# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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-Ce_complex_1
_database_code_depnum_ccdc_archive 'CCDC 1916431'
loop_
_audit_author_name
_audit_author_address
'Larry R. Falvello'
;University of Zaragoza
Spain
;
_audit_update_record             
;
2019-05-16 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
{(3-methoxy-2-oxidobenzylidene)ethylenediamine}-nickel(II)-trichlorido-aqua-cerium(III)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 Ce Cl3 N2 Ni O5'
_chemical_formula_sum            'C18 H20 Ce Cl3 N2 Ni O5'
_chemical_formula_weight         649.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.1269(3)
_cell_length_b                   14.4698(6)
_cell_length_c                   21.0732(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.014(4)
_cell_angle_gamma                90
_cell_volume                     2170.18(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    4431
_cell_measurement_theta_min      3.0620
_cell_measurement_theta_max      27.8260

_exptl_crystal_description       block
_exptl_crystal_colour            
;
dichroic red-orange and colourless
;
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_F_000             1276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    3.341
_shelx_estimated_absorpt_T_min   0.751
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            6159
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.653
_diffrn_reflns_theta_max         28.384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6159
_reflns_number_gt                4263
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6159
_refine_ls_number_parameters     280
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.1051
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.48229(6) 0.26022(3) 0.59221(2) 0.02408(12) Uani 1 1 d . . . . .
Ni1 Ni 0.49412(13) 0.23257(6) 0.75678(4) 0.0277(2) Uani 1 1 d . . . . .
O1 O 0.6283(8) 0.4323(3) 0.6072(3) 0.0350(15) Uani 1 1 d . . . . .
O2 O 0.5334(7) 0.3271(3) 0.7004(2) 0.0307(14) Uani 1 1 d . . . . .
O3 O 0.5207(7) 0.1591(3) 0.6864(2) 0.0284(14) Uani 1 1 d . . . . .
O4 O 0.6232(8) 0.0885(3) 0.5802(3) 0.0322(15) Uani 1 1 d . . . . .
N1 N 0.4713(9) 0.3087(4) 0.8251(3) 0.0340(18) Uani 1 1 d . . . . .
N2 N 0.4425(10) 0.1359(4) 0.8090(3) 0.0359(17) Uani 1 1 d . . . . .
C1 C 0.6943(12) 0.4878(5) 0.5575(4) 0.042(2) Uani 1 1 d . . . . .
H1A H 0.711432 0.450008 0.520811 0.062 Uiso 1 1 calc R U . . .
H1B H 0.812022 0.515487 0.571165 0.062 Uiso 1 1 calc R U . . .
H1C H 0.604209 0.535387 0.546938 0.062 Uiso 1 1 calc R U . . .
C2 C 0.5868(11) 0.4766(5) 0.6626(4) 0.0278(19) Uani 1 1 d . . . . .
C3 C 0.5907(11) 0.5704(5) 0.6699(4) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.620753 0.609313 0.636795 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5471(13) 0.6054(5) 0.7297(5) 0.043(3) Uani 1 1 d . . . . .
H4 H 0.549053 0.669087 0.735361 0.052 Uiso 1 1 calc R U . . .
C5 C 0.5011(12) 0.5502(5) 0.7810(4) 0.039(2) Uani 1 1 d . . . . .
H5 H 0.472704 0.575854 0.819789 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4998(12) 0.4544(5) 0.7712(4) 0.0301(19) Uani 1 1 d . . . . .
C7 C 0.5381(10) 0.4179(5) 0.7129(4) 0.0260(19) Uani 1 1 d . . . . .
C8 C 0.4692(11) 0.3971(6) 0.8238(4) 0.037(2) Uani 1 1 d . . . . .
H8 H 0.444823 0.426739 0.861671 0.044 Uiso 1 1 calc R U . . .
C9 C 0.4645(13) 0.2567(5) 0.8870(4) 0.052(2) Uani 1 1 d . . . . .
H9A H 0.590140 0.248853 0.906183 0.063 Uiso 1 1 calc R U . . .
H9B H 0.389547 0.290228 0.916456 0.063 Uiso 1 1 calc R U . . .
C10 C 0.3795(14) 0.1666(6) 0.8720(4) 0.054(3) Uani 1 1 d . . . . .
H10A H 0.243609 0.171541 0.870623 0.065 Uiso 1 1 calc R U . . .
H10B H 0.418049 0.121988 0.904453 0.065 Uiso 1 1 calc R U . . .
C11 C 0.4421(12) 0.0490(5) 0.7951(4) 0.038(2) Uani 1 1 d . . . . .
H11 H 0.408312 0.007865 0.826400 0.045 Uiso 1 1 calc R U . . .
C12 C 0.4892(11) 0.0111(5) 0.7355(4) 0.0316(18) Uani 1 1 d . . . . .
C13 C 0.4941(13) -0.0865(5) 0.7291(4) 0.039(2) Uani 1 1 d . . . . .
H13 H 0.462287 -0.124908 0.762267 0.047 Uiso 1 1 calc R U . . .
C14 C 0.5473(12) -0.1228(5) 0.6722(4) 0.040(2) Uani 1 1 d . . . . .
H14 H 0.557084 -0.186633 0.668118 0.049 Uiso 1 1 calc R U . . .
C15 C 0.5868(12) -0.0673(5) 0.6208(4) 0.038(2) Uani 1 1 d . . . . .
H15 H 0.616757 -0.094170 0.582495 0.045 Uiso 1 1 calc R U . . .
C16 C 0.5818(11) 0.0257(5) 0.6264(4) 0.0294(19) Uani 1 1 d . . . . .
C17 C 0.5290(10) 0.0666(5) 0.6830(4) 0.0236(19) Uani 1 1 d . . . . .
C18 C 0.7203(12) 0.0552(5) 0.5286(4) 0.036(2) Uani 1 1 d . . . . .
H18A H 0.752697 0.105905 0.501968 0.054 Uiso 1 1 calc R U . . .
H18B H 0.641794 0.012530 0.504512 0.054 Uiso 1 1 calc R U . . .
H18C H 0.832739 0.024232 0.544114 0.054 Uiso 1 1 calc R U . . .
O5 O 0.8360(7) 0.2603(4) 0.5971(4) 0.0477(16) Uani 1 1 d D . . . .
H1W H 0.906(8) 0.219(3) 0.583(4) 0.057 Uiso 1 1 d D U . . .
H2W H 0.909(7) 0.306(3) 0.602(4) 0.057 Uiso 1 1 d D U . . .
Cl1 Cl 0.5179(3) 0.27555(13) 0.46488(9) 0.0452(6) Uani 1 1 d . . . . .
Cl2 Cl 0.1864(3) 0.38799(14) 0.58595(13) 0.0450(6) Uani 1 1 d . . . . .
Cl3 Cl 0.1832(3) 0.13851(14) 0.56865(12) 0.0414(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O3 2.469(5) . ?
Ce1 O2 2.485(5) . ?
Ce1 O5 2.518(5) . ?
Ce1 O4 2.697(5) . ?
Ce1 O1 2.710(5) . ?
Ce1 Cl1 2.717(2) . ?
Ce1 Cl3 2.789(2) . ?
Ce1 Cl2 2.802(2) . ?
Ce1 Ni1 3.4876(10) . ?
Ni1 N1 1.827(6) . ?
Ni1 N2 1.829(7) . ?
Ni1 O3 1.843(5) . ?
Ni1 O2 1.843(5) . ?
O1 C2 1.378(9) . ?
O1 C1 1.420(9) . ?
O2 C7 1.340(7) . ?
O3 C17 1.342(8) . ?
O4 C16 1.375(9) . ?
O4 C18 1.405(9) . ?
N1 C8 1.279(9) . ?
N1 C9 1.508(9) . ?
N2 C11 1.291(9) . ?
N2 C10 1.492(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.365(9) . ?
C2 C7 1.415(10) . ?
C3 C4 1.408(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.378(10) . ?
C6 C8 1.411(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.465(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.427(11) . ?
C11 H11 0.9300 . ?
C12 C17 1.408(10) . ?
C12 C13 1.420(10) . ?
C13 C14 1.381(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.389(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.352(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.400(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O5 H1W 0.845(11) . ?
O5 H2W 0.842(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ce1 O2 59.27(15) . . ?
O3 Ce1 O5 84.21(19) . . ?
O2 Ce1 O5 82.19(19) . . ?
O3 Ce1 O4 60.21(15) . . ?
O2 Ce1 O4 114.04(16) . . ?
O5 Ce1 O4 68.12(17) . . ?
O3 Ce1 O1 115.14(17) . . ?
O2 Ce1 O1 59.89(16) . . ?
O5 Ce1 O1 67.50(16) . . ?
O4 Ce1 O1 135.61(16) . . ?
O3 Ce1 Cl1 146.07(12) . . ?
O2 Ce1 Cl1 148.97(12) . . ?
O5 Ce1 Cl1 83.97(18) . . ?
O4 Ce1 Cl1 85.87(12) . . ?
O1 Ce1 Cl1 89.15(13) . . ?
O3 Ce1 Cl3 79.64(13) . . ?
O2 Ce1 Cl3 118.88(12) . . ?
O5 Ce1 Cl3 139.62(13) . . ?
O4 Ce1 Cl3 71.72(13) . . ?
O1 Ce1 Cl3 152.36(13) . . ?
Cl1 Ce1 Cl3 89.19(7) . . ?
O3 Ce1 Cl2 118.70(13) . . ?
O2 Ce1 Cl2 81.95(13) . . ?
O5 Ce1 Cl2 138.67(13) . . ?
O4 Ce1 Cl2 152.43(13) . . ?
O1 Ce1 Cl2 71.51(13) . . ?
Cl1 Ce1 Cl2 90.50(7) . . ?
Cl3 Ce1 Cl2 80.92(6) . . ?
O3 Ce1 Ni1 30.35(11) . . ?
O2 Ce1 Ni1 30.46(11) . . ?
O5 Ce1 Ni1 89.29(17) . . ?
O4 Ce1 Ni1 89.88(11) . . ?
O1 Ce1 Ni1 90.01(13) . . ?
Cl1 Ce1 Ni1 173.00(5) . . ?
Cl3 Ce1 Ni1 94.75(6) . . ?
Cl2 Ce1 Ni1 95.82(6) . . ?
N1 Ni1 N2 87.6(3) . . ?
N1 Ni1 O3 178.0(2) . . ?
N2 Ni1 O3 94.3(2) . . ?
N1 Ni1 O2 94.8(2) . . ?
N2 Ni1 O2 176.1(3) . . ?
O3 Ni1 O2 83.3(2) . . ?
N1 Ni1 Ce1 135.7(2) . . ?
N2 Ni1 Ce1 133.7(2) . . ?
O3 Ni1 Ce1 42.59(14) . . ?
O2 Ni1 Ce1 43.12(15) . . ?
C2 O1 C1 117.1(6) . . ?
C2 O1 Ce1 115.4(4) . . ?
C1 O1 Ce1 125.0(5) . . ?
C7 O2 Ni1 127.1(5) . . ?
C7 O2 Ce1 124.3(4) . . ?
Ni1 O2 Ce1 106.41(19) . . ?
C17 O3 Ni1 128.7(4) . . ?
C17 O3 Ce1 123.5(4) . . ?
Ni1 O3 Ce1 107.06(19) . . ?
C16 O4 C18 117.0(6) . . ?
C16 O4 Ce1 116.6(4) . . ?
C18 O4 Ce1 126.2(4) . . ?
C8 N1 C9 121.1(7) . . ?
C8 N1 Ni1 126.0(5) . . ?
C9 N1 Ni1 112.9(5) . . ?
C11 N2 C10 119.7(7) . . ?
C11 N2 Ni1 127.3(6) . . ?
C10 N2 Ni1 112.8(5) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 123.6(7) . . ?
C3 C2 C7 121.2(7) . . ?
O1 C2 C7 115.2(6) . . ?
C2 C3 C4 116.9(8) . . ?
C2 C3 H3 121.5 . . ?
C4 C3 H3 121.5 . . ?
C5 C4 C3 124.0(7) . . ?
C5 C4 H4 118.0 . . ?
C3 C4 H4 118.0 . . ?
C4 C5 C6 116.8(8) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C7 C6 C5 120.7(8) . . ?
C7 C6 C8 121.4(7) . . ?
C5 C6 C8 117.8(8) . . ?
O2 C7 C6 123.2(7) . . ?
O2 C7 C2 116.5(7) . . ?
C6 C7 C2 120.3(6) . . ?
N1 C8 C6 127.0(7) . . ?
N1 C8 H8 116.5 . . ?
C6 C8 H8 116.5 . . ?
C10 C9 N1 106.8(7) . . ?
C10 C9 H9A 110.4 . . ?
N1 C9 H9A 110.4 . . ?
C10 C9 H9B 110.4 . . ?
N1 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
C9 C10 N2 108.5(7) . . ?
C9 C10 H10A 110.0 . . ?
N2 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
N2 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C12 125.2(8) . . ?
N2 C11 H11 117.4 . . ?
C12 C11 H11 117.4 . . ?
C17 C12 C13 119.1(7) . . ?
C17 C12 C11 122.6(7) . . ?
C13 C12 C11 118.3(7) . . ?
C14 C13 C12 118.0(8) . . ?
C14 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
C13 C14 C15 122.3(7) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 120.0(8) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 O4 126.0(7) . . ?
C15 C16 C17 120.3(8) . . ?
O4 C16 C17 113.6(6) . . ?
O3 C17 C16 118.8(6) . . ?
O3 C17 C12 121.1(7) . . ?
C16 C17 C12 120.1(7) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Ce1 O5 H1W 127(5) . . ?
Ce1 O5 H2W 128(4) . . ?
H1W O5 H2W 103(3) . . ?

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
N1 Ni1 O2 C7 -0.4(6) . . . . ?
O3 Ni1 O2 C7 -179.9(6) . . . . ?
Ce1 Ni1 O2 C7 163.6(7) . . . . ?
N1 Ni1 O2 Ce1 -164.0(3) . . . . ?
O3 Ni1 O2 Ce1 16.5(2) . . . . ?
N2 Ni1 O3 C17 -9.8(6) . . . . ?
O2 Ni1 O3 C17 173.3(6) . . . . ?
Ce1 Ni1 O3 C17 -170.0(7) . . . . ?
N2 Ni1 O3 Ce1 160.3(3) . . . . ?
O2 Ni1 O3 Ce1 -16.6(2) . . . . ?
N2 Ni1 N1 C8 -171.5(7) . . . . ?
O2 Ni1 N1 C8 5.5(7) . . . . ?
Ce1 Ni1 N1 C8 -10.1(8) . . . . ?
N2 Ni1 N1 C9 11.6(6) . . . . ?
O2 Ni1 N1 C9 -171.5(5) . . . . ?
Ce1 Ni1 N1 C9 172.9(4) . . . . ?
N1 Ni1 N2 C11 -175.9(7) . . . . ?
O3 Ni1 N2 C11 3.7(7) . . . . ?
Ce1 Ni1 N2 C11 22.1(9) . . . . ?
N1 Ni1 N2 C10 9.6(6) . . . . ?
O3 Ni1 N2 C10 -170.9(6) . . . . ?
Ce1 Ni1 N2 C10 -152.4(5) . . . . ?
C1 O1 C2 C3 5.7(11) . . . . ?
Ce1 O1 C2 C3 -157.2(6) . . . . ?
C1 O1 C2 C7 -174.4(7) . . . . ?
Ce1 O1 C2 C7 22.6(8) . . . . ?
O1 C2 C3 C4 -179.2(8) . . . . ?
C7 C2 C3 C4 1.0(12) . . . . ?
C2 C3 C4 C5 0.0(13) . . . . ?
C3 C4 C5 C6 0.2(14) . . . . ?
C4 C5 C6 C7 -1.5(13) . . . . ?
C4 C5 C6 C8 174.8(8) . . . . ?
Ni1 O2 C7 C6 -4.8(10) . . . . ?
Ce1 O2 C7 C6 156.1(6) . . . . ?
Ni1 O2 C7 C2 174.7(5) . . . . ?
Ce1 O2 C7 C2 -24.4(9) . . . . ?
C5 C6 C7 O2 -178.0(7) . . . . ?
C8 C6 C7 O2 5.8(13) . . . . ?
C5 C6 C7 C2 2.5(12) . . . . ?
C8 C6 C7 C2 -173.7(8) . . . . ?
C3 C2 C7 O2 178.2(7) . . . . ?
O1 C2 C7 O2 -1.6(10) . . . . ?
C3 C2 C7 C6 -2.3(12) . . . . ?
O1 C2 C7 C6 177.9(7) . . . . ?
C9 N1 C8 C6 170.9(8) . . . . ?
Ni1 N1 C8 C6 -5.9(12) . . . . ?
C7 C6 C8 N1 -0.3(14) . . . . ?
C5 C6 C8 N1 -176.7(8) . . . . ?
C8 N1 C9 C10 153.2(8) . . . . ?
Ni1 N1 C9 C10 -29.7(9) . . . . ?
N1 C9 C10 N2 35.7(10) . . . . ?
C11 N2 C10 C9 156.3(8) . . . . ?
Ni1 N2 C10 C9 -28.6(10) . . . . ?
C10 N2 C11 C12 176.5(9) . . . . ?
Ni1 N2 C11 C12 2.3(13) . . . . ?
N2 C11 C12 C17 -4.8(14) . . . . ?
N2 C11 C12 C13 175.9(8) . . . . ?
C17 C12 C13 C14 3.3(13) . . . . ?
C11 C12 C13 C14 -177.4(8) . . . . ?
C12 C13 C14 C15 -3.2(14) . . . . ?
C13 C14 C15 C16 2.9(14) . . . . ?
C14 C15 C16 O4 177.9(8) . . . . ?
C14 C15 C16 C17 -2.8(13) . . . . ?
C18 O4 C16 C15 -15.8(12) . . . . ?
Ce1 O4 C16 C15 158.7(7) . . . . ?
C18 O4 C16 C17 164.8(7) . . . . ?
Ce1 O4 C16 C17 -20.6(9) . . . . ?
Ni1 O3 C17 C16 -169.1(6) . . . . ?
Ce1 O3 C17 C16 22.4(9) . . . . ?
Ni1 O3 C17 C12 9.6(10) . . . . ?
Ce1 O3 C17 C12 -158.9(6) . . . . ?
C15 C16 C17 O3 -178.3(7) . . . . ?
O4 C16 C17 O3 1.1(11) . . . . ?
C15 C16 C17 C12 3.0(13) . . . . ?
O4 C16 C17 C12 -177.6(7) . . . . ?
C13 C12 C17 O3 178.1(7) . . . . ?
C11 C12 C17 O3 -1.3(12) . . . . ?
C13 C12 C17 C16 -3.2(12) . . . . ?
C11 C12 C17 C16 177.4(8) . . . . ?

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
C1 H1C Cl1 0.96 2.88 3.763(8) 153.9 3_666 yes
C3 H3 Cl1 0.93 2.85 3.661(9) 146.4 3_666 yes
C10 H10A Cl1 0.97 2.73 3.421(9) 128.6 4_566 yes
C11 H11 Cl2 0.93 2.65 3.577(8) 178.9 2_546 yes
C15 H15 Cl1 0.93 2.95 3.571(8) 125.4 3_656 yes
C18 H18C Cl3 0.96 3.02 3.572(9) 118.1 1_655 yes
C18 H18B Cl3 0.96 2.99 3.560(8) 119.7 3_656 yes
O5 H1W Cl3 0.845(11) 2.32(3) 3.122(5) 157(7) 1_655 yes
O5 H2W Cl2 0.842(11) 2.35(3) 3.125(5) 154(6) 1_655 yes

_refine_diff_density_max         0.708
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.161


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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-Gd_complex_2
_database_code_depnum_ccdc_archive 'CCDC 1916432'
loop_
_audit_author_name
_audit_author_address
'Larry R. Falvello'
;University of Zaragoza
Spain
;
_audit_update_record             
;
2019-05-16 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
{(3-methoxy-2-oxidobenzylidene)ethylenediamine}-nickel(II)-trichlorido-aqua-gadolinium(III)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 Cl3 Gd N2 Ni O5'
_chemical_formula_sum            'C18 H20 Cl3 Gd N2 Ni O5'
_chemical_formula_weight         666.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.0236(3)
_cell_length_b                   14.3753(9)
_cell_length_c                   20.9662(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.216(5)
_cell_angle_gamma                90
_cell_volume                     2115.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1050
_cell_measurement_theta_min      3.4210
_cell_measurement_theta_max      24.2040

_exptl_crystal_description       block
_exptl_crystal_colour            
;
pale pink
;
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    4.411
_shelx_estimated_absorpt_T_min   0.512
_shelx_estimated_absorpt_T_max   0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            9912
_diffrn_reflns_av_unetI/netI     0.1548
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.230
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3716
_reflns_number_gt                2084
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3716
_refine_ls_number_parameters     277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.943
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.48430(7) 0.25940(4) 0.59369(3) 0.02612(16) Uani 1 1 d . . . . .
Ni1 Ni 0.49249(18) 0.23287(10) 0.75472(6) 0.0286(4) Uani 1 1 d . . . . .
O1 O 0.6301(11) 0.4295(5) 0.6049(4) 0.033(2) Uani 1 1 d . . . . .
O2 O 0.5325(10) 0.3273(5) 0.6974(3) 0.035(2) Uani 1 1 d . . . . .
O3 O 0.5196(10) 0.1594(5) 0.6842(3) 0.031(2) Uani 1 1 d . . . . .
O4 O 0.6266(11) 0.0907(4) 0.5776(3) 0.030(2) Uani 1 1 d . . . . .
N1 N 0.4693(12) 0.3073(6) 0.8240(4) 0.035(3) Uani 1 1 d . . . . .
N2 N 0.4386(13) 0.1363(7) 0.8076(4) 0.031(3) Uani 1 1 d . . . . .
C1 C 0.7063(17) 0.4832(7) 0.5536(5) 0.042(3) Uani 1 1 d . . . . .
H1A H 0.726981 0.443188 0.517844 0.063 Uiso 1 1 calc R U . . .
H1B H 0.617572 0.531215 0.541060 0.063 Uiso 1 1 calc R U . . .
H1C H 0.824935 0.510803 0.567759 0.063 Uiso 1 1 calc R U . . .
C2 C 0.5911(16) 0.4760(7) 0.6607(6) 0.028(3) Uani 1 1 d . . . . .
C3 C 0.5945(15) 0.5703(7) 0.6666(6) 0.033(3) Uani 1 1 d . . . . .
H3 H 0.621745 0.608598 0.632344 0.040 Uiso 1 1 calc R U . . .
C4 C 0.5543(17) 0.6076(8) 0.7275(6) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.559169 0.671770 0.733108 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5095(16) 0.5540(8) 0.7774(6) 0.042(3) Uani 1 1 d . . . . .
H5 H 0.484584 0.580451 0.816691 0.051 Uiso 1 1 calc R U . . .
C6 C 0.5010(17) 0.4555(7) 0.7687(6) 0.031(3) Uani 1 1 d . . . . .
C7 C 0.5393(16) 0.4182(7) 0.7107(6) 0.027(3) Uani 1 1 d . . . . .
C8 C 0.4688(16) 0.3974(9) 0.8234(6) 0.029(3) Uani 1 1 d . . . . .
H8 H 0.450(14) 0.428(6) 0.860(5) 0.035 Uiso 1 1 d . U . . .
C9 C 0.4567(17) 0.2592(8) 0.8833(5) 0.053(3) Uani 1 1 d . . . . .
H9A H 0.377429 0.294169 0.911693 0.064 Uiso 1 1 calc R U . . .
H9B H 0.582511 0.253043 0.903621 0.064 Uiso 1 1 calc R U . . .
C10 C 0.3732(17) 0.1660(7) 0.8715(5) 0.043(3) Uani 1 1 d . . . . .
H10A H 0.235228 0.168969 0.871286 0.052 Uiso 1 1 calc R U . . .
H10B H 0.417101 0.122598 0.904227 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4405(18) 0.0485(9) 0.7934(7) 0.037(3) Uani 1 1 d . . . . .
H11 H 0.418(14) 0.004(7) 0.825(5) 0.045 Uiso 1 1 d . U . . .
C12 C 0.4884(15) 0.0097(7) 0.7337(6) 0.029(3) Uani 1 1 d . . . . .
C13 C 0.4966(16) -0.0881(7) 0.7254(6) 0.037(4) Uani 1 1 d . . . . .
H13 H 0.465311 -0.127625 0.758482 0.045 Uiso 1 1 calc R U . . .
C14 C 0.5504(16) -0.1236(7) 0.6688(6) 0.036(3) Uani 1 1 d . . . . .
H14 H 0.558806 -0.187841 0.664422 0.043 Uiso 1 1 calc R U . . .
C15 C 0.5932(15) -0.0676(7) 0.6174(5) 0.033(3) Uani 1 1 d . . . . .
H15 H 0.626948 -0.094111 0.579019 0.040 Uiso 1 1 calc R U . . .
C16 C 0.5852(15) 0.0264(7) 0.6239(6) 0.027(3) Uani 1 1 d . . . . .
C17 C 0.5302(14) 0.0655(7) 0.6823(6) 0.021(3) Uani 1 1 d . . . . .
C18 C 0.7289(16) 0.0578(7) 0.5245(5) 0.039(3) Uani 1 1 d . . . . .
H18A H 0.749353 0.108282 0.495591 0.058 Uiso 1 1 calc R U . . .
H18B H 0.849522 0.032995 0.539337 0.058 Uiso 1 1 calc R U . . .
H18C H 0.656392 0.009879 0.502777 0.058 Uiso 1 1 calc R U . . .
O5 O 0.8252(8) 0.2592(5) 0.5995(3) 0.045(2) Uani 1 1 d . . . . .
H1W H 0.898929 0.213430 0.594734 0.054 Uiso 1 1 d R U . . .
H2W H 0.899119 0.308589 0.600103 0.054 Uiso 1 1 d R U . . .
Cl1 Cl 0.5225(4) 0.27589(19) 0.46993(13) 0.0431(8) Uani 1 1 d . . . . .
Cl2 Cl 0.1921(4) 0.38308(18) 0.58916(16) 0.0445(9) Uani 1 1 d . . . . .
Cl3 Cl 0.1893(4) 0.14102(18) 0.57097(16) 0.0413(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.385(7) . ?
Gd1 O2 2.396(7) . ?
Gd1 O5 2.393(6) . ?
Gd1 Cl1 2.630(3) . ?
Gd1 O4 2.650(7) . ?
Gd1 O1 2.658(7) . ?
Gd1 Cl3 2.709(3) . ?
Gd1 Cl2 2.714(3) . ?
Gd1 Ni1 3.3959(14) . ?
Ni1 N1 1.816(9) . ?
Ni1 N2 1.825(9) . ?
Ni1 O3 1.833(7) . ?
Ni1 O2 1.842(7) . ?
O1 C2 1.384(12) . ?
O1 C1 1.443(12) . ?
O2 C7 1.335(11) . ?
O3 C17 1.353(11) . ?
O4 C16 1.379(12) . ?
O4 C18 1.430(11) . ?
N1 C8 1.295(13) . ?
N1 C9 1.430(12) . ?
N2 C11 1.297(13) . ?
N2 C10 1.495(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.362(13) . ?
C2 C7 1.398(14) . ?
C3 C4 1.425(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.347(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.429(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.365(14) . ?
C6 C8 1.444(15) . ?
C8 H8 0.90(9) . ?
C9 C10 1.479(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.422(16) . ?
C11 H11 0.95(10) . ?
C12 C17 1.384(14) . ?
C12 C13 1.417(13) . ?
C13 C14 1.358(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.360(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.416(14) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O5 H1W 0.8452 . ?
O5 H2W 0.8795 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Gd1 O2 61.1(2) . . ?
O3 Gd1 O5 83.4(2) . . ?
O2 Gd1 O5 81.3(2) . . ?
O3 Gd1 Cl1 145.86(17) . . ?
O2 Gd1 Cl1 147.43(18) . . ?
O5 Gd1 Cl1 84.86(17) . . ?
O3 Gd1 O4 61.4(2) . . ?
O2 Gd1 O4 116.6(2) . . ?
O5 Gd1 O4 67.9(2) . . ?
Cl1 Gd1 O4 84.47(17) . . ?
O3 Gd1 O1 117.1(2) . . ?
O2 Gd1 O1 60.3(2) . . ?
O5 Gd1 O1 67.4(2) . . ?
Cl1 Gd1 O1 87.16(18) . . ?
O4 Gd1 O1 135.0(2) . . ?
O3 Gd1 Cl3 79.44(19) . . ?
O2 Gd1 Cl3 119.72(18) . . ?
O5 Gd1 Cl3 139.92(18) . . ?
Cl1 Gd1 Cl3 89.41(10) . . ?
O4 Gd1 Cl3 72.08(17) . . ?
O1 Gd1 Cl3 151.99(18) . . ?
O3 Gd1 Cl2 118.54(17) . . ?
O2 Gd1 Cl2 81.08(19) . . ?
O5 Gd1 Cl2 139.16(18) . . ?
Cl1 Gd1 Cl2 90.71(9) . . ?
O4 Gd1 Cl2 152.07(18) . . ?
O1 Gd1 Cl2 71.87(18) . . ?
Cl3 Gd1 Cl2 80.39(8) . . ?
O3 Gd1 Ni1 31.17(16) . . ?
O2 Gd1 Ni1 31.46(16) . . ?
O5 Gd1 Ni1 88.31(15) . . ?
Cl1 Gd1 Ni1 173.06(7) . . ?
O4 Gd1 Ni1 91.80(16) . . ?
O1 Gd1 Ni1 91.38(17) . . ?
Cl3 Gd1 Ni1 95.03(8) . . ?
Cl2 Gd1 Ni1 95.29(8) . . ?
N1 Ni1 N2 86.3(4) . . ?
N1 Ni1 O3 178.8(4) . . ?
N2 Ni1 O3 94.7(4) . . ?
N1 Ni1 O2 96.2(4) . . ?
N2 Ni1 O2 175.8(4) . . ?
O3 Ni1 O2 82.8(3) . . ?
N1 Ni1 Gd1 136.9(3) . . ?
N2 Ni1 Gd1 133.9(3) . . ?
O3 Ni1 Gd1 42.3(2) . . ?
O2 Ni1 Gd1 42.8(2) . . ?
C2 O1 C1 117.6(8) . . ?
C2 O1 Gd1 115.5(6) . . ?
C1 O1 Gd1 125.4(6) . . ?
C7 O2 Ni1 126.2(7) . . ?
C7 O2 Gd1 126.2(7) . . ?
Ni1 O2 Gd1 105.8(3) . . ?
C17 O3 Ni1 127.3(6) . . ?
C17 O3 Gd1 125.6(6) . . ?
Ni1 O3 Gd1 106.5(3) . . ?
C16 O4 C18 116.9(8) . . ?
C16 O4 Gd1 115.7(6) . . ?
C18 O4 Gd1 127.2(6) . . ?
C8 N1 C9 119.4(10) . . ?
C8 N1 Ni1 125.6(8) . . ?
C9 N1 Ni1 114.9(7) . . ?
C11 N2 C10 119.3(9) . . ?
C11 N2 Ni1 126.6(9) . . ?
C10 N2 Ni1 113.9(7) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 123.7(11) . . ?
C3 C2 C7 121.9(11) . . ?
O1 C2 C7 114.4(9) . . ?
C2 C3 C4 116.9(11) . . ?
C2 C3 H3 121.5 . . ?
C4 C3 H3 121.5 . . ?
C5 C4 C3 122.8(11) . . ?
C5 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
C4 C5 C6 118.6(12) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C7 C6 C5 119.7(11) . . ?
C7 C6 C8 121.5(10) . . ?
C5 C6 C8 118.6(11) . . ?
O2 C7 C6 124.3(10) . . ?
O2 C7 C2 115.7(10) . . ?
C6 C7 C2 120.1(10) . . ?
N1 C8 C6 125.8(11) . . ?
N1 C8 H8 119(6) . . ?
C6 C8 H8 115(6) . . ?
N1 C9 C10 109.2(9) . . ?
N1 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
N1 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 N2 106.0(9) . . ?
C9 C10 H10A 110.5 . . ?
N2 C10 H10A 110.5 . . ?
C9 C10 H10B 110.5 . . ?
N2 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
N2 C11 C12 126.0(11) . . ?
N2 C11 H11 120(7) . . ?
C12 C11 H11 114(7) . . ?
C17 C12 C13 117.9(11) . . ?
C17 C12 C11 121.5(10) . . ?
C13 C12 C11 120.6(11) . . ?
C14 C13 C12 119.7(11) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 122.4(11) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 119.2(11) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 O4 125.9(10) . . ?
C15 C16 C17 119.7(10) . . ?
O4 C16 C17 114.5(9) . . ?
O3 C17 C12 122.9(10) . . ?
O3 C17 C16 116.0(9) . . ?
C12 C17 C16 121.1(10) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Gd1 O5 H1W 127.7 . . ?
Gd1 O5 H2W 126.0 . . ?
H1W O5 H2W 105.5 . . ?

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
C1 H1A Cl1 0.96 2.96 3.667(11) 131.7 . yes
C1 H1B Cl1 0.96 2.95 3.842(11) 155.4 3_666 yes
C3 H3 Cl1 0.93 2.87 3.684(12) 147.4 3_666 yes
C9 H9A Cl1 0.97 2.99 3.644(11) 125.6 4_566 yes
C10 H10A Cl1 0.97 2.72 3.379(11) 126.1 4_566 yes
C11 H11 Cl2 0.95(10) 2.63(10) 3.572(13) 173(9) 2_546 yes
C15 H15 Cl1 0.93 2.98 3.587(11) 123.9 3_656 yes
C18 H18A Cl1 0.96 2.93 3.621(11) 130.2 . yes
C18 H18B Cl3 0.96 2.90 3.549(12) 125.7 1_655 yes
C18 H18C Cl3 0.96 2.90 3.548(10) 125.9 3_656 yes
O5 H1W Cl3 0.85 2.36 3.146(7) 155.0 1_655 yes
O5 H2W Cl2 0.88 2.34 3.147(7) 152.8 1_655 yes

_refine_diff_density_max         1.613
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.190


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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-Dy_complex_3
_database_code_depnum_ccdc_archive 'CCDC 1916433'
loop_
_audit_author_name
_audit_author_address
'Larry R. Falvello'
;University of Zaragoza
Spain
;
_audit_update_record             
;
2019-05-16 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
{(3-methoxy-2-oxidobenzylidene)ethylenediamine}-nickel(II)-trichlorido-aqua-dysprosium(III)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 Cl3 Dy N2 Ni O5'
_chemical_formula_sum            'C18 H20 Cl3 Dy N2 Ni O5'
_chemical_formula_weight         671.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.00940(10)
_cell_length_b                   14.3916(3)
_cell_length_c                   20.9556(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.833(2)
_cell_angle_gamma                90
_cell_volume                     2112.85(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8257
_cell_measurement_theta_min      3.0940
_cell_measurement_theta_max      28.8870

_exptl_crystal_description       rombic
_exptl_crystal_colour            
;
red/colorless dichroic
;
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.813
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_reflns_number            26349
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.831
_diffrn_reflns_theta_max         30.302
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5820
_reflns_number_gt                4431
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0242P)²+0.1475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5820
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.48421(2) 0.25899(2) 0.59405(2) 0.02261(6) Uani 1 1 d . . . . .
Ni1 Ni 0.49159(6) 0.23280(3) 0.75409(2) 0.02495(11) Uani 1 1 d . . . . .
O1 O 0.6291(3) 0.42909(16) 0.60238(13) 0.0326(6) Uani 1 1 d . . . . .
O2 O 0.5329(3) 0.32643(16) 0.69614(12) 0.0307(6) Uani 1 1 d . . . . .
O3 O 0.5183(3) 0.16017(15) 0.68254(12) 0.0282(6) Uani 1 1 d . . . . .
O4 O 0.6271(3) 0.09087(15) 0.57670(12) 0.0293(6) Uani 1 1 d . . . . .
N2 N 0.4387(4) 0.1357(2) 0.80754(15) 0.0297(7) Uani 1 1 d . . . . .
N1 N 0.4698(4) 0.3093(2) 0.82348(15) 0.0322(7) Uani 1 1 d . . . . .
C1 C 0.7102(6) 0.4825(3) 0.5514(2) 0.0403(10) Uani 1 1 d . . . . .
H1A H 0.731208 0.442600 0.515582 0.061 Uiso 1 1 calc R U . . .
H1B H 0.623633 0.531319 0.538734 0.061 Uiso 1 1 calc R U . . .
H1C H 0.829386 0.508993 0.566029 0.061 Uiso 1 1 calc R U . . .
C2 C 0.5894(5) 0.4757(2) 0.65791(19) 0.0283(8) Uani 1 1 d . . . . .
C3 C 0.5962(5) 0.5705(2) 0.6662(2) 0.0345(9) Uani 1 1 d . . . . .
H3 H 0.628069 0.608981 0.632473 0.041 Uiso 1 1 calc R U . . .
C4 C 0.5549(5) 0.6089(3) 0.7257(2) 0.0394(10) Uani 1 1 d . . . . .
H4 H 0.558595 0.672972 0.731106 0.047 Uiso 1 1 calc R U . . .
C5 C 0.5093(5) 0.5534(3) 0.7756(2) 0.0352(10) Uani 1 1 d . . . . .
H5 H 0.482692 0.579837 0.814836 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5025(5) 0.4559(2) 0.76810(19) 0.0282(8) Uani 1 1 d . . . . .
C7 C 0.5398(5) 0.4176(2) 0.70824(19) 0.0272(8) Uani 1 1 d . . . . .
C8 C 0.4685(5) 0.3990(3) 0.8225(2) 0.0354(9) Uani 1 1 d . . . . .
H8 H 0.443123 0.429308 0.860487 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4607(7) 0.2579(3) 0.8845(2) 0.0503(12) Uani 1 1 d . . . . .
H9A H 0.383502 0.291772 0.914250 0.060 Uiso 1 1 calc R U . . .
H9B H 0.587869 0.250444 0.903442 0.060 Uiso 1 1 calc R U . . .
C10 C 0.3743(6) 0.1654(3) 0.8704(2) 0.0455(11) Uani 1 1 d . . . . .
H10A H 0.414677 0.120855 0.902869 0.055 Uiso 1 1 calc R U . . .
H10B H 0.236178 0.169681 0.870006 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4384(5) 0.0483(3) 0.7932(2) 0.0331(9) Uani 1 1 d . . . . .
H11 H 0.402729 0.006679 0.824621 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4889(5) 0.0105(2) 0.73237(19) 0.0279(8) Uani 1 1 d . . . . .
C13 C 0.4980(5) -0.0868(2) 0.7253(2) 0.0347(10) Uani 1 1 d . . . . .
H13 H 0.469927 -0.125453 0.759346 0.042 Uiso 1 1 calc R U . . .
C14 C 0.5484(5) -0.1240(3) 0.6683(2) 0.0386(10) Uani 1 1 d . . . . .
H14 H 0.552514 -0.188239 0.663871 0.046 Uiso 1 1 calc R U . . .
C15 C 0.5942(5) -0.0678(2) 0.6163(2) 0.0317(9) Uani 1 1 d . . . . .
H15 H 0.630082 -0.094200 0.578023 0.038 Uiso 1 1 calc R U . . .
C16 C 0.5849(5) 0.0271(2) 0.62318(19) 0.0266(8) Uani 1 1 d . . . . .
C17 C 0.5288(5) 0.0672(2) 0.68087(18) 0.0254(8) Uani 1 1 d . . . . .
C18 C 0.7305(5) 0.0576(3) 0.52311(19) 0.0352(9) Uani 1 1 d . . . . .
H18A H 0.751376 0.108007 0.494139 0.053 Uiso 1 1 calc R U . . .
H18B H 0.851184 0.032835 0.537843 0.053 Uiso 1 1 calc R U . . .
H18C H 0.657897 0.009800 0.501561 0.053 Uiso 1 1 calc R U . . .
O5 O 0.8232(4) 0.25875(17) 0.60025(17) 0.0424(8) Uani 1 1 d D . . . .
H1W H 0.896(4) 0.2149(15) 0.592(2) 0.051 Uiso 1 1 d D U . . .
H2W H 0.890(4) 0.3067(13) 0.597(2) 0.051 Uiso 1 1 d D U . . .
Cl1 Cl 0.51893(15) 0.27574(7) 0.47141(5) 0.0402(2) Uani 1 1 d . . . . .
Cl2 Cl 0.19309(13) 0.38129(6) 0.59066(6) 0.0404(3) Uani 1 1 d . . . . .
Cl3 Cl 0.19010(13) 0.14146(6) 0.57186(6) 0.0392(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O3 2.343(2) . ?
Dy1 O2 2.364(3) . ?
Dy1 O5 2.375(3) . ?
Dy1 Cl1 2.6005(10) . ?
Dy1 O4 2.648(2) . ?
Dy1 O1 2.654(2) . ?
Dy1 Cl2 2.6940(9) . ?
Dy1 Cl3 2.6955(9) . ?
Dy1 Ni1 3.3735(5) . ?
Ni1 N1 1.834(3) . ?
Ni1 N2 1.836(3) . ?
Ni1 O3 1.842(2) . ?
Ni1 O2 1.843(2) . ?
O1 C2 1.379(4) . ?
O1 C1 1.447(4) . ?
O2 C7 1.337(4) . ?
O3 C17 1.341(4) . ?
O4 C16 1.378(4) . ?
O4 C18 1.438(4) . ?
N2 C11 1.293(4) . ?
N2 C10 1.470(5) . ?
N1 C8 1.291(5) . ?
N1 C9 1.480(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.377(5) . ?
C2 C7 1.398(5) . ?
C3 C4 1.402(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.413(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.402(5) . ?
C6 C8 1.429(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.488(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.441(5) . ?
C11 H11 0.9300 . ?
C12 C17 1.388(5) . ?
C12 C13 1.410(5) . ?
C13 C14 1.366(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.402(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.407(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O5 H1W 0.836(10) . ?
O5 H2W 0.836(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Dy1 O2 61.63(8) . . ?
O3 Dy1 O5 83.06(10) . . ?
O2 Dy1 O5 80.56(10) . . ?
O3 Dy1 Cl1 145.89(6) . . ?
O2 Dy1 Cl1 147.24(6) . . ?
O5 Dy1 Cl1 85.93(9) . . ?
O3 Dy1 O4 61.62(8) . . ?
O2 Dy1 O4 117.07(8) . . ?
O5 Dy1 O4 67.92(8) . . ?
Cl1 Dy1 O4 84.33(6) . . ?
O3 Dy1 O1 118.60(8) . . ?
O2 Dy1 O1 61.18(8) . . ?
O5 Dy1 O1 67.53(8) . . ?
Cl1 Dy1 O1 86.08(6) . . ?
O4 Dy1 O1 134.92(8) . . ?
O3 Dy1 Cl2 118.39(6) . . ?
O2 Dy1 Cl2 80.96(6) . . ?
O5 Dy1 Cl2 139.28(6) . . ?
Cl1 Dy1 Cl2 90.47(3) . . ?
O4 Dy1 Cl2 151.99(6) . . ?
O1 Dy1 Cl2 71.76(6) . . ?
O3 Dy1 Cl3 79.27(6) . . ?
O2 Dy1 Cl3 120.08(6) . . ?
O5 Dy1 Cl3 140.05(6) . . ?
Cl1 Dy1 Cl3 89.02(3) . . ?
O4 Dy1 Cl3 72.16(6) . . ?
O1 Dy1 Cl3 151.54(6) . . ?
Cl2 Dy1 Cl3 80.27(3) . . ?
O3 Dy1 Ni1 31.52(6) . . ?
O2 Dy1 Ni1 31.68(6) . . ?
O5 Dy1 Ni1 87.82(9) . . ?
Cl1 Dy1 Ni1 173.66(3) . . ?
O4 Dy1 Ni1 92.33(6) . . ?
O1 Dy1 Ni1 92.52(6) . . ?
Cl2 Dy1 Ni1 94.97(3) . . ?
Cl3 Dy1 Ni1 95.09(3) . . ?
N1 Ni1 N2 87.10(14) . . ?
N1 Ni1 O3 177.51(12) . . ?
N2 Ni1 O3 95.32(12) . . ?
N1 Ni1 O2 95.87(13) . . ?
N2 Ni1 O2 175.90(13) . . ?
O3 Ni1 O2 81.74(11) . . ?
N1 Ni1 Dy1 136.23(10) . . ?
N2 Ni1 Dy1 134.00(10) . . ?
O3 Ni1 Dy1 41.67(7) . . ?
O2 Ni1 Dy1 42.36(8) . . ?
C2 O1 C1 117.4(3) . . ?
C2 O1 Dy1 114.6(2) . . ?
C1 O1 Dy1 126.9(2) . . ?
C7 O2 Ni1 126.7(2) . . ?
C7 O2 Dy1 125.3(2) . . ?
Ni1 O2 Dy1 105.96(10) . . ?
C17 O3 Ni1 126.5(2) . . ?
C17 O3 Dy1 126.1(2) . . ?
Ni1 O3 Dy1 106.81(10) . . ?
C16 O4 C18 117.1(3) . . ?
C16 O4 Dy1 114.90(19) . . ?
C18 O4 Dy1 127.9(2) . . ?
C11 N2 C10 119.5(3) . . ?
C11 N2 Ni1 126.7(3) . . ?
C10 N2 Ni1 113.6(2) . . ?
C8 N1 C9 120.9(4) . . ?
C8 N1 Ni1 126.0(3) . . ?
C9 N1 Ni1 113.1(2) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 125.5(4) . . ?
C3 C2 C7 120.4(4) . . ?
O1 C2 C7 114.1(3) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 118.9(4) . . ?
C7 C6 C8 121.9(3) . . ?
C5 C6 C8 119.1(4) . . ?
O2 C7 C2 116.9(3) . . ?
O2 C7 C6 123.2(3) . . ?
C2 C7 C6 119.9(3) . . ?
N1 C8 C6 125.7(4) . . ?
N1 C8 H8 117.1 . . ?
C6 C8 H8 117.1 . . ?
N1 C9 C10 107.7(4) . . ?
N1 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
N1 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N2 C10 C9 107.6(3) . . ?
N2 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
N2 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N2 C11 C12 125.0(3) . . ?
N2 C11 H11 117.5 . . ?
C12 C11 H11 117.5 . . ?
C17 C12 C13 119.4(4) . . ?
C17 C12 C11 121.8(3) . . ?
C13 C12 C11 118.7(4) . . ?
C14 C13 C12 119.6(4) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 121.7(3) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C16 C15 C14 118.6(4) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 O4 125.2(3) . . ?
C15 C16 C17 120.8(4) . . ?
O4 C16 C17 114.0(3) . . ?
O3 C17 C12 123.6(3) . . ?
O3 C17 C16 116.7(3) . . ?
C12 C17 C16 119.7(3) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Dy1 O5 H1W 128(2) . . ?
Dy1 O5 H2W 124(2) . . ?
H1W O5 H2W 105(2) . . ?

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
C1 H1A Cl1 0.96 2.96 3.649(4) 129.9 . yes
C1 H1B Cl1 0.96 2.96 3.855(4) 156.4 3_666 yes
C3 H3 Cl1 0.93 2.90 3.703(4) 145.3 3_666 yes
C10 H10B Cl1 0.97 2.77 3.426(4) 125.8 4_566 yes
C11 H11 Cl2 0.93 2.63 3.562(4) 176.9 2_546 yes
C15 H15 Cl1 0.93 2.99 3.588(4) 123.7 3_656 yes
C18 H18A Cl1 0.96 2.94 3.623(4) 128.8 . yes
C18 H18B Cl3 0.96 2.91 3.559(4) 125.6 1_655 yes
C18 H18C Cl3 0.96 2.89 3.542(4) 126.3 3_656 yes
O5 H1W Cl3 0.836(10) 2.363(18) 3.149(3) 157(3) 1_655 yes
O5 H2W Cl2 0.836(10) 2.39(2) 3.148(3) 151(3) 1_655 yes

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.188


_exptl_crystal_preparation       'Magnetic properties'
