B 2.9915 no . 2_556
C14 H3 3.5002 no . 2_555
C14 H4 3.0766 no . 2_555
C14 H8A 3.5001 no . 3_566
C15 H4 3.2844 no . 2_555
C16 H5 3.2402 no . 2_555
C16 H9A 2.9123 no . 3_666
C16 H10 3.5788 no . 3_666
H3 O2 3.1324 no . 4_454
H3 O4 3.0116 no . 4_554
H3 O5 3.0199 no . 2_555
H3 C14 3.5002 no . 2_545
H3 H8A 3.3672 no . 4_554
H3 H8B 2.6353 no . 4_454
H3 H14 2.6544 no . 2_545
H4 N2 3.3458 no . 4_554
H4 C8 3.1982 no . 4_554
H4 C9 3.3002 no . 4_554
H4 C14 3.0766 no . 2_545
H4 C15 3.2844 no . 2_545
H4 H8A 2.4422 no . 4_554
H4 H8B 3.1378 no . 4_454
H4 H9A 3.1113 no . 4_454
H4 H9B 2.9318 no . 4_554
H4 H14 2.3576 no . 2_545
H4 H15 2.7744 no . 2_545
H4 H16C 3.5837 no . 2_545
H5 O4 2.8255 no . 1_655
H5 C13 3.4603 no . 3_666
H5 C16 3.2402 no . 2_545
H5 H9A 3.4776 no . 4_454
H5 H9B 2.8502 no . 4_554
H5 H10 3.5301 no . 4_554
H5 H13 3.4094 no . 3_666
H5 H16B 3.3529 no . 2_545
H5 H16C 2.4045 no . 2_545
H8A O5 2.9799 no . 3_556
H8A C3 3.3704 no . 4_455
H8A C4 2.8579 no . 4_455
H8A C12 3.2153 no . 2_546
H8A C14 3.5001 no . 3_566
H8A H3 3.3672 no . 4_455
H8A H4 2.4422 no . 4_455
H8A H12 2.3827 no . 2_546
H8A H14 2.7681 no . 3_566
H8B O5 3.5937 no . 3_556
H8B C2 3.3234 no . 4_555
H8B C3 2.6825 no . 4_555
H8B C4 2.9870 no . 4_555
H8B C12 3.3384 no . 2_546
H8B H3 2.6353 no . 4_555
H8B H4 3.1378 no . 4_555
H8B H12 2.4620 no . 2_546
H8B H13 3.5492 no . 2_546
H8B H14 3.5847 no . 3_666
H8B H16B 3.3066 no . 4_555
H9A O3 2.6165 no . 3_666
H9A C4 3.1779 no . 4_555
H9A C5 3.3983 no . 4_555
H9A C16 2.9123 no . 3_666
H9A H4 3.1113 no . 4_555
H9A H5 3.4776 no . 4_555
H9A H13 3.1010 no . 2_546
H9A H15 3.0933 no . 3_666
H9A H16A 3.2047 no . 3_666
H9A H16C 2.4716 no . 3_666
H9B O4 3.0195 no . 4_555
H9B C4 3.2716 no . 4_455
H9B C5 3.2335 no . 4_455
H9B C12 3.2308 no . 2_546
H9B C13 2.9915 no . 2_546
H9B H4 2.9318 no . 4_455
H9B H5 2.8502 no . 4_455
H9B H12 2.8536 no . 2_546
H9B H13 2.3621 no . 2_546
H9B H16C 3.3541 no . 3_666
H10 O3 3.5525 no . 3_566
H10 O3 3.3542 no . 3_666
H10 O4 3.2307 no . 4_555
H10 O5 2.8552 no . 4_555
H10 C2 3.2880 no . 3_666
H10 C3 3.5069 no . 3_666
H10 C16 3.5788 no . 3_666
H10 H5 3.5301 no . 4_455
H10 H16A 3.0428 no . 3_666
H10 H16B 3.1163 no . 3_566
H12 O3 3.2214 no . 3_566
H12 O5 3.5918 no . 4_555
H12 C1 3.3362 no . 3_566
H12 C2 3.0587 no . 3_566
H12 C3 3.4871 no . 3_566
H12 C4 3.3986 no . 3_666
H12 C5 3.5407 no . 3_666
H12 C8 2.7567 no . 2_556
H12 C9 3.2470 no . 2_556
H12 H8A 2.3827 no . 2_556
H12 H8B 2.4620 no . 2_556
H12 H9B 2.8536 no . 2_556
H12 H16B 3.3065 no . 3_566
H13 O4 2.6805 no . 3_566
H13 C1 3.2762 no . 3_566
H13 C5 3.4701 no . 3_566
H13 C6 3.0521 no . 3_566
H13 C7 3.3309 no . 3_566
H13 C9 3.0944 no . 2_556
H13 H5 3.4094 no . 3_666
H13 H8B 3.5492 no . 2_556
H13 H9A 3.1010 no . 2_556
H13 H9B 2.3621 no . 2_556
H13 H16C 3.5317 no . 4_465
H14 Ni1 3.4370 no . 3_566
H14 O2 3.4491 no . 3_666
H14 O4 3.1158 no . 3_566
H14 O5 3.4461 no . 1_565
H14 N1 3.1730 no . 3_566
H14 C3 3.1813 no . 2_555
H14 C4 3.0400 no . 2_555
H14 C7 3.5277 no . 3_566
H14 C7 3.5055 no . 3_666
H14 C8 3.3917 no . 3_566
H14 H3 2.6544 no . 2_555
H14 H4 2.3576 no . 2_555
H14 H8A 2.7681 no . 3_566
H14 H8B 3.5847 no . 3_666
H15 Ni1 3.4624 no . 3_566
H15 Ni1 3.4749 no . 3_666
H15 N1 3.1834 no . 3_666
H15 N3 3.3478 no . 3_566
H15 C4 3.5975 no . 2_555
H15 C11 3.5125 no . 3_566
H15 H4 2.7744 no . 2_555
H15 H9A 3.0933 no . 3_666
H16A O4 3.2963 no . 2_555
H16A O4 2.8397 no . 4_554
H16A O5 2.9206 no . 2_555
H16A O5 3.2450 no . 4_554
H16A C10 3.5599 no . 3_666
H16A H9A 3.2047 no . 3_666
H16A H10 3.0428 no . 3_666
H16B O2 3.0483 no . 4_454
H16B O4 3.3685 no . 4_554
H16B O5 2.9654 no . 2_455
H16B H5 3.3529 no . 2_555
H16B H8B 3.3066 no . 4_454
H16B H10 3.1163 no . 3_566
H16B H12 3.3065 no . 3_566
H16C O2 3.2624 no . 2_555
H16C O5 3.2946 no . 4_554
H16C C5 2.9715 no . 2_555
H16C C9 3.2982 no . 3_666
H16C H4 3.5837 no . 2_555
H16C H5 2.4045 no . 2_555
H16C H9A 2.4716 no . 3_666
H16C H9B 3.3541 no . 3_666
H16C H13 3.5317 no . 4_564

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# 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_Ni4
_database_code_depnum_ccdc_archive 'CCDC 1548883'
_audit_update_record             
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_audit_creation_date             2016-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H80 Ni4 O24'
_chemical_formula_sum            'C68 H80 Ni4 O24'
_chemical_formula_weight         1516.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P21/n
_space_group_name_Hall           '-P 2yn'
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                   16.105(3)
_cell_length_b                   25.712(5)
_cell_length_c                   16.804(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.54(3)
_cell_angle_gamma                90
_cell_volume                     6952(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.449
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            112825
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.449
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.938
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71074
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10951
_reflns_number_total             14970
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'shelxT (sheldrick, 2015)'
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00513(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         14970
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+9.8500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1263
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O23-H23
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O24-H24
 0.85 with sigma of 0.01
 O22-H22
 0.85 with sigma of 0.01
 C67-H23
 1.891831 with sigma of 0.02
 Ni4-H23
 2.675256 with sigma of 0.02
 C61-H17
 1.882386 with sigma of 0.02
 Ni1-H17
 2.657736 with sigma of 0.02
 C68-H24
 1.888604 with sigma of 0.02
 Ni2-H24
 2.673646 with sigma of 0.02
 C66-H22
 1.851453 with sigma of 0.02
 Ni3-H22
 2.640382 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C24(H24A,H24B), C39(H39A,H39B), C54(H54A,H54B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C49(H49), C50(H50), C51(H51), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C46(H46A,H46B,
 H46C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58505(2) 0.29735(2) 0.46969(2) 0.01722(10) Uani 1 1 d D . . . .
Ni2 Ni 0.70462(2) 0.21407(2) 0.41846(2) 0.01694(10) Uani 1 1 d D . . . .
Ni3 Ni 0.64732(2) 0.29556(2) 0.29660(2) 0.01717(10) Uani 1 1 d D . . . .
Ni4 Ni 0.52010(2) 0.21679(2) 0.35163(2) 0.01712(10) Uani 1 1 d D . . . .
O1 O 0.71507(14) 0.26689(9) 0.70758(13) 0.0237(5) Uani 1 1 d . . . . .
O2 O 0.64424(14) 0.29521(9) 0.57597(13) 0.0214(5) Uani 1 1 d . . . . .
O3 O 0.58354(14) 0.37616(9) 0.47853(13) 0.0224(5) Uani 1 1 d . . . . .
O4 O 0.60240(18) 0.45523(9) 0.52961(14) 0.0332(6) Uani 1 1 d . . . . .
O5 O 0.93895(14) 0.23102(9) 0.28175(14) 0.0232(5) Uani 1 1 d . . . . .
O6 O 0.81145(14) 0.21112(8) 0.36310(13) 0.0205(5) Uani 1 1 d . . . . .
O7 O 0.71027(14) 0.13533(9) 0.42970(13) 0.0225(5) Uani 1 1 d . . . . .
O8 O 0.75415(16) 0.05366(9) 0.41905(15) 0.0308(6) Uani 1 1 d . . . . .
O9 O 0.50622(14) 0.26568(9) 0.06239(13) 0.0244(5) Uani 1 1 d . . . . .
O10 O 0.58822(14) 0.29296(9) 0.18993(13) 0.0210(5) Uani 1 1 d . . . . .
O11 O 0.66280(14) 0.37415(9) 0.28061(13) 0.0216(5) Uani 1 1 d . . . . .
O12 O 0.67780(15) 0.44792(9) 0.21281(14) 0.0279(5) Uani 1 1 d . . . . .
O13 O 0.28021(14) 0.24283(9) 0.48059(15) 0.0267(5) Uani 1 1 d . . . . .
O14 O 0.41322(13) 0.21808(8) 0.40816(13) 0.0202(5) Uani 1 1 d . . . . .
O15 O 0.50951(13) 0.13813(9) 0.34287(13) 0.0215(5) Uani 1 1 d . . . . .
O16 O 0.46030(15) 0.05807(9) 0.35873(15) 0.0274(5) Uani 1 1 d . . . . .
O17 O 0.46664(14) 0.28971(9) 0.51488(14) 0.0243(5) Uani 1 1 d D . . . .
H17 H 0.4325(10) 0.2694(10) 0.4886(18) 0.036 Uiso 1 1 d DR . . . .
O18 O 0.53740(13) 0.29568(8) 0.35538(12) 0.0173(4) Uani 1 1 d . . . . .
O19 O 0.58782(13) 0.21813(8) 0.45913(12) 0.0177(4) Uani 1 1 d . . . . .
O20 O 0.69542(13) 0.29339(8) 0.41094(12) 0.0188(4) Uani 1 1 d . . . . .
O21 O 0.63703(14) 0.21663(8) 0.31075(13) 0.0193(4) Uani 1 1 d . . . . .
O22 O 0.76859(15) 0.28738(10) 0.25876(14) 0.0284(5) Uani 1 1 d D . . . .
H22 H 0.8007(14) 0.2668(13) 0.2864(13) 0.043 Uiso 1 1 d DR . . . .
O23 O 0.46682(14) 0.22733(9) 0.23619(13) 0.0226(5) Uani 1 1 d D . . . .
H23 H 0.4944(17) 0.2475(10) 0.2058(10) 0.034 Uiso 1 1 d DR . . . .
O24 O 0.75806(14) 0.22465(9) 0.53414(13) 0.0227(5) Uani 1 1 d D . . . .
H24 H 0.7336(18) 0.2467(10) 0.5640(10) 0.034 Uiso 1 1 d DR . . . .
C1 C 0.7511(2) 0.24857(14) 0.7814(2) 0.0282(8) Uani 1 1 d . . . . .
H1A H 0.7584 0.2116 0.7787 0.042 Uiso 1 1 calc GR . . . .
H1B H 0.7151 0.2568 0.8236 0.042 Uiso 1 1 calc GR . . . .
H1C H 0.8041 0.2650 0.7915 0.042 Uiso 1 1 calc GR . . . .
C2 C 0.65630(19) 0.33229(13) 0.62651(18) 0.0194(6) Uani 1 1 d . . . . .
C3 C 0.69516(19) 0.31896(12) 0.70225(19) 0.0202(6) Uani 1 1 d . . . . .
C4 C 0.7095(2) 0.35497(13) 0.7614(2) 0.0241(7) Uani 1 1 d . . . . .
H4 H 0.7348 0.3450 0.8098 0.029 Uiso 1 1 calc R . . . .
C5 C 0.6857(2) 0.40725(13) 0.74858(19) 0.0243(7) Uani 1 1 d . . . . .
H5 H 0.6941 0.4315 0.7892 0.029 Uiso 1 1 calc R . . . .
C6 C 0.6505(2) 0.42241(13) 0.67692(19) 0.0236(7) Uani 1 1 d . . . . .
H6 H 0.6360 0.4571 0.6687 0.028 Uiso 1 1 calc R . . . .
C7 C 0.6360(2) 0.38555(12) 0.61468(18) 0.0206(6) Uani 1 1 d . . . . .
C8 C 0.6050(2) 0.40309(12) 0.53644(19) 0.0208(6) Uani 1 1 d . . . . .
C9 C 0.5902(3) 0.47629(15) 0.4502(2) 0.0350(9) Uani 1 1 d . . . . .
H9A H 0.5337 0.4890 0.4422 0.042 Uiso 1 1 calc R . . . .
H9B H 0.5994 0.4495 0.4110 0.042 Uiso 1 1 calc R . . . .
C10 C 0.6513(2) 0.52038(14) 0.4408(2) 0.0302(8) Uani 1 1 d . . . . .
C11 C 0.6412(3) 0.55147(15) 0.3732(2) 0.0354(9) Uani 1 1 d . . . . .
H11 H 0.5956 0.5465 0.3381 0.043 Uiso 1 1 calc R . . . .
C12 C 0.6988(3) 0.58984(15) 0.3579(2) 0.0380(9) Uani 1 1 d . . . . .
H12 H 0.6926 0.6098 0.3119 0.046 Uiso 1 1 calc R . . . .
C13 C 0.7649(3) 0.59849(18) 0.4105(3) 0.0458(11) Uani 1 1 d . . . . .
H13 H 0.8036 0.6242 0.4001 0.055 Uiso 1 1 calc R . . . .
C14 C 0.7739(3) 0.5689(2) 0.4792(3) 0.0578(13) Uani 1 1 d . . . . .
H14 H 0.8181 0.5753 0.5154 0.069 Uiso 1 1 calc R . . . .
C15 C 0.7176(3) 0.52980(19) 0.4943(3) 0.0470(11) Uani 1 1 d . . . . .
H15 H 0.7243 0.5099 0.5403 0.056 Uiso 1 1 calc R . . . .
C16 C 1.0118(2) 0.24420(15) 0.2401(3) 0.0358(9) Uani 1 1 d . . . . .
H16A H 1.0112 0.2259 0.1903 0.054 Uiso 1 1 calc GR . . . .
H16B H 1.0604 0.2346 0.2718 0.054 Uiso 1 1 calc GR . . . .
H16C H 1.0125 0.2810 0.2303 0.054 Uiso 1 1 calc GR . . . .
C17 C 0.85409(19) 0.17080(12) 0.34361(18) 0.0187(6) Uani 1 1 d . . . . .
C18 C 0.9280(2) 0.17987(13) 0.30005(19) 0.0207(6) Uani 1 1 d . . . . .
C19 C 0.9807(2) 0.14013(13) 0.2816(2) 0.0248(7) Uani 1 1 d . . . . .
H19 H 1.0283 0.1472 0.2542 0.030 Uiso 1 1 calc R . . . .
C20 C 0.9630(2) 0.08876(14) 0.3038(2) 0.0275(7) Uani 1 1 d . . . . .
H20 H 0.9996 0.0621 0.2923 0.033 Uiso 1 1 calc R . . . .
C21 C 0.8921(2) 0.07782(13) 0.3424(2) 0.0249(7) Uani 1 1 d . . . . .
H21 H 0.8800 0.0436 0.3554 0.030 Uiso 1 1 calc R . . . .
C22 C 0.8367(2) 0.11806(12) 0.36284(18) 0.0197(6) Uani 1 1 d . . . . .
C23 C 0.7628(2) 0.10533(12) 0.40561(19) 0.0218(6) Uani 1 1 d . . . . .
C24 C 0.6937(2) 0.03950(14) 0.4765(2) 0.0336(9) Uani 1 1 d . . . . .
H24A H 0.6783 0.0033 0.4691 0.040 Uiso 1 1 calc R . . . .
H24B H 0.6441 0.0604 0.4676 0.040 Uiso 1 1 calc R . . . .
C25 C 0.7278(3) 0.04752(14) 0.5604(2) 0.0343(9) Uani 1 1 d . . . . .
C26 C 0.6732(3) 0.05398(16) 0.6215(3) 0.0430(10) Uani 1 1 d . . . . .
H26 H 0.6162 0.0542 0.6098 0.052 Uiso 1 1 calc R . . . .
C27 C 0.7029(3) 0.06008(18) 0.6997(3) 0.0526(12) Uani 1 1 d . . . . .
H27 H 0.6658 0.0639 0.7402 0.063 Uiso 1 1 calc R . . . .
C28 C 0.7874(4) 0.06052(19) 0.7176(3) 0.0541(12) Uani 1 1 d . . . . .
H28 H 0.8072 0.0649 0.7699 0.065 Uiso 1 1 calc R . . . .
C29 C 0.8426(3) 0.05435(19) 0.6572(3) 0.0514(12) Uani 1 1 d . . . . .
H29 H 0.8996 0.0548 0.6691 0.062 Uiso 1 1 calc R . . . .
C30 C 0.8131(3) 0.04759(16) 0.5795(3) 0.0412(10) Uani 1 1 d . . . . .
H30 H 0.8504 0.0430 0.5394 0.049 Uiso 1 1 calc R . . . .
C31 C 0.4659(2) 0.24824(15) -0.0106(2) 0.0305(8) Uani 1 1 d . . . . .
H31A H 0.4994 0.2571 -0.0544 0.046 Uiso 1 1 calc GR . . . .
H31B H 0.4126 0.2647 -0.0174 0.046 Uiso 1 1 calc GR . . . .
H31C H 0.4586 0.2112 -0.0087 0.046 Uiso 1 1 calc GR . . . .
C32 C 0.57100(19) 0.33075(13) 0.14064(18) 0.0210(6) Uani 1 1 d . . . . .
C33 C 0.5251(2) 0.31770(13) 0.06788(19) 0.0226(7) Uani 1 1 d . . . . .
C34 C 0.5046(2) 0.35426(14) 0.0115(2) 0.0271(7) Uani 1 1 d . . . . .
H34 H 0.4741 0.3447 -0.0345 0.033 Uiso 1 1 calc R . . . .
C35 C 0.5296(2) 0.40674(15) 0.0228(2) 0.0303(8) Uani 1 1 d . . . . .
H35 H 0.5158 0.4315 -0.0159 0.036 Uiso 1 1 calc R . . . .
C36 C 0.5737(2) 0.42082(14) 0.0906(2) 0.0277(7) Uani 1 1 d . . . . .
H36 H 0.5898 0.4553 0.0979 0.033 Uiso 1 1 calc R . . . .
C37 C 0.5953(2) 0.38328(13) 0.15014(19) 0.0221(7) Uani 1 1 d . . . . .
C38 C 0.6464(2) 0.39941(12) 0.21985(19) 0.0219(7) Uani 1 1 d . . . . .
C39 C 0.7472(2) 0.46082(14) 0.2665(2) 0.0277(7) Uani 1 1 d . . . . .
H39A H 0.7353 0.4495 0.3199 0.033 Uiso 1 1 calc R . . . .
H39B H 0.7545 0.4983 0.2676 0.033 Uiso 1 1 calc R . . . .
C40 C 0.8265(2) 0.43555(13) 0.2418(2) 0.0263(7) Uani 1 1 d . . . . .
C41 C 0.8386(2) 0.42453(15) 0.1620(2) 0.0330(8) Uani 1 1 d . . . . .
H41 H 0.7965 0.4318 0.1239 0.040 Uiso 1 1 calc R . . . .
C42 C 0.9127(3) 0.40280(17) 0.1385(3) 0.0423(10) Uani 1 1 d . . . . .
H42 H 0.9203 0.3960 0.0850 0.051 Uiso 1 1 calc R . . . .
C43 C 0.9750(3) 0.39143(16) 0.1949(3) 0.0442(10) Uani 1 1 d . . . . .
H43 H 1.0245 0.3768 0.1793 0.053 Uiso 1 1 calc R . . . .
C44 C 0.9642(3) 0.40160(17) 0.2739(3) 0.0429(10) Uani 1 1 d . . . . .
H44 H 1.0064 0.3940 0.3117 0.051 Uiso 1 1 calc R . . . .
C45 C 0.8891(3) 0.42361(16) 0.2977(2) 0.0374(9) Uani 1 1 d . . . . .
H45 H 0.8817 0.4301 0.3513 0.045 Uiso 1 1 calc R . . . .
C46 C 0.1990(2) 0.25882(16) 0.5019(3) 0.0412(10) Uani 1 1 d . . . . .
H46A H 0.1582 0.2443 0.4649 0.062 Uiso 1 1 calc GR . . . .
H46B H 0.1955 0.2961 0.5003 0.062 Uiso 1 1 calc GR . . . .
H46C H 0.1889 0.2468 0.5547 0.062 Uiso 1 1 calc GR . . . .
C47 C 0.3661(2) 0.17919(13) 0.42644(18) 0.0202(6) Uani 1 1 d . . . . .
C48 C 0.2906(2) 0.19075(13) 0.46548(19) 0.0219(7) Uani 1 1 d . . . . .
C49 C 0.2345(2) 0.15234(14) 0.4832(2) 0.0247(7) Uani 1 1 d . . . . .
H49 H 0.1861 0.1609 0.5083 0.030 Uiso 1 1 calc R . . . .
C50 C 0.2503(2) 0.10063(13) 0.4636(2) 0.0252(7) Uani 1 1 d . . . . .
H50 H 0.2117 0.0750 0.4749 0.030 Uiso 1 1 calc R . . . .
C51 C 0.3219(2) 0.08736(13) 0.42806(19) 0.0233(7) Uani 1 1 d . . . . .
H51 H 0.3321 0.0527 0.4159 0.028 Uiso 1 1 calc R . . . .
C52 C 0.3811(2) 0.12624(12) 0.40943(18) 0.0204(6) Uani 1 1 d . . . . .
C53 C 0.4549(2) 0.11018(12) 0.36847(19) 0.0214(6) Uani 1 1 d . . . . .
C54 C 0.5177(2) 0.04046(14) 0.3007(2) 0.0299(8) Uani 1 1 d . . . . .
H54A H 0.5295 0.0038 0.3092 0.036 Uiso 1 1 calc R . . . .
H54B H 0.5695 0.0595 0.3078 0.036 Uiso 1 1 calc R . . . .
C55 C 0.4826(2) 0.04836(14) 0.2172(2) 0.0312(8) Uani 1 1 d . . . . .
C56 C 0.5362(3) 0.05053(17) 0.1541(3) 0.0423(10) Uani 1 1 d . . . . .
H56 H 0.5933 0.0481 0.1641 0.051 Uiso 1 1 calc R . . . .
C57 C 0.5045(3) 0.0563(2) 0.0768(3) 0.0576(13) Uani 1 1 d . . . . .
H57 H 0.5403 0.0566 0.0349 0.069 Uiso 1 1 calc R . . . .
C58 C 0.4200(3) 0.0614(2) 0.0613(3) 0.0579(13) Uani 1 1 d . . . . .
H58 H 0.3992 0.0660 0.0092 0.069 Uiso 1 1 calc R . . . .
C59 C 0.3663(3) 0.05977(19) 0.1228(3) 0.0457(11) Uani 1 1 d . . . . .
H59 H 0.3094 0.0633 0.1123 0.055 Uiso 1 1 calc R . . . .
C60 C 0.3971(2) 0.05281(16) 0.2004(2) 0.0368(9) Uani 1 1 d . . . . .
H60 H 0.3606 0.0511 0.2416 0.044 Uiso 1 1 calc R . . . .
C61 C 0.4170(2) 0.32927(14) 0.5477(2) 0.0304(8) Uani 1 1 d D . . . .
H61A H 0.4493 0.3481 0.5875 0.046 Uiso 1 1 calc GR . . . .
H61B H 0.3699 0.3138 0.5716 0.046 Uiso 1 1 calc GR . . . .
H61C H 0.3981 0.3527 0.5063 0.046 Uiso 1 1 calc GR . . . .
C62 C 0.4716(2) 0.33025(13) 0.33188(19) 0.0238(7) Uani 1 1 d . . . . .
H62A H 0.4221 0.3205 0.3578 0.036 Uiso 1 1 calc GR . . . .
H62B H 0.4618 0.3284 0.2752 0.036 Uiso 1 1 calc GR . . . .
H62C H 0.4868 0.3651 0.3468 0.036 Uiso 1 1 calc GR . . . .
C63 C 0.5653(2) 0.18643(13) 0.52417(19) 0.0213(6) Uani 1 1 d . . . . .
H63A H 0.5983 0.1959 0.5709 0.032 Uiso 1 1 calc GR . . . .
H63B H 0.5749 0.1506 0.5117 0.032 Uiso 1 1 calc GR . . . .
H63C H 0.5075 0.1915 0.5338 0.032 Uiso 1 1 calc GR . . . .
C64 C 0.76203(19) 0.32656(13) 0.43385(19) 0.0221(6) Uani 1 1 d . . . . .
H64A H 0.7473 0.3619 0.4211 0.033 Uiso 1 1 calc GR . . . .
H64B H 0.8104 0.3169 0.4059 0.033 Uiso 1 1 calc GR . . . .
H64C H 0.7737 0.3235 0.4902 0.033 Uiso 1 1 calc GR . . . .
C65 C 0.6560(2) 0.18323(13) 0.24705(19) 0.0212(6) Uani 1 1 d . . . . .
H65A H 0.7141 0.1859 0.2370 0.032 Uiso 1 1 calc GR . . . .
H65B H 0.6237 0.1931 0.2001 0.032 Uiso 1 1 calc GR . . . .
H65C H 0.6431 0.1480 0.2609 0.032 Uiso 1 1 calc GR . . . .
C66 C 0.7973(3) 0.28923(18) 0.1825(2) 0.0431(11) Uani 1 1 d D . . . .
H66A H 0.7637 0.3129 0.1508 0.065 Uiso 1 1 calc GR . . . .
H66B H 0.7940 0.2552 0.1592 0.065 Uiso 1 1 calc GR . . . .
H66C H 0.8540 0.3009 0.1846 0.065 Uiso 1 1 calc GR . . . .
C67 C 0.4270(2) 0.18868(13) 0.1870(2) 0.0268(7) Uani 1 1 d D . . . .
H67A H 0.3962 0.2052 0.1438 0.040 Uiso 1 1 calc GR . . . .
H67B H 0.3898 0.1687 0.2180 0.040 Uiso 1 1 calc GR . . . .
H67C H 0.4682 0.1661 0.1660 0.040 Uiso 1 1 calc GR . . . .
C68 C 0.7934(2) 0.18582(13) 0.5860(2) 0.0262(7) Uani 1 1 d D . . . .
H68A H 0.8289 0.1636 0.5567 0.039 Uiso 1 1 calc GR . . . .
H68B H 0.7498 0.1655 0.6077 0.039 Uiso 1 1 calc GR . . . .
H68C H 0.8253 0.2023 0.6286 0.039 Uiso 1 1 calc GR . . . .


_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 1.988(2) . ?
Ni1 O3 2.032(2) . ?
Ni1 O17 2.093(2) . ?
Ni1 O18 2.037(2) . ?
Ni1 O19 2.045(2) . ?
Ni1 O20 2.074(2) . ?
Ni2 O6 1.993(2) . ?
Ni2 O7 2.035(2) . ?
Ni2 O19 2.032(2) . ?
Ni2 O20 2.048(2) . ?
Ni2 O21 2.071(2) . ?
Ni2 O24 2.108(2) . ?
Ni3 O10 1.993(2) . ?
Ni3 O11 2.055(2) . ?
Ni3 O18 2.065(2) . ?
Ni3 O20 2.040(2) . ?
Ni3 O21 2.051(2) . ?
Ni3 O22 2.091(2) . ?
Ni4 O14 2.003(2) . ?
Ni4 O15 2.034(2) . ?
Ni4 O18 2.048(2) . ?
Ni4 O19 2.069(2) . ?
Ni4 O21 2.033(2) . ?
Ni4 O23 2.104(2) . ?
O1 C1 1.426(4) . ?
O1 C3 1.379(4) . ?
O2 C2 1.286(4) . ?
O3 C8 1.231(4) . ?
O4 C8 1.346(4) . ?
O4 C9 1.445(4) . ?
O5 C16 1.432(4) . ?
O5 C18 1.364(4) . ?
O6 C17 1.294(4) . ?
O7 C23 1.226(4) . ?
O8 C23 1.356(4) . ?
O8 C24 1.447(4) . ?
O9 C31 1.434(4) . ?
O9 C33 1.374(4) . ?
O10 C32 1.299(4) . ?
O11 C38 1.229(4) . ?
O12 C38 1.353(4) . ?
O12 C39 1.444(4) . ?
O13 C46 1.431(4) . ?
O13 C48 1.374(4) . ?
O14 C47 1.301(4) . ?
O15 C53 1.228(4) . ?
O16 C53 1.353(4) . ?
O16 C54 1.445(4) . ?
O17 H17 0.866(9) . ?
O17 C61 1.420(4) . ?
O18 C62 1.425(4) . ?
O19 C63 1.423(3) . ?
O20 C64 1.411(4) . ?
O21 C65 1.416(4) . ?
O22 H22 0.861(9) . ?
O22 C66 1.382(4) . ?
O23 H23 0.864(9) . ?
O23 C67 1.427(4) . ?
O24 H24 0.864(9) . ?
O24 C68 1.427(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.435(4) . ?
C2 C7 1.420(4) . ?
C3 C4 1.371(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.412(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.365(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.423(4) . ?
C7 C8 1.457(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.514(5) . ?
C10 C11 1.393(5) . ?
C10 C15 1.386(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.372(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.384(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.385(6) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.444(4) . ?
C17 C22 1.425(4) . ?
C18 C19 1.372(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.406(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.366(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.419(4) . ?
C22 C23 1.455(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.505(6) . ?
C25 C26 1.392(5) . ?
C25 C30 1.396(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.387(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.380(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.388(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.381(6) . ?
C30 H30 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.440(5) . ?
C32 C37 1.413(5) . ?
C33 C34 1.365(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.418(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.364(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.422(5) . ?
C37 C38 1.461(5) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.507(5) . ?
C40 C41 1.392(5) . ?
C40 C45 1.382(5) . ?
C41 H41 0.9300 . ?
C41 C42 1.391(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.381(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.371(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.409(6) . ?
C45 H45 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.437(4) . ?
C47 C52 1.414(4) . ?
C48 C49 1.380(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.395(5) . ?
C50 H50 0.9300 . ?
C50 C51 1.365(5) . ?
C51 H51 0.9300 . ?
C51 C52 1.426(4) . ?
C52 C53 1.459(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.504(5) . ?
C55 C56 1.398(5) . ?
C55 C60 1.398(5) . ?
C56 H56 0.9300 . ?
C56 C57 1.382(7) . ?
C57 H57 0.9300 . ?
C57 C58 1.381(7) . ?
C58 H58 0.9300 . ?
C58 C59 1.377(6) . ?
C59 H59 0.9300 . ?
C59 C60 1.386(6) . ?
C60 H60 0.9300 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O3 88.21(9) . . ?
O2 Ni1 O17 94.58(10) . . ?
O2 Ni1 O18 172.90(9) . . ?
O2 Ni1 O19 92.24(9) . . ?
O2 Ni1 O20 92.25(9) . . ?
O3 Ni1 O17 93.04(9) . . ?
O3 Ni1 O18 94.86(9) . . ?
O3 Ni1 O19 179.01(9) . . ?
O3 Ni1 O20 95.57(9) . . ?
O18 Ni1 O17 91.65(9) . . ?
O18 Ni1 O19 84.60(9) . . ?
O18 Ni1 O20 81.09(9) . . ?
O19 Ni1 O17 87.81(9) . . ?
O19 Ni1 O20 83.53(8) . . ?
O20 Ni1 O17 169.17(9) . . ?
O6 Ni2 O7 88.26(9) . . ?
O6 Ni2 O19 171.82(9) . . ?
O6 Ni2 O20 94.05(9) . . ?
O6 Ni2 O21 91.40(9) . . ?
O6 Ni2 O24 96.30(9) . . ?
O7 Ni2 O20 177.56(9) . . ?
O7 Ni2 O21 97.61(9) . . ?
O7 Ni2 O24 91.61(9) . . ?
O19 Ni2 O7 93.33(9) . . ?
O19 Ni2 O20 84.50(8) . . ?
O19 Ni2 O21 80.43(9) . . ?
O19 Ni2 O24 91.69(9) . . ?
O20 Ni2 O21 83.14(8) . . ?
O20 Ni2 O24 87.35(9) . . ?
O21 Ni2 O24 168.17(9) . . ?
O10 Ni3 O11 88.35(9) . . ?
O10 Ni3 O18 92.57(9) . . ?
O10 Ni3 O20 172.87(9) . . ?
O10 Ni3 O21 91.90(9) . . ?
O10 Ni3 O22 97.96(10) . . ?
O11 Ni3 O18 99.94(9) . . ?
O11 Ni3 O22 86.49(9) . . ?
O18 Ni3 O22 167.84(9) . . ?
O20 Ni3 O11 96.14(9) . . ?
O20 Ni3 O18 81.22(9) . . ?
O20 Ni3 O21 83.86(9) . . ?
O20 Ni3 O22 87.87(10) . . ?
O21 Ni3 O11 177.47(9) . . ?
O21 Ni3 O18 82.57(8) . . ?
O21 Ni3 O22 90.98(9) . . ?
O14 Ni4 O15 88.84(9) . . ?
O14 Ni4 O18 95.02(9) . . ?
O14 Ni4 O19 90.94(9) . . ?
O14 Ni4 O21 171.40(9) . . ?
O14 Ni4 O23 96.38(9) . . ?
O15 Ni4 O18 176.09(8) . . ?
O15 Ni4 O19 96.84(9) . . ?
O15 Ni4 O23 91.83(9) . . ?
O18 Ni4 O19 83.74(8) . . ?
O18 Ni4 O23 87.14(9) . . ?
O19 Ni4 O23 168.77(9) . . ?
O21 Ni4 O15 92.85(9) . . ?
O21 Ni4 O18 83.43(8) . . ?
O21 Ni4 O19 80.49(9) . . ?
O21 Ni4 O23 91.99(9) . . ?
C3 O1 C1 117.5(3) . . ?
C2 O2 Ni1 128.7(2) . . ?
C8 O3 Ni1 127.9(2) . . ?
C8 O4 C9 117.0(3) . . ?
C18 O5 C16 117.0(3) . . ?
C17 O6 Ni2 128.9(2) . . ?
C23 O7 Ni2 128.6(2) . . ?
C23 O8 C24 115.7(3) . . ?
C33 O9 C31 116.9(3) . . ?
C32 O10 Ni3 128.9(2) . . ?
C38 O11 Ni3 127.3(2) . . ?
C38 O12 C39 116.1(3) . . ?
C48 O13 C46 116.5(3) . . ?
C47 O14 Ni4 128.5(2) . . ?
C53 O15 Ni4 128.0(2) . . ?
C53 O16 C54 116.0(3) . . ?
Ni1 O17 H17 116.1(14) . . ?
C61 O17 Ni1 127.7(2) . . ?
C61 O17 H17 105.9(14) . . ?
Ni1 O18 Ni3 98.97(9) . . ?
Ni1 O18 Ni4 95.45(9) . . ?
Ni4 O18 Ni3 95.86(9) . . ?
C62 O18 Ni1 119.50(18) . . ?
C62 O18 Ni3 120.70(18) . . ?
C62 O18 Ni4 120.73(19) . . ?
Ni1 O19 Ni4 94.57(9) . . ?
Ni2 O19 Ni1 96.00(9) . . ?
Ni2 O19 Ni4 99.53(9) . . ?
C63 O19 Ni1 119.77(18) . . ?
C63 O19 Ni2 119.99(19) . . ?
C63 O19 Ni4 121.25(19) . . ?
Ni2 O20 Ni1 94.63(9) . . ?
Ni3 O20 Ni1 98.59(9) . . ?
Ni3 O20 Ni2 96.24(9) . . ?
C64 O20 Ni1 119.86(18) . . ?
C64 O20 Ni2 122.22(19) . . ?
C64 O20 Ni3 119.52(18) . . ?
Ni3 O21 Ni2 95.21(9) . . ?
Ni4 O21 Ni2 99.41(9) . . ?
Ni4 O21 Ni3 96.78(9) . . ?
C65 O21 Ni2 121.24(19) . . ?
C65 O21 Ni3 119.43(18) . . ?
C65 O21 Ni4 119.37(19) . . ?
Ni3 O22 H22 116.4(14) . . ?
C66 O22 Ni3 129.3(2) . . ?
C66 O22 H22 107.6(14) . . ?
Ni4 O23 H23 115.0(14) . . ?
C67 O23 Ni4 126.8(2) . . ?
C67 O23 H23 107.7(14) . . ?
Ni2 O24 H24 116.2(14) . . ?
C68 O24 Ni2 127.5(2) . . ?
C68 O24 H24 106.5(14) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C3 117.1(3) . . ?
O2 C2 C7 126.5(3) . . ?
C7 C2 C3 116.3(3) . . ?
O1 C3 C2 112.4(3) . . ?
C4 C3 O1 125.3(3) . . ?
C4 C3 C2 122.3(3) . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.5(3) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C6 120.7(3) . . ?
C2 C7 C8 119.5(3) . . ?
C6 C7 C8 119.7(3) . . ?
O3 C8 O4 119.1(3) . . ?
O3 C8 C7 127.7(3) . . ?
O4 C8 C7 113.2(3) . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.3(3) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
C11 C10 C9 117.5(4) . . ?
C15 C10 C9 123.3(3) . . ?
C15 C10 C11 119.2(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.2(4) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.9(4) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.4(5) . . ?
C15 C14 H14 119.8 . . ?
C10 C15 H15 120.0 . . ?
C14 C15 C10 120.0(4) . . ?
C14 C15 H15 120.0 . . ?
O5 C16 H16A 109.5 . . ?
O5 C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C17 C18 117.2(3) . . ?
O6 C17 C22 126.4(3) . . ?
C22 C17 C18 116.3(3) . . ?
O5 C18 C17 112.8(3) . . ?
O5 C18 C19 125.4(3) . . ?
C19 C18 C17 121.8(3) . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.3(3) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(3) . . ?
C22 C21 H21 119.6 . . ?
C17 C22 C23 120.0(3) . . ?
C21 C22 C17 120.5(3) . . ?
C21 C22 C23 119.5(3) . . ?
O7 C23 O8 119.0(3) . . ?
O7 C23 C22 127.8(3) . . ?
O8 C23 C22 113.3(3) . . ?
O8 C24 H24A 109.4 . . ?
O8 C24 H24B 109.4 . . ?
O8 C24 C25 111.2(3) . . ?
H24A C24 H24B 108.0 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 C30 118.6(4) . . ?
C30 C25 C24 122.0(3) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(4) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.9(5) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.1(5) . . ?
C30 C29 H29 120.0 . . ?
C25 C30 H30 119.6 . . ?
C29 C30 C25 120.7(4) . . ?
C29 C30 H30 119.6 . . ?
O9 C31 H31A 109.5 . . ?
O9 C31 H31B 109.5 . . ?
O9 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O10 C32 C33 117.0(3) . . ?
O10 C32 C37 126.4(3) . . ?
C37 C32 C33 116.6(3) . . ?
O9 C33 C32 112.8(3) . . ?
C34 C33 O9 125.3(3) . . ?
C34 C33 C32 121.9(3) . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.2(3) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 119.9(3) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 119.7 . . ?
C35 C36 C37 120.6(3) . . ?
C37 C36 H36 119.7 . . ?
C32 C37 C36 120.7(3) . . ?
C32 C37 C38 120.3(3) . . ?
C36 C37 C38 118.9(3) . . ?
O11 C38 O12 119.5(3) . . ?
O11 C38 C37 127.5(3) . . ?
O12 C38 C37 113.0(3) . . ?
O12 C39 H39A 109.3 . . ?
O12 C39 H39B 109.3 . . ?
O12 C39 C40 111.7(3) . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.3 . . ?
C40 C39 H39B 109.3 . . ?
C41 C40 C39 120.6(3) . . ?
C45 C40 C39 120.7(3) . . ?
C45 C40 C41 118.7(4) . . ?
C40 C41 H41 119.5 . . ?
C40 C41 C42 120.9(4) . . ?
C42 C41 H41 119.5 . . ?
C41 C42 H42 120.1 . . ?
C43 C42 C41 119.8(4) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 H43 119.9 . . ?
C44 C43 C42 120.3(4) . . ?
C44 C43 H43 119.9 . . ?
C43 C44 H44 120.1 . . ?
C43 C44 C45 119.9(4) . . ?
C45 C44 H44 120.1 . . ?
C40 C45 C44 120.4(4) . . ?
C40 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
O13 C46 H46A 109.5 . . ?
O13 C46 H46B 109.5 . . ?
O13 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O14 C47 C48 117.6(3) . . ?
O14 C47 C52 125.8(3) . . ?
C52 C47 C48 116.6(3) . . ?
O13 C48 C47 113.5(3) . . ?
O13 C48 C49 124.8(3) . . ?
C49 C48 C47 121.7(3) . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.2(3) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 119.8 . . ?
C51 C50 C49 120.5(3) . . ?
C51 C50 H50 119.8 . . ?
C50 C51 H51 119.8 . . ?
C50 C51 C52 120.5(3) . . ?
C52 C51 H51 119.8 . . ?
C47 C52 C51 120.5(3) . . ?
C47 C52 C53 121.2(3) . . ?
C51 C52 C53 118.2(3) . . ?
O15 C53 O16 119.1(3) . . ?
O15 C53 C52 127.6(3) . . ?
O16 C53 C52 113.3(3) . . ?
O16 C54 H54A 109.4 . . ?
O16 C54 H54B 109.4 . . ?
O16 C54 C55 111.3(3) . . ?
H54A C54 H54B 108.0 . . ?
C55 C54 H54A 109.4 . . ?
C55 C54 H54B 109.4 . . ?
C56 C55 C54 119.7(4) . . ?
C56 C55 C60 118.6(4) . . ?
C60 C55 C54 121.7(3) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 C55 120.2(4) . . ?
C57 C56 H56 119.9 . . ?
C56 C57 H57 119.7 . . ?
C58 C57 C56 120.5(4) . . ?
C58 C57 H57 119.7 . . ?
C57 C58 H58 119.9 . . ?
C59 C58 C57 120.1(5) . . ?
C59 C58 H58 119.9 . . ?
C58 C59 H59 120.0 . . ?
C58 C59 C60 120.0(4) . . ?
C60 C59 H59 120.0 . . ?
C55 C60 H60 119.7 . . ?
C59 C60 C55 120.6(4) . . ?
C59 C60 H60 119.7 . . ?
O17 C61 H61A 109.5 . . ?
O17 C61 H61B 109.5 . . ?
O17 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O18 C62 H62A 109.5 . . ?
O18 C62 H62B 109.5 . . ?
O18 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O19 C63 H63A 109.5 . . ?
O19 C63 H63B 109.5 . . ?
O19 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O20 C64 H64A 109.5 . . ?
O20 C64 H64B 109.5 . . ?
O20 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O21 C65 H65A 109.5 . . ?
O21 C65 H65B 109.5 . . ?
O21 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O22 C66 H66A 109.5 . . ?
O22 C66 H66B 109.5 . . ?
O22 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O23 C67 H67A 109.5 . . ?
O23 C67 H67B 109.5 . . ?
O23 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O24 C68 H68A 109.5 . . ?
O24 C68 H68B 109.5 . . ?
O24 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ni7
_database_code_depnum_ccdc_archive 'CCDC 1548884'
_audit_update_record             
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_audit_creation_date             2017-06-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C108 H120 N12 Ni7 O24), 2(Cl), 0.25(H2 O)'
_chemical_formula_sum            'C108 H120.50 Cl2 N12 Ni7 O24.25'
_chemical_formula_weight         2456.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   22.615(3)
_cell_length_b                   22.615(3)
_cell_length_c                   22.615(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11566(4)
_cell_formula_units_Z            4.00008
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.478
_cell_measurement_theta_min      2.014
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5106
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            181274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.014
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71074
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3505
_reflns_number_total             4427
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.166
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1256P)²+11.6427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2084
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C12, C17, C16, C15, C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(O4) = Uanis(C18)
4. Others
 Fixed Sof: O1W(0.04167)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.39775(2) 0.50460(2) 0.58978(2) 0.0510(2) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.5000 0.5000 0.0504(3) Uani 1 6 d S T P . .
O1 O 0.32684(12) 0.61758(13) 0.44674(13) 0.0601(7) Uani 1 1 d . . . . .
O2 O 0.35065(12) 0.55304(12) 0.53591(13) 0.0580(7) Uani 1 1 d . . . . .
O3 O 0.32173(12) 0.46131(13) 0.60670(12) 0.0603(7) Uani 1 1 d . . . . .
O4 O 0.43828(15) 0.44234(14) 0.53708(13) 0.0664(7) Uani 1 1 d . . . . .
N1 N 0.22724(16) 0.43979(17) 0.61722(17) 0.0659(9) Uani 1 1 d . . . . .
H1 H 0.1909 0.4453 0.6075 0.079 Uiso 1 1 calc R . . . .
N2 N 0.2715(2) 0.3811(2) 0.76407(18) 0.0761(11) Uani 1 1 d . . . . .
C1 C 0.3167(2) 0.6597(2) 0.4009(2) 0.0694(11) Uani 1 1 d . . . . .
H1A H 0.2909 0.6902 0.4152 0.104 Uiso 1 1 calc GR . . . .
H1B H 0.2987 0.6404 0.3677 0.104 Uiso 1 1 calc GR . . . .
H1C H 0.3537 0.6768 0.3890 0.104 Uiso 1 1 calc GR . . . .
C2 C 0.29632(16) 0.54776(17) 0.51645(18) 0.0524(8) Uani 1 1 d . . . . .
C3 C 0.28010(18) 0.58501(18) 0.46833(18) 0.0561(9) Uani 1 1 d . . . . .
C4 C 0.2231(2) 0.5874(2) 0.4473(2) 0.0696(12) Uani 1 1 d . . . . .
H4 H 0.2130 0.6128 0.4165 0.084 Uiso 1 1 calc R . . . .
C5 C 0.1809(2) 0.5507(2) 0.4731(3) 0.0794(15) Uani 1 1 d . . . . .
H5 H 0.1422 0.5518 0.4592 0.095 Uiso 1 1 calc R . . . .
C6 C 0.1952(2) 0.5133(2) 0.5184(2) 0.0678(11) Uani 1 1 d . . . . .
H6 H 0.1661 0.4890 0.5344 0.081 Uiso 1 1 calc R . . . .
C7 C 0.25339(18) 0.51080(17) 0.54142(18) 0.0555(9) Uani 1 1 d . . . . .
C8 C 0.26968(18) 0.47006(18) 0.58999(18) 0.0561(9) Uani 1 1 d . . . . .
C9 C 0.2418(2) 0.3975(2) 0.6632(2) 0.0702(12) Uani 1 1 d . . . . .
H9A H 0.2768 0.3756 0.6515 0.084 Uiso 1 1 calc R . . . .
H9B H 0.2095 0.3696 0.6672 0.084 Uiso 1 1 calc R . . . .
C10 C 0.2529(3) 0.4268(2) 0.7223(2) 0.0820(14) Uani 1 1 d . . . . .
H10A H 0.2836 0.4565 0.7185 0.098 Uiso 1 1 calc R . . . .
H10B H 0.2171 0.4458 0.7363 0.098 Uiso 1 1 calc R . . . .
C11 C 0.3241(2) 0.3836(3) 0.7840(2) 0.0773(13) Uani 1 1 d . . . . .
H11 H 0.3477 0.4152 0.7725 0.093 Uiso 1 1 calc R . . . .
C12 C 0.3490(2) 0.3403(3) 0.8233(2) 0.0790(13) Uani 1 1 d . U . . .
C13 C 0.4045(3) 0.3524(4) 0.8482(3) 0.114(2) Uani 1 1 d . U . . .
H13 H 0.4246 0.3870 0.8385 0.136 Uiso 1 1 calc R . . . .
C14 C 0.4283(4) 0.3134(5) 0.8865(4) 0.139(3) Uani 1 1 d . U . . .
H14 H 0.4659 0.3207 0.9014 0.167 Uiso 1 1 calc R . . . .
C15 C 0.3991(4) 0.2628(5) 0.9046(4) 0.132(3) Uani 1 1 d . U . . .
H15 H 0.4160 0.2378 0.9325 0.158 Uiso 1 1 calc R . . . .
C16 C 0.3442(3) 0.2501(3) 0.8805(3) 0.1021(18) Uani 1 1 d . U . . .
H16 H 0.3242 0.2160 0.8915 0.123 Uiso 1 1 calc R . . . .
C17 C 0.3193(3) 0.2891(3) 0.8395(2) 0.0817(13) Uani 1 1 d . U . . .
H17 H 0.2825 0.2807 0.8231 0.098 Uiso 1 1 calc R . . . .
C18 C 0.4038(2) 0.4033(2) 0.5061(2) 0.0664(7) Uani 1 1 d . . . . .
H18A H 0.3762 0.3848 0.5325 0.100 Uiso 1 1 calc GR . . . .
H18B H 0.4284 0.3736 0.4884 0.100 Uiso 1 1 calc GR . . . .
H18C H 0.3826 0.4241 0.4758 0.100 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.09299(4) 0.40701(4) 0.59299(4) 0.0533(4) Uani 1 3 d S T P . .
O1W O 0.0000 0.5000 0.5000 0.073(8) Uiso 0.25 6 d S T P . .


_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 2.210(3) 21_666 ?
Ni1 O2 1.973(3) 21_666 ?
Ni1 O2 1.954(3) . ?
Ni1 O3 2.015(3) . ?
Ni1 O4 2.060(3) . ?
Ni1 O4 2.090(3) 17_666 ?
Ni2 O4 2.086(3) 21_666 ?
Ni2 O4 2.086(3) 5 ?
Ni2 O4 2.086(3) 17_666 ?
Ni2 O4 2.086(3) 13_666 ?
Ni2 O4 2.086(3) 9 ?
Ni2 O4 2.086(3) . ?
O1 Ni1 2.210(3) 17_666 ?
O1 C1 1.426(5) . ?
O1 C3 1.378(5) . ?
O2 Ni1 1.973(3) 17_666 ?
O2 C2 1.311(5) . ?
O3 C8 1.252(5) . ?
O4 Ni1 2.090(3) 21_666 ?
O4 C18 1.371(6) . ?
N1 H1 0.8600 . ?
N1 C8 1.330(5) . ?
N1 C9 1.449(6) . ?
N2 C10 1.462(7) . ?
N2 C11 1.274(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.424(6) . ?
C2 C7 1.400(5) . ?
C3 C4 1.375(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.368(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.416(6) . ?
C7 C8 1.480(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.512(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C11 C12 1.438(8) . ?
C12 C13 1.403(8) . ?
C12 C17 1.387(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.350(11) . ?
C14 H14 0.9300 . ?
C14 C15 1.381(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(11) . ?
C16 H16 0.9300 . ?
C16 C17 1.398(9) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O1 74.76(11) 21_666 21_666 ?
O2 Ni1 O1 99.63(11) . 21_666 ?
O2 Ni1 O2 173.43(7) . 21_666 ?
O2 Ni1 O3 85.74(11) . . ?
O2 Ni1 O3 97.24(12) 21_666 . ?
O2 Ni1 O4 97.27(12) 21_666 17_666 ?
O2 Ni1 O4 80.02(12) 21_666 . ?
O2 Ni1 O4 105.36(12) . . ?
O2 Ni1 O4 79.70(12) . 17_666 ?
O3 Ni1 O1 86.91(12) . 21_666 ?
O3 Ni1 O4 165.44(12) . 17_666 ?
O3 Ni1 O4 99.05(13) . . ?
O4 Ni1 O1 154.64(12) . 21_666 ?
O4 Ni1 O1 95.70(13) 17_666 21_666 ?
O4 Ni1 O4 84.70(19) . 17_666 ?
O4 Ni2 O4 95.85(12) 21_666 17_666 ?
O4 Ni2 O4 84.15(12) 17_666 9 ?
O4 Ni2 O4 84.15(12) . 21_666 ?
O4 Ni2 O4 180.00(14) 5 17_666 ?
O4 Ni2 O4 180.0 21_666 9 ?
O4 Ni2 O4 180.00(13) . 13_666 ?
O4 Ni2 O4 95.85(12) 21_666 13_666 ?
O4 Ni2 O4 95.85(12) 13_666 17_666 ?
O4 Ni2 O4 95.85(12) . 5 ?
O4 Ni2 O4 95.85(12) . 9 ?
O4 Ni2 O4 84.15(12) 21_666 5 ?
O4 Ni2 O4 84.15(12) 13_666 9 ?
O4 Ni2 O4 84.15(12) 13_666 5 ?
O4 Ni2 O4 84.15(12) . 17_666 ?
O4 Ni2 O4 95.85(12) 5 9 ?
C1 O1 Ni1 127.1(3) . 17_666 ?
C3 O1 Ni1 113.2(2) . 17_666 ?
C3 O1 C1 119.4(3) . . ?
Ni1 O2 Ni1 103.50(12) . 17_666 ?
C2 O2 Ni1 122.4(3) . 17_666 ?
C2 O2 Ni1 132.0(3) . . ?
C8 O3 Ni1 131.9(3) . . ?
Ni1 O4 Ni1 96.00(13) . 21_666 ?
Ni1 O4 Ni2 95.91(14) . . ?
Ni2 O4 Ni1 95.00(14) . 21_666 ?
C18 O4 Ni1 118.9(3) . . ?
C18 O4 Ni1 119.2(3) . 21_666 ?
C18 O4 Ni2 125.3(3) . . ?
C8 N1 H1 119.7 . . ?
C8 N1 C9 120.5(4) . . ?
C9 N1 H1 119.7 . . ?
C11 N2 C10 117.7(5) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C3 116.4(3) . . ?
O2 C2 C7 124.7(4) . . ?
C7 C2 C3 118.9(3) . . ?
O1 C3 C2 112.9(3) . . ?
C4 C3 O1 125.1(4) . . ?
C4 C3 C2 121.9(4) . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.3(4) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.3(4) . . ?
C7 C6 H6 119.3 . . ?
C2 C7 C6 118.2(4) . . ?
C2 C7 C8 119.9(4) . . ?
C6 C7 C8 121.9(4) . . ?
O3 C8 N1 117.2(4) . . ?
O3 C8 C7 123.8(4) . . ?
N1 C8 C7 119.0(4) . . ?
N1 C9 H9A 109.1 . . ?
N1 C9 H9B 109.1 . . ?
N1 C9 C10 112.6(4) . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
N2 C10 C9 108.1(4) . . ?
N2 C10 H10A 110.1 . . ?
N2 C10 H10B 110.1 . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 H11 118.2 . . ?
N2 C11 C12 123.7(5) . . ?
C12 C11 H11 118.2 . . ?
C13 C12 C11 117.7(6) . . ?
C17 C12 C11 122.8(5) . . ?
C17 C12 C13 119.4(6) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.1(7) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 118.6 . . ?
C13 C14 C15 122.8(8) . . ?
C15 C14 H14 118.6 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 118.9(7) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.3 . . ?
C15 C16 C17 119.4(7) . . ?
C17 C16 H16 120.3 . . ?
C12 C17 C16 120.4(6) . . ?
C12 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
