# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_n151012a_sq
_database_code_depnum_ccdc_archive 'CCDC 1476691'
_audit_update_record             
;
2018-09-13 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_audit_creation_date             2018-08-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.04(C672 H816 Dy48 N240 Ni24 O336)'
_chemical_formula_sum            'C28 H34 Dy2 N10 Ni O14'
_chemical_formula_weight         1118.36
_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'
Dy Dy -0.1892 4.4098 '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           206
_space_group_name_H-M_alt        'I a -3'
_space_group_name_Hall           '-I 2b 2c 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'z, x, y'
'-z, -x+1/2, y'
'z, -x, -y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'y, -z, -x+1/2'
'-y, z+1/2, -x+1/2'
'-y, -z+1/2, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1, -z+1'
'z+1/2, x+1/2, y+1/2'
'-z+1/2, -x+1, y+1/2'
'z+1/2, -x+1/2, -y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+1/2, z+1, -x+1'
'-y+1/2, -z+1, x+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x, -y-1/2, z-1/2'
'-z, -x, -y'
'z, x-1/2, -y'
'-z, x, y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'-y, z, x-1/2'
'y, -z-1/2, x-1/2'
'y, z-1/2, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, z'
'-z+1/2, -x+1/2, -y+1/2'
'z+1/2, x, -y+1/2'
'-z+1/2, x+1/2, y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'-y+1/2, z+1/2, x'
'y+1/2, -z, x'
'y+1/2, z, -x+1/2'

_cell_length_a                   32.1011(3)
_cell_length_b                   32.1011(3)
_cell_length_c                   32.1011(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     33079.6(9)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.578
_shelx_estimated_absorpt_T_min   0.551
_exptl_absorpt_coefficient_mu    3.074
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0942 before and 0.0644 after correction. The Ratio of minimum to maximum transmission is 0.8148. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             13056
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         1.554
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5754
_reflns_number_total             6856
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.

The unit cell contains 72 methanol molecules and 72 acetonitrile molecules 
 and 24 water molecules which have been treated as a diffuse 
contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON. 
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²+43.4606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0493
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H2(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
3.a Riding coordinates:
 O2(H2), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Dy1 Dy 0.38244(2) 0.55082(2) 0.78458(2) 0.01246(3) Uani 1 1 d . . . . .
Ni1 Ni 0.27122(2) 0.500000 0.750000 0.01177(8) Uani 1 2 d S T P . .
O1 O 0.30873(4) 0.54725(4) 0.77640(4) 0.0126(3) Uani 1 1 d . . . . .
O2 O 0.18702(5) 0.53161(5) 0.77182(6) 0.0243(4) Uani 1 1 d . . . . .
H2 H 0.181909 0.515509 0.751834 0.036 Uiso 0.5 1 d R . . A -1
O3 O 0.38177(5) 0.58811(5) 0.71822(5) 0.0177(3) Uani 1 1 d . . . . .
O4 O 0.37296(5) 0.52071(5) 0.71165(5) 0.0155(3) Uani 1 1 d . . . . .
O5 O 0.42531(5) 0.54096(6) 0.84640(6) 0.0286(4) Uani 1 1 d . . . . .
O6 O 0.35834(6) 0.55114(5) 0.85614(5) 0.0261(4) Uani 1 1 d . . . . .
O7 O 0.44776(5) 0.53295(5) 0.76081(5) 0.0214(4) Uani 1 1 d . . . . .
N1 N 0.42561(6) 0.61732(6) 0.78915(6) 0.0160(4) Uani 1 1 d . . . . .
N2 N 0.46816(6) 0.69211(6) 0.77667(6) 0.0149(4) Uani 1 1 d . . . . .
N3 N 0.34323(6) 0.61699(6) 0.79519(6) 0.0142(4) Uani 1 1 d . . . . .
N4 N 0.30027(6) 0.61544(6) 0.80020(6) 0.0159(4) Uani 1 1 d . . . . .
N5 N 0.22821(6) 0.53961(6) 0.77340(6) 0.0152(4) Uani 1 1 d . . . . .
C1 C 0.46688(7) 0.61861(7) 0.78448(8) 0.0199(5) Uani 1 1 d . . . . .
H1 H 0.482190 0.593298 0.785133 0.024 Uiso 1 1 calc R . . . .
C2 C 0.48808(7) 0.65574(7) 0.77871(7) 0.0191(5) Uani 1 1 d . . . . .
H2A H 0.517563 0.655274 0.776141 0.023 Uiso 1 1 calc R . . . .
C3 C 0.42672(7) 0.69081(7) 0.78155(7) 0.0160(5) Uani 1 1 d . . . . .
H3 H 0.411462 0.716147 0.780404 0.019 Uiso 1 1 calc R . . . .
C4 C 0.40528(7) 0.65400(7) 0.78819(7) 0.0150(4) Uani 1 1 d . . . . .
C5 C 0.35969(7) 0.65364(7) 0.79447(7) 0.0157(4) Uani 1 1 d . . . . .
C6 C 0.33674(8) 0.69404(7) 0.79879(9) 0.0269(6) Uani 1 1 d . . . . .
H6A H 0.306859 0.688496 0.801691 0.040 Uiso 1 1 d R . . . .
H6B H 0.341549 0.711056 0.773911 0.040 Uiso 1 1 d R . . . .
H6C H 0.346749 0.708986 0.823451 0.040 Uiso 1 1 d R . . . .
C7 C 0.28616(7) 0.57851(7) 0.79019(7) 0.0132(4) Uani 1 1 d . . . . .
C8 C 0.24025(7) 0.57325(7) 0.79163(7) 0.0167(5) Uani 1 1 d . . . . .
C9 C 0.21195(8) 0.60440(8) 0.81117(10) 0.0324(7) Uani 1 1 d . . . . .
H9A H 0.190047 0.612216 0.791404 0.049 Uiso 1 1 d R . . . .
H9B H 0.227937 0.629206 0.819004 0.049 Uiso 1 1 d R . . . .
H9C H 0.199257 0.592186 0.836105 0.049 Uiso 1 1 d R . . . .
C10 C 0.38082(7) 0.55651(7) 0.69561(7) 0.0168(5) Uani 1 1 d . . . . .
C11 C 0.38945(8) 0.55944(7) 0.64996(7) 0.0231(5) Uani 1 1 d . . . . .
H11A H 0.385742 0.588305 0.640775 0.035 Uiso 1 1 d R . . . .
H11B H 0.370082 0.541355 0.634795 0.035 Uiso 1 1 d R . . . .
H11C H 0.418132 0.550575 0.644365 0.035 Uiso 1 1 d R . . . .
C12 C 0.39443(9) 0.54403(8) 0.87057(8) 0.0269(6) Uani 1 1 d . . . . .
C13 C 0.40008(11) 0.53866(10) 0.91701(9) 0.0423(8) Uani 1 1 d . . . . .
H13A H 0.429849 0.536540 0.923426 0.063 Uiso 1 1 d R . . . .
H13B H 0.385849 0.513270 0.926206 0.063 Uiso 1 1 d R . . . .
H13C H 0.388239 0.562780 0.931506 0.063 Uiso 1 1 d R . . . .
C14 C 0.46613(10) 0.500000 0.750000 0.0195(7) Uani 1 2 d S T P . .
C15 C 0.51324(11) 0.500000 0.750000 0.0400(11) Uani 1 2 d S T P . .
H15A H 0.523418 0.489100 0.776640 0.060 Uiso 0.5 1 d R . . . .
H15B H 0.523418 0.528520 0.746120 0.060 Uiso 0.5 1 d R . . . .
H15C H 0.523418 0.482380 0.727240 0.060 Uiso 0.5 1 d R . . . .


_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
Dy1 Dy1 3.9465(2) 3_566 ?
Dy1 O1 2.3833(15) . ?
Dy1 O3 2.4436(15) . ?
Dy1 O4 2.3193(15) 3_566 ?
Dy1 O4 2.5509(15) . ?
Dy1 O5 2.4357(17) . ?
Dy1 O6 2.4241(17) . ?
Dy1 O7 2.3042(16) . ?
Dy1 N1 2.5493(18) . ?
Dy1 N3 2.4923(18) . ?
Ni1 O1 2.1138(15) 3_566 ?
Ni1 O1 2.1138(15) . ?
Ni1 N2 2.1281(18) 44_465 ?
Ni1 N2 2.1281(18) 42_456 ?
Ni1 N5 2.0218(19) 3_566 ?
Ni1 N5 2.0218(19) . ?
O1 C7 1.315(3) . ?
O2 H2 0.8401 . ?
O2 N5 1.348(2) . ?
O3 C10 1.248(3) . ?
O4 C10 1.285(3) . ?
O5 C12 1.263(3) . ?
O6 C12 1.268(3) . ?
O7 C14 1.260(2) . ?
N1 C1 1.334(3) . ?
N1 C4 1.347(3) . ?
N2 C2 1.333(3) . ?
N2 C3 1.340(3) . ?
N3 N4 1.389(2) . ?
N3 C5 1.290(3) . ?
N4 C7 1.309(3) . ?
N5 C8 1.288(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.385(3) . ?
C2 H2A 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.384(3) . ?
C4 C5 1.478(3) . ?
C5 C6 1.498(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9799 . ?
C6 H6C 0.9799 . ?
C7 C8 1.484(3) . ?
C8 C9 1.490(3) . ?
C9 H9A 0.9798 . ?
C9 H9B 0.9803 . ?
C9 H9C 0.9798 . ?
C10 C11 1.494(3) . ?
C11 H11A 0.9798 . ?
C11 H11B 0.9801 . ?
C11 H11C 0.9802 . ?
C12 C13 1.511(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9799 . ?
C13 H13C 0.9801 . ?
C14 C15 1.512(5) . ?
C15 H15A 0.9802 3_566 ?
C15 H15A 0.9801 . ?
C15 H15B 0.9800 3_566 ?
C15 H15B 0.9800 . ?
C15 H15C 0.9801 3_566 ?
C15 H15C 0.9801 . ?

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 Dy1 Dy1 84.16(3) . 3_566 ?
O1 Dy1 O3 85.35(5) . . ?
O1 Dy1 O4 76.25(5) . . ?
O1 Dy1 O5 130.12(6) . . ?
O1 Dy1 O6 77.75(5) . . ?
O1 Dy1 N1 125.90(5) . . ?
O1 Dy1 N3 63.56(5) . . ?
O3 Dy1 Dy1 85.10(4) . 3_566 ?
O3 Dy1 O4 52.02(5) . . ?
O3 Dy1 N1 69.19(6) . . ?
O3 Dy1 N3 72.38(5) . . ?
O4 Dy1 Dy1 33.95(3) . 3_566 ?
O4 Dy1 Dy1 37.89(4) 3_566 3_566 ?
O4 Dy1 O1 80.09(5) 3_566 . ?
O4 Dy1 O3 121.95(5) 3_566 . ?
O4 Dy1 O4 69.94(6) 3_566 . ?
O4 Dy1 O5 84.43(6) 3_566 . ?
O4 Dy1 O6 85.00(6) 3_566 . ?
O4 Dy1 N1 153.79(6) 3_566 . ?
O4 Dy1 N3 140.38(6) 3_566 . ?
O5 Dy1 Dy1 110.53(4) . 3_566 ?
O5 Dy1 O3 141.16(6) . . ?
O5 Dy1 O4 139.97(6) . . ?
O5 Dy1 N1 75.80(6) . . ?
O5 Dy1 N3 106.55(6) . . ?
O6 Dy1 Dy1 122.45(4) . 3_566 ?
O6 Dy1 O3 145.22(5) . . ?
O6 Dy1 O4 146.43(6) . . ?
O6 Dy1 O5 53.75(6) . . ?
O6 Dy1 N1 96.63(6) . . ?
O6 Dy1 N3 72.89(6) . . ?
O7 Dy1 Dy1 66.91(4) . 3_566 ?
O7 Dy1 O1 148.77(5) . . ?
O7 Dy1 O3 80.86(6) . . ?
O7 Dy1 O4 73.16(5) . . ?
O7 Dy1 O4 83.69(5) . 3_566 ?
O7 Dy1 O5 73.93(6) . . ?
O7 Dy1 O6 127.25(6) . . ?
O7 Dy1 N1 74.50(6) . . ?
O7 Dy1 N3 135.82(6) . . ?
N1 Dy1 Dy1 136.44(4) . 3_566 ?
N1 Dy1 O4 115.79(5) . . ?
N3 Dy1 Dy1 141.40(4) . 3_566 ?
N3 Dy1 O4 112.85(5) . . ?
N3 Dy1 N1 63.46(6) . . ?
O1 Ni1 O1 110.56(8) 3_566 . ?
O1 Ni1 N2 87.00(6) . 42_456 ?
O1 Ni1 N2 87.00(6) 3_566 44_465 ?
O1 Ni1 N2 87.64(6) . 44_465 ?
O1 Ni1 N2 87.63(6) 3_566 42_456 ?
N2 Ni1 N2 170.57(10) 42_456 44_465 ?
N5 Ni1 O1 77.81(7) . . ?
N5 Ni1 O1 171.58(7) 3_566 . ?
N5 Ni1 O1 171.58(7) . 3_566 ?
N5 Ni1 O1 77.81(6) 3_566 3_566 ?
N5 Ni1 N2 94.50(7) 3_566 42_456 ?
N5 Ni1 N2 94.50(7) . 44_465 ?
N5 Ni1 N2 91.94(7) . 42_456 ?
N5 Ni1 N2 91.94(7) 3_566 44_465 ?
N5 Ni1 N5 93.85(11) 3_566 . ?
Ni1 O1 Dy1 130.10(7) . . ?
C7 O1 Dy1 118.25(13) . . ?
C7 O1 Ni1 111.64(13) . . ?
N5 O2 H2 109.7 . . ?
C10 O3 Dy1 96.26(13) . . ?
Dy1 O4 Dy1 108.16(6) 3_566 . ?
C10 O4 Dy1 151.77(14) . 3_566 ?
C10 O4 Dy1 90.30(13) . . ?
C12 O5 Dy1 92.70(15) . . ?
C12 O6 Dy1 93.09(15) . . ?
C14 O7 Dy1 136.58(16) . . ?
C1 N1 Dy1 124.03(15) . . ?
C1 N1 C4 116.85(19) . . ?
C4 N1 Dy1 117.86(14) . . ?
C2 N2 Ni1 122.58(15) . 34_656 ?
C2 N2 C3 116.32(19) . . ?
C3 N2 Ni1 120.89(15) . 34_656 ?
N4 N3 Dy1 119.11(13) . . ?
C5 N3 Dy1 124.60(15) . . ?
C5 N3 N4 116.20(18) . . ?
C7 N4 N3 110.34(18) . . ?
O2 N5 Ni1 122.43(14) . . ?
C8 N5 Ni1 119.43(15) . . ?
C8 N5 O2 118.12(18) . . ?
N1 C1 H1 119.0 . . ?
N1 C1 C2 122.0(2) . . ?
C2 C1 H1 119.0 . . ?
N2 C2 C1 121.6(2) . . ?
N2 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
N2 C3 H3 118.7 . . ?
N2 C3 C4 122.5(2) . . ?
C4 C3 H3 118.7 . . ?
N1 C4 C3 120.6(2) . . ?
N1 C4 C5 118.1(2) . . ?
C3 C4 C5 121.3(2) . . ?
N3 C5 C4 114.55(19) . . ?
N3 C5 C6 125.9(2) . . ?
C4 C5 C6 119.54(19) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.3 . . ?
C5 C6 H6C 109.7 . . ?
H6A C6 H6B 109.4 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 C8 118.10(19) . . ?
N4 C7 O1 125.7(2) . . ?
N4 C7 C8 116.04(19) . . ?
N5 C8 C7 112.29(19) . . ?
N5 C8 C9 124.8(2) . . ?
C7 C8 C9 122.9(2) . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.2 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 O4 119.9(2) . . ?
O3 C10 C11 121.0(2) . . ?
O4 C10 C11 119.1(2) . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C10 C11 H11C 109.6 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.4 . . ?
O5 C12 O6 120.4(2) . . ?
O5 C12 C13 120.2(3) . . ?
O6 C12 C13 119.4(3) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.6 . . ?
C12 C13 H13C 109.4 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O7 C14 O7 124.2(3) . 3_566 ?
O7 C14 C15 117.91(15) 3_566 . ?
O7 C14 C15 117.91(15) . . ?
C14 C15 H15A 109.480(1) . 3_566 ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15B 109.483(2) . 3_566 ?
C14 C15 H15C 109.5 . . ?
C14 C15 H15C 109.481(1) . 3_566 ?
H15A C15 H15A 141.0 . 3_566 ?
H15A C15 H15B 109.5 3_566 3_566 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15B 56.2 . 3_566 ?
H15A C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 3_566 3_566 ?
H15A C15 H15C 56.3 . 3_566 ?
H15B C15 H15A 56.2 . 3_566 ?
H15B C15 H15B 141.0 . 3_566 ?
H15B C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 3_566 3_566 ?
H15B C15 H15C 56.2 . 3_566 ?
H15C C15 H15A 56.2 . 3_566 ?
H15C C15 H15B 56.3 . 3_566 ?
H15C C15 H15C 141.0 . 3_566 ?

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
_geom_hbond_publ_flag
O2 H2 N5 0.84 2.45 3.014(2) 125.4 3_566 yes
C1 H1 O7 0.95 2.36 2.918(3) 116.9 . yes
C3 H3 O1 0.95 2.51 3.001(3) 111.9 34_656 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C7 N4 15.3(3) . . . . ?
Dy1 O1 C7 C8 -169.86(14) . . . . ?
Dy1 O3 C10 O4 12.6(2) . . . . ?
Dy1 O3 C10 C11 -166.30(19) . . . . ?
Dy1 O4 C10 O3 -12.0(2) . . . . ?
Dy1 O4 C10 O3 -144.0(2) 3_566 . . . ?
Dy1 O4 C10 C11 35.0(4) 3_566 . . . ?
Dy1 O4 C10 C11 166.93(19) . . . . ?
Dy1 O5 C12 O6 -1.7(2) . . . . ?
Dy1 O5 C12 C13 177.5(2) . . . . ?
Dy1 O6 C12 O5 1.7(2) . . . . ?
Dy1 O6 C12 C13 -177.5(2) . . . . ?
Dy1 O7 C14 O7 20.18(12) . . . 3_566 ?
Dy1 O7 C14 C15 -159.83(12) . . . . ?
Dy1 N1 C1 C2 166.54(17) . . . . ?
Dy1 N1 C4 C3 -166.04(16) . . . . ?
Dy1 N1 C4 C5 14.0(3) . . . . ?
Dy1 N3 N4 C7 -12.5(2) . . . . ?
Dy1 N3 C5 C4 -2.1(3) . . . . ?
Dy1 N3 C5 C6 177.03(18) . . . . ?
Ni1 O1 C7 N4 -165.25(18) . . . . ?
Ni1 O1 C7 C8 9.6(2) . . . . ?
Ni1 N2 C2 C1 176.50(17) 34_656 . . . ?
Ni1 N2 C3 C4 -175.24(16) 34_656 . . . ?
Ni1 N5 C8 C7 3.3(3) . . . . ?
Ni1 N5 C8 C9 -178.2(2) . . . . ?
O1 C7 C8 N5 -8.9(3) . . . . ?
O1 C7 C8 C9 172.6(2) . . . . ?
O2 N5 C8 C7 -178.70(18) . . . . ?
O2 N5 C8 C9 -0.2(4) . . . . ?
N1 C1 C2 N2 -1.4(4) . . . . ?
N1 C4 C5 N3 -8.2(3) . . . . ?
N1 C4 C5 C6 172.6(2) . . . . ?
N2 C3 C4 N1 -1.4(3) . . . . ?
N2 C3 C4 C5 178.5(2) . . . . ?
N3 N4 C7 O1 -1.4(3) . . . . ?
N3 N4 C7 C8 -176.40(18) . . . . ?
N4 N3 C5 C4 -178.75(18) . . . . ?
N4 N3 C5 C6 0.4(3) . . . . ?
N4 C7 C8 N5 166.5(2) . . . . ?
N4 C7 C8 C9 -12.0(3) . . . . ?
C1 N1 C4 C3 1.6(3) . . . . ?
C1 N1 C4 C5 -178.3(2) . . . . ?
C2 N2 C3 C4 -0.3(3) . . . . ?
C3 N2 C2 C1 1.6(3) . . . . ?
C3 C4 C5 N3 171.9(2) . . . . ?
C3 C4 C5 C6 -7.3(3) . . . . ?
C4 N1 C1 C2 -0.3(3) . . . . ?
C5 N3 N4 C7 164.26(19) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.013 -0.015 0.000 12693 3050 ' '
2 0.250 0.250 0.250 88 8 ' '
3 0.750 0.250 0.250 88 8 ' '
4 0.750 0.250 0.750 88 8 ' '
5 0.250 0.250 0.750 88 8 ' '
6 0.250 0.750 0.250 88 8 ' '
7 0.750 0.750 0.250 88 8 ' '
8 0.750 0.750 0.750 88 8 ' '
9 0.250 0.750 0.750 88 8 ' '

_platon_squeeze_void_probe_radius 1.20
_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_n151022a_sq
_database_code_depnum_ccdc_archive 'CCDC 1476692'
_audit_update_record             
;
2018-09-13 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_audit_creation_date             2018-08-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.04(C672 H816 N240 Ni24 O336 Tb48)'
_chemical_formula_sum            'C28 H34 N10 Ni O14 Tb2'
_chemical_formula_weight         1111.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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           206
_space_group_name_H-M_alt        'I a -3'
_space_group_name_Hall           '-I 2b 2c 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+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-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+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'

_cell_length_a                   32.2995(5)
_cell_length_b                   32.2995(5)
_cell_length_c                   32.2995(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     33696.7(16)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    9139
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   0.626
_shelx_estimated_absorpt_T_min   0.570
_exptl_absorpt_coefficient_mu    2.875
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1249 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8835. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             13008
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            123673
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         1.261
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5702
_reflns_number_total             6999
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.

The unit cell contains 96 methanol molecules and 72 acetonitrile molecules 
 and 24 water molecules which have been treated as a diffuse 
contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON. 
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²+112.1332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0608
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Others
 Fixed Sof: H2(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Riding coordinates:
 O2(H2), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Tb1 Tb 0.38362(2) 0.55085(2) 0.78411(2) 0.02070(4) Uani 1 1 d . . . . .
Ni1 Ni 0.27293(2) 0.500000 0.750000 0.01885(10) Uani 1 2 d S T P . .
O1 O 0.31009(6) 0.54720(5) 0.77609(5) 0.0195(4) Uani 1 1 d . . . . .
O2 O 0.18930(6) 0.53166(7) 0.77159(8) 0.0365(5) Uani 1 1 d . . . . .
H2 H 0.184191 0.515559 0.751603 0.055 Uiso 0.5 1 d R . . A -1
O3 O 0.38258(6) 0.58744(6) 0.71754(6) 0.0248(4) Uani 1 1 d . . . . .
O4 O 0.37425(6) 0.52049(6) 0.71150(6) 0.0234(4) Uani 1 1 d . . . . .
O5 O 0.42601(9) 0.54204(8) 0.84552(9) 0.0529(7) Uani 1 1 d . . . . .
O6 O 0.35952(9) 0.55146(7) 0.85579(7) 0.0474(6) Uani 1 1 d . . . . .
O7 O 0.44889(6) 0.53296(6) 0.76019(8) 0.0395(6) Uani 1 1 d . . . . .
N1 N 0.42645(7) 0.61748(7) 0.78838(7) 0.0245(5) Uani 1 1 d . . . . .
N2 N 0.46862(7) 0.69213(7) 0.77800(7) 0.0230(5) Uani 1 1 d . . . . .
N3 N 0.34453(7) 0.61687(7) 0.79445(7) 0.0198(4) Uani 1 1 d . . . . .
N4 N 0.30179(7) 0.61531(7) 0.79898(7) 0.0223(5) Uani 1 1 d . . . . .
N5 N 0.23019(7) 0.53954(7) 0.77298(8) 0.0260(5) Uani 1 1 d . . . . .
C1 C 0.46734(9) 0.61883(9) 0.78385(10) 0.0305(6) Uani 1 1 d . . . . .
H1 H 0.482563 0.593663 0.783955 0.037 Uiso 1 1 calc R . . . .
C2 C 0.48839(9) 0.65591(9) 0.77897(9) 0.0278(6) Uani 1 1 d . . . . .
H2A H 0.517678 0.655507 0.776255 0.033 Uiso 1 1 calc R . . . .
C3 C 0.42743(8) 0.69081(8) 0.78283(8) 0.0226(5) Uani 1 1 d . . . . .
H3 H 0.412245 0.715997 0.782379 0.027 Uiso 1 1 calc R . . . .
C4 C 0.40620(8) 0.65384(8) 0.78847(8) 0.0214(5) Uani 1 1 d . . . . .
C5 C 0.36069(8) 0.65340(8) 0.79428(8) 0.0218(5) Uani 1 1 d . . . . .
C6 C 0.33774(9) 0.69336(9) 0.79847(11) 0.0342(7) Uani 1 1 d . . . . .
H6A H 0.307860 0.687799 0.801369 0.051 Uiso 1 1 d R . . . .
H6B H 0.342550 0.710379 0.773589 0.051 Uiso 1 1 d R . . . .
H6C H 0.347750 0.708299 0.823129 0.051 Uiso 1 1 d R . . . .
C7 C 0.28788(8) 0.57851(8) 0.78929(8) 0.0210(5) Uani 1 1 d . . . . .
C8 C 0.24243(9) 0.57339(9) 0.79057(9) 0.0284(6) Uani 1 1 d . . . . .
C9 C 0.21402(10) 0.60487(11) 0.80918(14) 0.0512(11) Uani 1 1 d . . . . .
H9A H 0.192116 0.612686 0.789393 0.077 Uiso 1 1 d R . . . .
H9B H 0.229986 0.629666 0.816993 0.077 Uiso 1 1 d R . . . .
H9C H 0.201316 0.592656 0.834113 0.077 Uiso 1 1 d R . . . .
C10 C 0.38165(8) 0.55585(8) 0.69535(9) 0.0234(5) Uani 1 1 d . . . . .
C11 C 0.39036(10) 0.55845(9) 0.64974(9) 0.0317(7) Uani 1 1 d . . . . .
H11A H 0.386646 0.587342 0.640557 0.048 Uiso 1 1 d R . . . .
H11B H 0.370986 0.540382 0.634586 0.048 Uiso 1 1 d R . . . .
H11C H 0.419026 0.549602 0.644147 0.048 Uiso 1 1 d R . . . .
C12 C 0.39589(16) 0.54496(11) 0.86930(12) 0.0507(10) Uani 1 1 d . U . . .
C13 C 0.40236(19) 0.53971(16) 0.91573(13) 0.0791(15) Uani 1 1 d . U . . .
H13A H 0.432125 0.537587 0.922143 0.119 Uiso 1 1 d R . . . .
H13B H 0.388125 0.514307 0.924923 0.119 Uiso 1 1 d R . . . .
H13C H 0.390515 0.563827 0.930233 0.119 Uiso 1 1 d R . . . .
C14 C 0.46717(14) 0.500000 0.750000 0.0445(12) Uani 1 2 d S TU P . .
C15 C 0.5136(2) 0.500000 0.750000 0.089(2) Uani 1 2 d S TU P . .
H15A H 0.523811 0.489100 0.776640 0.133 Uiso 0.5 1 d R . . . .
H15B H 0.523811 0.528520 0.746120 0.133 Uiso 0.5 1 d R . . . .
H15C H 0.523811 0.482380 0.727240 0.133 Uiso 0.5 1 d R . . . .


_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
Tb1 Tb1 3.9553(3) 16_456 ?
Tb1 O1 2.3921(18) . ?
Tb1 O3 2.4540(19) . ?
Tb1 O4 2.5600(18) . ?
Tb1 O4 2.3282(18) 16_456 ?
Tb1 O5 2.427(2) . ?
Tb1 O6 2.443(2) . ?
Tb1 O7 2.318(2) . ?
Tb1 N1 2.562(2) . ?
Tb1 N3 2.501(2) . ?
Ni1 O1 2.1153(18) . ?
Ni1 O1 2.1154(18) 16_456 ?
Ni1 N2 2.133(2) 44_465 ?
Ni1 N2 2.133(2) 31_557 ?
Ni1 N5 2.022(2) . ?
Ni1 N5 2.022(2) 16_456 ?
O1 C7 1.311(3) . ?
O2 H2 0.8453 . ?
O2 N5 1.346(3) . ?
O3 C10 1.247(3) . ?
O4 C10 1.278(3) . ?
O5 C12 1.243(5) . ?
O6 C12 1.271(5) . ?
O7 C14 1.261(3) . ?
N1 C1 1.329(4) . ?
N1 C4 1.344(3) . ?
N2 C2 1.333(4) . ?
N2 C3 1.340(3) . ?
N3 N4 1.389(3) . ?
N3 C5 1.290(3) . ?
N4 C7 1.309(3) . ?
N5 C8 1.294(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.386(4) . ?
C2 H2A 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.389(4) . ?
C4 C5 1.482(4) . ?
C5 C6 1.494(4) . ?
C6 H6A 0.9861 . ?
C6 H6B 0.9860 . ?
C6 H6C 0.9858 . ?
C7 C8 1.478(4) . ?
C8 C9 1.496(4) . ?
C9 H9A 0.9863 . ?
C9 H9B 0.9856 . ?
C9 H9C 0.9860 . ?
C10 C11 1.502(4) . ?
C11 H11A 0.9864 . ?
C11 H11B 0.9857 . ?
C11 H11C 0.9858 . ?
C12 C13 1.524(5) . ?
C13 H13A 0.9860 . ?
C13 H13B 0.9861 . ?
C13 H13C 0.9862 . ?
C14 C15 1.501(8) . ?
C15 H15A 0.9860 . ?
C15 H15A 0.9861 16_456 ?
C15 H15B 0.9860 . ?
C15 H15B 0.9860 16_456 ?
C15 H15C 0.9861 16_456 ?
C15 H15C 0.9860 . ?

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 Tb1 Tb1 84.19(4) . 16_456 ?
O1 Tb1 O3 85.13(6) . . ?
O1 Tb1 O4 76.37(6) . . ?
O1 Tb1 O5 130.01(9) . . ?
O1 Tb1 O6 77.68(8) . . ?
O1 Tb1 N1 125.68(7) . . ?
O1 Tb1 N3 63.58(6) . . ?
O3 Tb1 Tb1 84.94(4) . 16_456 ?
O3 Tb1 O4 51.69(6) . . ?
O3 Tb1 N1 69.51(7) . . ?
O3 Tb1 N3 72.50(6) . . ?
O4 Tb1 Tb1 34.06(4) . 16_456 ?
O4 Tb1 Tb1 38.01(5) 16_456 16_456 ?
O4 Tb1 O1 80.14(6) 16_456 . ?
O4 Tb1 O3 121.89(6) 16_456 . ?
O4 Tb1 O4 70.20(7) 16_456 . ?
O4 Tb1 O5 84.70(8) 16_456 . ?
O4 Tb1 O6 84.77(7) 16_456 . ?
O4 Tb1 N1 153.93(7) 16_456 . ?
O4 Tb1 N1 115.78(7) . . ?
O4 Tb1 N3 140.36(7) 16_456 . ?
O5 Tb1 Tb1 110.98(6) . 16_456 ?
O5 Tb1 O3 141.30(8) . . ?
O5 Tb1 O4 140.41(8) . . ?
O5 Tb1 O6 53.57(10) . . ?
O5 Tb1 N1 75.52(8) . . ?
O5 Tb1 N3 106.00(8) . . ?
O6 Tb1 Tb1 122.33(6) . 16_456 ?
O6 Tb1 O3 145.31(7) . . ?
O6 Tb1 O4 146.48(8) . . ?
O6 Tb1 N1 96.56(8) . . ?
O6 Tb1 N3 72.87(7) . . ?
O7 Tb1 Tb1 66.88(5) . 16_456 ?
O7 Tb1 O1 148.70(7) . . ?
O7 Tb1 O3 80.82(8) . . ?
O7 Tb1 O4 72.95(7) . . ?
O7 Tb1 O4 83.80(7) . 16_456 ?
O7 Tb1 O5 74.35(10) . . ?
O7 Tb1 O6 127.43(9) . . ?
O7 Tb1 N1 74.71(7) . . ?
O7 Tb1 N3 135.74(7) . . ?
N1 Tb1 Tb1 136.68(5) . 16_456 ?
N3 Tb1 Tb1 141.50(5) . 16_456 ?
N3 Tb1 O4 112.91(6) . . ?
N3 Tb1 N1 63.20(7) . . ?
O1 Ni1 O1 110.86(10) . 16_456 ?
O1 Ni1 N2 87.88(8) 16_456 31_557 ?
O1 Ni1 N2 87.12(8) 16_456 44_465 ?
O1 Ni1 N2 87.12(8) . 31_557 ?
O1 Ni1 N2 87.88(8) . 44_465 ?
N2 Ni1 N2 171.19(12) 31_557 44_465 ?
N5 Ni1 O1 77.64(8) 16_456 16_456 ?
N5 Ni1 O1 77.64(8) . . ?
N5 Ni1 O1 171.45(8) . 16_456 ?
N5 Ni1 O1 171.46(8) 16_456 . ?
N5 Ni1 N2 94.24(9) 16_456 31_557 ?
N5 Ni1 N2 91.77(9) . 31_557 ?
N5 Ni1 N2 91.77(9) 16_456 44_465 ?
N5 Ni1 N2 94.24(9) . 44_465 ?
N5 Ni1 N5 93.88(13) 16_456 . ?
Ni1 O1 Tb1 129.94(8) . . ?
C7 O1 Tb1 118.03(16) . . ?
C7 O1 Ni1 112.02(16) . . ?
N5 O2 H2 109.5 . . ?
C10 O3 Tb1 96.30(16) . . ?
Tb1 O4 Tb1 107.93(7) 16_456 . ?
C10 O4 Tb1 90.54(15) . . ?
C10 O4 Tb1 152.23(17) . 16_456 ?
C12 O5 Tb1 93.1(2) . . ?
C12 O6 Tb1 91.7(2) . . ?
C14 O7 Tb1 136.3(2) . . ?
C1 N1 Tb1 123.91(18) . . ?
C1 N1 C4 117.1(2) . . ?
C4 N1 Tb1 118.10(17) . . ?
C2 N2 Ni1 122.90(19) . 34_576 ?
C2 N2 C3 116.4(2) . . ?
C3 N2 Ni1 120.57(18) . 34_576 ?
N4 N3 Tb1 119.00(15) . . ?
C5 N3 Tb1 125.09(18) . . ?
C5 N3 N4 115.8(2) . . ?
C7 N4 N3 110.4(2) . . ?
O2 N5 Ni1 122.57(17) . . ?
C8 N5 Ni1 119.10(19) . . ?
C8 N5 O2 118.3(2) . . ?
N1 C1 H1 119.1 . . ?
N1 C1 C2 121.9(3) . . ?
C2 C1 H1 119.1 . . ?
N2 C2 C1 121.7(3) . . ?
N2 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
N2 C3 H3 118.9 . . ?
N2 C3 C4 122.2(3) . . ?
C4 C3 H3 118.9 . . ?
N1 C4 C3 120.7(2) . . ?
N1 C4 C5 118.3(2) . . ?
C3 C4 C5 121.0(2) . . ?
N3 C5 C4 114.2(2) . . ?
N3 C5 C6 126.1(3) . . ?
C4 C5 C6 119.7(2) . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.2 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 C8 117.8(2) . . ?
N4 C7 O1 126.2(2) . . ?
N4 C7 C8 115.8(2) . . ?
N5 C8 C7 112.7(2) . . ?
N5 C8 C9 124.3(3) . . ?
C7 C8 C9 123.0(3) . . ?
C8 C9 H9A 110.7 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 108.2 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 O4 120.1(2) . . ?
O3 C10 C11 120.9(2) . . ?
O4 C10 C11 119.0(2) . . ?
C10 C11 H11A 109.0 . . ?
C10 C11 H11B 109.6 . . ?
C10 C11 H11C 109.8 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 O6 121.6(3) . . ?
O5 C12 C13 119.5(4) . . ?
O6 C12 C13 118.9(4) . . ?
C12 C13 H13A 110.4 . . ?
C12 C13 H13B 109.0 . . ?
C12 C13 H13C 109.0 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O7 C14 O7 124.2(4) 16_456 . ?
O7 C14 C15 117.9(2) 16_456 . ?
O7 C14 C15 117.9(2) . . ?
C14 C15 H15A 109.461(1) . 16_456 ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15B 109.463(1) . 16_456 ?
C14 C15 H15C 109.5 . . ?
C14 C15 H15C 109.462(1) . 16_456 ?
H15A C15 H15A 141.1 . 16_456 ?
H15A C15 H15B 109.5 16_456 16_456 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15B 56.2 . 16_456 ?
H15A C15 H15C 109.5 . . ?
H15A C15 H15C 56.3 . 16_456 ?
H15A C15 H15C 109.5 16_456 16_456 ?
H15B C15 H15A 56.3 . 16_456 ?
H15B C15 H15B 141.1 . 16_456 ?
H15B C15 H15C 109.5 . . ?
H15B C15 H15C 56.2 . 16_456 ?
H15B C15 H15C 109.5 16_456 16_456 ?
H15C C15 H15A 56.3 . 16_456 ?
H15C C15 H15B 56.3 . 16_456 ?
H15C C15 H15C 141.1 . 16_456 ?

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
_geom_hbond_publ_flag
O2 H2 N5 0.85 2.45 3.018(3) 125.2 16_456 yes
C1 H1 O7 0.95 2.37 2.938(3) 118.0 . yes
C3 H3 O1 0.95 2.51 3.006(3) 112.8 47_655 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C7 N4 14.7(3) . . . . ?
Tb1 O1 C7 C8 -170.26(18) . . . . ?
Tb1 O3 C10 O4 12.3(3) . . . . ?
Tb1 O3 C10 C11 -165.9(2) . . . . ?
Tb1 O4 C10 O3 -11.7(3) . . . . ?
Tb1 O4 C10 O3 -144.5(3) 16_456 . . . ?
Tb1 O4 C10 C11 33.8(5) 16_456 . . . ?
Tb1 O4 C10 C11 166.5(2) . . . . ?
Tb1 O5 C12 O6 -1.5(4) . . . . ?
Tb1 O5 C12 C13 177.1(3) . . . . ?
Tb1 O6 C12 O5 1.5(4) . . . . ?
Tb1 O6 C12 C13 -177.1(3) . . . . ?
Tb1 O7 C14 O7 20.77(17) . . . 16_456 ?
Tb1 O7 C14 C15 -159.24(17) . . . . ?
Tb1 N1 C1 C2 168.2(2) . . . . ?
Tb1 N1 C4 C3 -167.72(19) . . . . ?
Tb1 N1 C4 C5 11.6(3) . . . . ?
Tb1 N3 N4 C7 -11.8(3) . . . . ?
Tb1 N3 C5 C4 -1.7(3) . . . . ?
Tb1 N3 C5 C6 177.0(2) . . . . ?
Ni1 O1 C7 N4 -165.2(2) . . . . ?
Ni1 O1 C7 C8 9.9(3) . . . . ?
Ni1 N2 C2 C1 177.5(2) 34_576 . . . ?
Ni1 N2 C3 C4 -176.5(2) 34_576 . . . ?
Ni1 N5 C8 C7 2.5(3) . . . . ?
Ni1 N5 C8 C9 -179.3(3) . . . . ?
O1 C7 C8 N5 -8.5(4) . . . . ?
O1 C7 C8 C9 173.2(3) . . . . ?
O2 N5 C8 C7 -179.0(2) . . . . ?
O2 N5 C8 C9 -0.7(5) . . . . ?
N1 C1 C2 N2 -1.0(5) . . . . ?
N1 C4 C5 N3 -6.8(4) . . . . ?
N1 C4 C5 C6 174.3(3) . . . . ?
N2 C3 C4 N1 -1.5(4) . . . . ?
N2 C3 C4 C5 179.2(2) . . . . ?
N3 N4 C7 O1 -1.6(4) . . . . ?
N3 N4 C7 C8 -176.7(2) . . . . ?
N4 N3 C5 C4 -178.7(2) . . . . ?
N4 N3 C5 C6 0.0(4) . . . . ?
N4 C7 C8 N5 167.0(3) . . . . ?
N4 C7 C8 C9 -11.2(4) . . . . ?
C1 N1 C4 C3 1.8(4) . . . . ?
C1 N1 C4 C5 -178.8(2) . . . . ?
C2 N2 C3 C4 -0.1(4) . . . . ?
C3 N2 C2 C1 1.3(4) . . . . ?
C3 C4 C5 N3 172.5(2) . . . . ?
C3 C4 C5 C6 -6.3(4) . . . . ?
C4 N1 C1 C2 -0.7(4) . . . . ?
C5 N3 N4 C7 165.4(2) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.010 -0.013 0.001 13059 3471 ' '
2 0.250 0.250 0.250 90 10 ' '
3 0.750 0.250 0.250 90 10 ' '
4 0.750 0.250 0.750 90 10 ' '
5 0.250 0.250 0.750 90 10 ' '
6 0.250 0.750 0.250 90 10 ' '
7 0.750 0.750 0.250 90 10 ' '
8 0.750 0.750 0.750 90 10 ' '
9 0.250 0.750 0.750 90 10 ' '

_platon_squeeze_void_probe_radius 1.20
_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_a151118b_sq
_database_code_depnum_ccdc_archive 'CCDC 1864015'
_audit_update_record             
;
2018-09-13 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_audit_creation_date             2018-08-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.04(C672 H816 Gd48 N240 Ni24 O336)'
_chemical_formula_sum            'C28 H34 Gd2 N10 Ni O14'
_chemical_formula_weight         1107.86
_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 0.0181 0.0091 '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'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           206
_space_group_name_H-M_alt        'I a -3'
_space_group_name_Hall           '-I 2b 2c 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+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-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+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'

_cell_length_a                   32.6462(5)
_cell_length_b                   32.6462(5)
_cell_length_c                   32.6462(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     34793.6(16)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    3034
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.7750
_cell_measurement_theta_min      5.0510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.402
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             12960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11691
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.934
_diffrn_reflns_theta_max         66.934
_diffrn_reflns_theta_min         3.830
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -49.00  -1.00   1.00   27.54    --  -41.49  19.00  30.00   48
  2  ω     35.00 109.00   1.00   40.15    --  107.08 -95.00 150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0322844000
_diffrn_orient_matrix_UB_12      -0.0226594000
_diffrn_orient_matrix_UB_13      -0.0258823000
_diffrn_orient_matrix_UB_21      0.0178551000
_diffrn_orient_matrix_UB_22      0.0414117000
_diffrn_orient_matrix_UB_23      -0.0140442000
_diffrn_orient_matrix_UB_31      0.0294512000
_diffrn_orient_matrix_UB_32      -0.0001986000
_diffrn_orient_matrix_UB_33      0.0368298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3805
_reflns_number_total             5173
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.

The unit cell contains 48 ethanol molecules and 72 acetonitrile molecules 
 and 48 water molecules which have been treated as a diffuse 
contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON. 
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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         0.970
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.039
_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)+(0.0582P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1178
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: H2(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
4.a Riding coordinates:
 O2(H2), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Gd1 Gd 0.36401(2) 0.03353(2) 0.30082(2) 0.03689(12) Uani 1 1 d . . . . .
Ni1 Ni 0.47390(4) 0.000000 0.250000 0.0368(3) Uani 1 2 d S T P . .
O1 O 0.43699(11) 0.02492(11) 0.29742(11) 0.0359(9) Uani 1 1 d . . . . .
O2 O 0.55678(12) 0.01957(17) 0.28186(14) 0.0641(14) Uani 1 1 d . . . . .
H2 H 0.560440 0.019216 0.257004 0.096 Uiso 0.5 1 d R . . A -1
O6 O 0.39128(18) 0.10424(15) 0.30029(16) 0.0742(15) Uani 1 1 d . U . . .
O5 O 0.32248(19) 0.09481(18) 0.29453(18) 0.0856(17) Uani 1 1 d . U . . .
O3 O 0.37400(11) 0.03801(11) 0.22983(11) 0.0366(9) Uani 1 1 d . . . . .
O4 O 0.36571(12) 0.03319(12) 0.16360(12) 0.0454(10) Uani 1 1 d . . . . .
O7 O 0.29923(13) 0.00961(16) 0.28276(12) 0.0586(13) Uani 1 1 d . . . . .
N1 N 0.32211(15) 0.03737(15) 0.36747(15) 0.0422(12) Uani 1 1 d . . . . .
N2 N 0.28094(15) 0.03015(15) 0.44216(15) 0.0433(12) Uani 1 1 d . . . . .
N3 N 0.40304(15) 0.04346(14) 0.36638(14) 0.0397(11) Uani 1 1 d . . . . .
N4 N 0.44513(15) 0.04713(15) 0.36406(14) 0.0430(12) Uani 1 1 d . . . . .
N5 N 0.51628(15) 0.02129(17) 0.28981(15) 0.0464(12) Uani 1 1 d . . . . .
C1 C 0.34234(18) 0.03912(17) 0.40397(17) 0.0384(13) Uani 1 1 d . . . . .
C2 C 0.2819(2) 0.0325(2) 0.3692(2) 0.0550(17) Uani 1 1 d . . . . .
H2A H 0.267048 0.031097 0.344941 0.055(19) Uiso 1 1 calc R . . . .
C3 C 0.26113(19) 0.0292(2) 0.40665(18) 0.0478(15) Uani 1 1 d . . . . .
H3 H 0.232786 0.026401 0.406623 0.047(18) Uiso 1 1 calc R . . . .
C4 C 0.32157(18) 0.03558(17) 0.44029(17) 0.0389(13) Uani 1 1 d . . . . .
H4 H 0.336292 0.037001 0.464639 0.029(14) Uiso 1 1 calc R . . . .
C5 C 0.38675(18) 0.04434(17) 0.40219(18) 0.0396(13) Uani 1 1 d . . . . .
C6 C 0.4097(2) 0.0495(2) 0.4421(2) 0.0596(19) Uani 1 1 d . . . . .
H6A H 0.437956 0.055169 0.436516 0.09(3) Uiso 1 1 calc GR . . . .
H6B H 0.407554 0.024751 0.457880 0.09(3) Uiso 1 1 calc GR . . . .
H6C H 0.397990 0.071806 0.457297 0.07(2) Uiso 1 1 calc GR . . . .
C7 C 0.45882(18) 0.03754(17) 0.32817(17) 0.0393(13) Uani 1 1 d . . . . .
C8 C 0.50438(19) 0.0380(2) 0.32347(19) 0.0483(15) Uani 1 1 d . . . . .
C9 C 0.5326(2) 0.0547(3) 0.3550(2) 0.081(3) Uani 1 1 d . . . . .
H9A H 0.523077 0.047310 0.381770 0.122 Uiso 1 1 d R . . . .
H9B H 0.534327 0.084020 0.352930 0.122 Uiso 1 1 d R . . . .
H9C H 0.559217 0.043040 0.350430 0.122 Uiso 1 1 d R . . . .
C10 C 0.3544(3) 0.1185(3) 0.2980(3) 0.086(3) Uani 1 1 d . U . . .
C11 C 0.3493(4) 0.1636(3) 0.2900(4) 0.133(4) Uani 1 1 d . U . . .
H11A H 0.352509 0.174993 0.316928 0.200 Uiso 1 1 d R . . . .
H11B H 0.322539 0.170193 0.279718 0.200 Uiso 1 1 d R . . . .
H11C H 0.369729 0.174853 0.272108 0.200 Uiso 1 1 d R . . . .
C12 C 0.36652(18) 0.05455(17) 0.19530(18) 0.0403(13) Uani 1 1 d . . . . .
C13 C 0.3592(2) 0.09892(18) 0.19323(19) 0.0501(16) Uani 1 1 d . . . . .
H13A H 0.363575 0.108302 0.165701 0.08(2) Uiso 1 1 calc GR . . . .
H13B H 0.377732 0.112778 0.211368 0.038(16) Uiso 1 1 calc GR . . . .
H13C H 0.331495 0.104675 0.201249 0.12(4) Uiso 1 1 calc GR . . . .
C14 C 0.2819(3) 0.000000 0.250000 0.069(3) Uani 1 2 d S TU P . .
C15 C 0.2383(6) -0.0230(6) 0.2540(7) 0.114(7) Uani 0.5 1 d . U . B -1
H15A H 0.238280 -0.052198 0.257232 0.171 Uiso 0.5 1 d R . . B -1
H15B H 0.223880 -0.015788 0.229431 0.171 Uiso 0.5 1 d R . . B -1
H15C H 0.225090 -0.010558 0.277162 0.171 Uiso 0.5 1 d R . . B -1


_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
Gd1 Gd1 3.9753(6) 16_445 ?
Gd1 O1 2.402(4) . ?
Gd1 O6 2.474(5) . ?
Gd1 O5 2.426(5) . ?
Gd1 O3 2.345(4) . ?
Gd1 O3 2.562(4) 16_445 ?
Gd1 O4 2.469(4) 16_445 ?
Gd1 O7 2.330(4) . ?
Gd1 N1 2.573(5) . ?
Gd1 N3 2.512(5) . ?
Gd1 C12 2.880(6) 16_445 ?
Ni1 O1 2.124(4) 16_445 ?
Ni1 O1 2.124(4) . ?
Ni1 N2 2.146(5) 45 ?
Ni1 N2 2.146(5) 35_655 ?
Ni1 N5 2.022(5) 16_445 ?
Ni1 N5 2.022(5) . ?
O1 C7 1.298(6) . ?
O2 H2 0.8204 . ?
O2 N5 1.349(6) . ?
O6 C10 1.293(10) . ?
O5 C10 1.302(11) . ?
O3 C12 1.274(7) . ?
O4 C12 1.248(7) . ?
O7 C14 1.249(6) . ?
N1 C1 1.363(7) . ?
N1 C2 1.323(8) . ?
N2 C3 1.328(7) . ?
N2 C4 1.339(7) . ?
N3 N4 1.381(7) . ?
N3 C5 1.284(7) . ?
N4 C7 1.293(7) . ?
N5 C8 1.287(8) . ?
C1 C4 1.371(8) . ?
C1 C5 1.461(8) . ?
C2 H2A 0.9300 . ?
C2 C3 1.402(9) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C6 1.512(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.495(8) . ?
C8 C9 1.485(9) . ?
C9 H9A 0.9599 . ?
C9 H9B 0.9598 . ?
C9 H9C 0.9602 . ?
C10 C11 1.506(13) . ?
C11 H11A 0.9599 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9599 . ?
C12 C13 1.470(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.61(2) . ?
C15 H15A 0.9597 . ?
C15 H15B 0.9602 . ?
C15 H15C 0.9602 . ?

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 Gd1 Gd1 84.08(9) . 16_445 ?
O1 Gd1 O6 75.63(16) . . ?
O1 Gd1 O5 130.33(18) . . ?
O1 Gd1 O3 75.46(12) . 16_445 ?
O1 Gd1 O4 84.04(13) . 16_445 ?
O1 Gd1 N1 124.90(14) . . ?
O1 Gd1 N3 63.34(14) . . ?
O1 Gd1 C12 81.78(14) . 16_445 ?
O6 Gd1 Gd1 120.53(13) . 16_445 ?
O6 Gd1 O3 143.33(16) . 16_445 ?
O6 Gd1 N1 98.73(17) . . ?
O6 Gd1 N3 72.73(16) . . ?
O6 Gd1 C12 157.19(18) . 16_445 ?
O5 Gd1 Gd1 112.56(15) . 16_445 ?
O5 Gd1 O6 55.3(2) . . ?
O5 Gd1 O3 142.20(18) . 16_445 ?
O5 Gd1 O4 141.26(17) . 16_445 ?
O5 Gd1 N1 74.59(17) . . ?
O5 Gd1 N3 104.43(19) . . ?
O5 Gd1 C12 147.5(2) . 16_445 ?
O3 Gd1 Gd1 34.09(8) 16_445 16_445 ?
O3 Gd1 Gd1 37.76(9) . 16_445 ?
O3 Gd1 O1 79.84(13) . . ?
O3 Gd1 O6 83.39(16) . . ?
O3 Gd1 O5 86.71(16) . . ?
O3 Gd1 O3 69.70(14) . 16_445 ?
O3 Gd1 O4 121.12(13) . 16_445 ?
O3 Gd1 N1 155.04(14) . . ?
O3 Gd1 N1 116.25(14) 16_445 . ?
O3 Gd1 N3 139.78(14) . . ?
O3 Gd1 C12 26.25(14) 16_445 16_445 ?
O3 Gd1 C12 95.84(15) . 16_445 ?
O4 Gd1 Gd1 84.66(9) 16_445 16_445 ?
O4 Gd1 O6 144.91(16) 16_445 . ?
O4 Gd1 O3 51.44(12) 16_445 16_445 ?
O4 Gd1 N1 69.94(14) 16_445 . ?
O4 Gd1 N3 72.64(14) 16_445 . ?
O4 Gd1 C12 25.55(14) 16_445 16_445 ?
O7 Gd1 Gd1 66.69(10) . 16_445 ?
O7 Gd1 O1 148.15(14) . . ?
O7 Gd1 O6 129.60(18) . . ?
O7 Gd1 O5 75.4(2) . . ?
O7 Gd1 O3 73.21(14) . 16_445 ?
O7 Gd1 O3 84.09(14) . . ?
O7 Gd1 O4 81.01(16) . 16_445 ?
O7 Gd1 N1 75.39(15) . . ?
O7 Gd1 N3 135.98(15) . . ?
O7 Gd1 C12 72.68(17) . 16_445 ?
N1 Gd1 Gd1 137.11(11) . 16_445 ?
N1 Gd1 C12 91.52(16) . 16_445 ?
N3 Gd1 Gd1 141.47(10) . 16_445 ?
N3 Gd1 O3 112.70(13) . 16_445 ?
N3 Gd1 N1 62.79(16) . . ?
N3 Gd1 C12 94.42(16) . 16_445 ?
C12 Gd1 Gd1 59.12(12) 16_445 16_445 ?
O1 Ni1 O1 110.9(2) 16_445 . ?
O1 Ni1 N2 87.66(16) 16_445 45 ?
O1 Ni1 N2 88.34(16) . 45 ?
O1 Ni1 N2 88.34(16) 16_445 35_655 ?
O1 Ni1 N2 87.66(16) . 35_655 ?
N2 Ni1 N2 173.0(3) 35_655 45 ?
N5 Ni1 O1 171.37(18) 16_445 . ?
N5 Ni1 O1 171.37(18) . 16_445 ?
N5 Ni1 O1 77.75(17) 16_445 16_445 ?
N5 Ni1 O1 77.75(17) . . ?
N5 Ni1 N2 92.4(2) . 45 ?
N5 Ni1 N2 92.4(2) 16_445 35_655 ?
N5 Ni1 N2 92.4(2) 16_445 45 ?
N5 Ni1 N2 92.4(2) . 35_655 ?
N5 Ni1 N5 93.6(3) 16_445 . ?
Ni1 O1 Gd1 129.89(17) . . ?
C7 O1 Gd1 118.1(3) . . ?
C7 O1 Ni1 112.0(3) . . ?
N5 O2 H2 109.5 . . ?
C10 O6 Gd1 90.0(5) . . ?
C10 O5 Gd1 92.0(5) . . ?
Gd1 O3 Gd1 108.15(14) . 16_445 ?
C12 O3 Gd1 90.9(3) . 16_445 ?
C12 O3 Gd1 151.0(4) . . ?
C12 O4 Gd1 95.9(3) . 16_445 ?
C14 O7 Gd1 135.3(5) . . ?
C1 N1 Gd1 118.9(4) . . ?
C2 N1 Gd1 123.9(4) . . ?
C2 N1 C1 116.6(5) . . ?
C3 N2 Ni1 122.5(4) . 41 ?
C3 N2 C4 116.5(5) . . ?
C4 N2 Ni1 121.0(4) . 41 ?
N4 N3 Gd1 118.0(3) . . ?
C5 N3 Gd1 124.6(4) . . ?
C5 N3 N4 117.4(5) . . ?
C7 N4 N3 111.9(5) . . ?
O2 N5 Ni1 122.2(4) . . ?
C8 N5 Ni1 119.2(4) . . ?
C8 N5 O2 118.6(5) . . ?
N1 C1 C4 120.8(5) . . ?
N1 C1 C5 116.8(5) . . ?
C4 C1 C5 122.4(5) . . ?
N1 C2 H2A 119.1 . . ?
N1 C2 C3 121.7(6) . . ?
C3 C2 H2A 119.1 . . ?
N2 C3 C2 121.6(6) . . ?
N2 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
N2 C4 C1 122.7(6) . . ?
N2 C4 H4 118.6 . . ?
C1 C4 H4 118.6 . . ?
N3 C5 C1 116.4(5) . . ?
N3 C5 C6 125.6(6) . . ?
C1 C5 C6 118.0(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 C8 118.0(5) . . ?
N4 C7 O1 126.0(5) . . ?
N4 C7 C8 115.8(5) . . ?
N5 C8 C7 112.6(5) . . ?
N5 C8 C9 124.0(6) . . ?
C9 C8 C7 123.4(6) . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 110.8 . . ?
C8 C9 H9C 107.9 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.4 . . ?
O6 C10 O5 122.5(8) . . ?
O6 C10 C11 117.7(10) . . ?
O5 C10 C11 118.5(9) . . ?
C10 C11 H11A 102.0 . . ?
C10 C11 H11B 112.4 . . ?
C10 C11 H11C 113.7 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 Gd1 62.8(3) . 16_445 ?
O3 C12 C13 119.3(5) . . ?
O4 C12 Gd1 58.5(3) . 16_445 ?
O4 C12 O3 120.1(5) . . ?
O4 C12 C13 120.6(5) . . ?
C13 C12 Gd1 169.0(4) . 16_445 ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O7 C14 O7 126.3(10) . 16_445 ?
O7 C14 C15 116.4(9) . . ?
O7 C14 C15 110.6(9) 16_445 . ?
C14 C15 H15A 118.2 . . ?
C14 C15 H15B 104.6 . . ?
C14 C15 H15C 105.4 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C7 N4 14.5(8) . . . . ?
Gd1 O1 C7 C8 -171.0(4) . . . . ?
Gd1 O6 C10 O5 -4.2(9) . . . . ?
Gd1 O6 C10 C11 -170.9(8) . . . . ?
Gd1 O5 C10 O6 4.3(9) . . . . ?
Gd1 O5 C10 C11 170.9(8) . . . . ?
Gd1 O3 C12 Gd1 -132.2(7) . . . 16_445 ?
Gd1 O3 C12 O4 -12.7(6) 16_445 . . . ?
Gd1 O3 C12 O4 -144.9(5) . . . . ?
Gd1 O3 C12 C13 35.5(11) . . . . ?
Gd1 O3 C12 C13 167.8(5) 16_445 . . . ?
Gd1 O4 C12 O3 13.3(6) 16_445 . . . ?
Gd1 O4 C12 C13 -167.2(5) 16_445 . . . ?
Gd1 O7 C14 O7 20.9(3) . . . 16_445 ?
Gd1 O7 C14 C15 169.3(8) . . . . ?
Gd1 N1 C1 C4 -171.1(4) . . . . ?
Gd1 N1 C1 C5 8.1(7) . . . . ?
Gd1 N1 C2 C3 171.1(5) . . . . ?
Gd1 N3 N4 C7 -11.5(6) . . . . ?
Gd1 N3 C5 C1 0.0(7) . . . . ?
Gd1 N3 C5 C6 178.8(5) . . . . ?
Ni1 O1 C7 N4 -166.6(5) . . . . ?
Ni1 O1 C7 C8 7.9(6) . . . . ?
Ni1 N2 C3 C2 179.2(5) 41 . . . ?
Ni1 N2 C4 C1 -178.7(4) 41 . . . ?
Ni1 N5 C8 C7 1.9(7) . . . . ?
Ni1 N5 C8 C9 -179.9(6) . . . . ?
O1 C7 C8 N5 -6.8(8) . . . . ?
O1 C7 C8 C9 175.0(6) . . . . ?
O2 N5 C8 C7 -179.8(5) . . . . ?
O2 N5 C8 C9 -1.6(10) . . . . ?
N1 C1 C4 N2 0.2(9) . . . . ?
N1 C1 C5 N3 -5.5(8) . . . . ?
N1 C1 C5 C6 175.6(5) . . . . ?
N1 C2 C3 N2 -1.4(11) . . . . ?
N3 N4 C7 O1 -1.6(8) . . . . ?
N3 N4 C7 C8 -176.2(5) . . . . ?
N4 N3 C5 C1 -178.1(5) . . . . ?
N4 N3 C5 C6 0.7(9) . . . . ?
N4 C7 C8 N5 168.3(6) . . . . ?
N4 C7 C8 C9 -9.9(10) . . . . ?
C1 N1 C2 C3 0.0(10) . . . . ?
C2 N1 C1 C4 0.5(9) . . . . ?
C2 N1 C1 C5 179.7(5) . . . . ?
C3 N2 C4 C1 -1.5(9) . . . . ?
C4 N2 C3 C2 2.0(9) . . . . ?
C4 C1 C5 N3 173.7(5) . . . . ?
C4 C1 C5 C6 -5.2(9) . . . . ?
C5 N3 N4 C7 166.8(5) . . . . ?
C5 C1 C4 N2 -178.9(5) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 90 7 ' '
2 0.500 0.000 0.000 90 7 ' '
3 0.131 0.013 0.189 14037 3271 ' '
4 0.000 0.000 0.500 90 7 ' '
5 0.500 0.000 0.500 90 7 ' '
6 0.000 0.500 0.000 90 7 ' '
7 0.500 0.500 0.500 90 7 ' '
8 0.000 0.500 0.500 90 7 ' '
9 0.500 0.500 1.000 90 7 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.848
