# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_complex1
_audit_block_doi                 10.5517/ccszw6t
_database_code_depnum_ccdc_archive 'CCDC 744657'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.200903430 2010
_audit_update_record             
;
2009-08-18 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C168 H432 Cl18 La12 N24 Ni15 O276'
_chemical_formula_weight         10391.05

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pm-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   21.0408(13)
_cell_length_b                   21.0408(13)
_cell_length_c                   21.0408(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9315.1(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8408
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5226
_exptl_absorpt_coefficient_mu    2.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_T_max  0.5933
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            65636
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1651
_reflns_number_gt                1621
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0966P)²+86.5993P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1651
_refine_ls_number_parameters     169
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1724
_refine_ls_wR_factor_gt          0.1716
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.5000 0.20644(2) -0.20644(2) 0.03567(15) Uani 1 4 d S . .
Ni1 Ni 0.32548(5) 0.32548(5) 0.0000 0.0399(3) Uani 1 4 d S . .
Ni2 Ni 0.5000 0.5000 0.0000 0.0317(5) Uani 1 16 d SD . .
Cl1 Cl 0.21739(8) 0.21739(8) 0.21739(8) 0.0429(6) Uani 1 6 d S . .
Cl2 Cl 0.3885(2) 0.0000 0.0000 0.0628(11) Uani 1 8 d S . .
N1 N 0.3222(3) 0.2296(3) 0.0000 0.078(3) Uani 1 2 d S . .
C1 C 0.3518(6) 0.1981(5) -0.0444(5) 0.053(3) Uani 0.466(4) 1 d P . 1
H1A H 0.3227 0.1665 -0.0637 0.064 Uiso 0.466(4) 1 calc PR . 1
H1B H 0.3884 0.1750 -0.0259 0.064 Uiso 0.466(4) 1 calc PR . 1
C2 C 0.3742(4) 0.2427(6) -0.0933(5) 0.041(3) Uani 0.466(4) 1 d P . 1
O1 O 0.4061(3) 0.2197(4) -0.1354(3) 0.052(2) Uani 0.466(4) 1 d P . 1
O2 O 0.3572(4) 0.3000(4) -0.0877(3) 0.048(2) Uani 0.466(4) 1 d P . 1
C1' C 0.3606(7) 0.2194(6) -0.0724(5) 0.058(4) Uani 0.534(4) 1 d P . 2
H1'A H 0.3756 0.1751 -0.0770 0.070 Uiso 0.534(4) 1 calc PR . 2
H1'B H 0.3315 0.2293 -0.1080 0.070 Uiso 0.534(4) 1 calc PR . 2
C2' C 0.4167(5) 0.2654(5) -0.0718(5) 0.054(3) Uani 0.534(4) 1 d P . 2
O1' O 0.4610(4) 0.2543(5) -0.1097(5) 0.089(3) Uani 0.534(4) 1 d P . 2
O2' O 0.4149(3) 0.3124(4) -0.0367(3) 0.062(2) Uani 0.534(4) 1 d P . 2
C3 C 0.2529(5) 0.2146(5) -0.0245(4) 0.042(2) Uani 0.50 1 d P . .
C4 C 0.2371(7) 0.1431(5) -0.0221(5) 0.067(4) Uani 0.50 1 d P . .
C5 C 0.1660(6) 0.1324(7) -0.0299(6) 0.078(4) Uani 0.50 1 d P . .
O3W O 0.5000 0.1158(3) -0.1158(3) 0.069(2) Uani 1 4 d S . .
O2W O 0.5000 0.2231(5) -0.3292(4) 0.110(3) Uani 1 2 d S . .
O1W O 0.3933(4) 0.2493(3) -0.2493(3) 0.177(4) Uani 1 2 d S . .
O3 O 0.2548(5) 0.1789(4) 0.1789(4) 0.148(4) Uani 1 2 d S . .
O4 O 0.2543(8) 0.2543(8) 0.2543(8) 0.308(14) Uani 1 6 d S . .
O5 O 0.3270(15) 0.0000 0.0000 0.231(18) Uani 1 8 d S . .
O6 O 0.4092(10) 0.0398(5) -0.0398(5) 0.243(8) Uani 0.75 2 d SP . .
O5W O 0.5000 0.6023(9) -0.0635(9) 0.116(6) Uani 0.50 2 d SP . .
O5W' O 0.5000 0.6116(16) 0.0000 0.065(10) Uani 0.25 4 d SP . .
O4W O 0.5000 0.5000 0.1066(4) 0.18(2) Uiso 0.50 8 d SPD . .


_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
La1 O1' 2.414(9) 28_655 ?
La1 O1' 2.414(9) 42 ?
La1 O1' 2.414(9) . ?
La1 O1' 2.414(9) 19_655 ?
La1 O1 2.493(7) 42 ?
La1 O1 2.493(7) 28_655 ?
La1 O1 2.493(7) . ?
La1 O1 2.493(7) 19_655 ?
La1 O1W 2.582(9) . ?
La1 O1W 2.582(9) 28_655 ?
La1 O2W 2.607(9) . ?
La1 O2W 2.607(9) 42 ?
Ni1 N1 2.018(7) 13 ?
Ni1 N1 2.018(7) . ?
Ni1 O2 2.034(7) 13 ?
Ni1 O2 2.034(7) 26 ?
Ni1 O2 2.034(7) . ?
Ni1 O2 2.034(7) 38 ?
Ni1 O2' 2.052(7) 13 ?
Ni1 O2' 2.052(7) 26 ?
Ni1 O2' 2.052(7) . ?
Ni1 O2' 2.052(7) 38 ?
Ni2 O4W 2.244(7) . ?
Ni2 O4W 2.244(7) 25_665 ?
Ni2 O5W' 2.35(3) 37_665 ?
Ni2 O5W' 2.35(3) . ?
Ni2 O5W' 2.35(3) 25_665 ?
Ni2 O5W' 2.35(3) 13 ?
Cl1 O4 1.34(3) . ?
Cl1 O3 1.390(10) 9 ?
Cl1 O3 1.390(10) . ?
Cl1 O3 1.390(10) 5 ?
Cl2 O6 1.262(15) 26 ?
Cl2 O6 1.262(15) 4 ?
Cl2 O6 1.262(15) . ?
Cl2 O6 1.262(15) 27 ?
Cl2 O5 1.29(3) . ?
N1 C1 1.304(11) 26 ?
N1 C1 1.304(11) . ?
N1 C3 1.578(12) 26 ?
N1 C3 1.578(12) . ?
N1 C1' 1.737(11) 26 ?
N1 C1' 1.737(11) . ?
C1 C2 1.471(16) . ?
C1 C1 1.87(2) 26 ?
C2 O1 1.212(12) . ?
C2 O2 1.262(14) . ?
O2 O2 1.703(15) 38 ?
C1' C2' 1.527(17) . ?
C2' O2' 1.235(13) . ?
C2' O1' 1.250(13) . ?
O1' O1' 1.640(16) 28_655 ?
O2' O2' 1.543(14) 26 ?
C3 C3 1.031(18) 26 ?
C3 C3 1.139(19) 38 ?
C3 C3 1.537(18) 13 ?
C3 C4 1.542(15) . ?
C3 C4 1.827(14) 26 ?
C4 C4 0.93(2) 26 ?
C4 C5 1.52(2) . ?
C4 C3 1.827(14) 26 ?
C4 C5 1.866(19) 26 ?
C5 C5 1.00(3) 38 ?
C5 C5 1.26(3) 26 ?
C5 C5 1.61(3) 13 ?
C5 C4 1.866(19) 26 ?
O6 O6 1.68(2) 26 ?
O6 O6 1.68(2) 27 ?
O5W O5W' 1.35(2) . ?
O5W' O5W 1.35(2) 26 ?

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' La1 O1' 144.9(5) 28_655 42 ?
O1' La1 O1' 39.7(4) 28_655 . ?
O1' La1 O1' 126.0(5) 42 . ?
O1' La1 O1' 126.0(5) 28_655 19_655 ?
O1' La1 O1' 39.7(4) 42 19_655 ?
O1' La1 O1' 144.9(5) . 19_655 ?
O1' La1 O1 127.8(3) 28_655 42 ?
O1' La1 O1 34.8(3) 42 42 ?
O1' La1 O1 94.3(3) . 42 ?
O1' La1 O1 73.6(3) 19_655 42 ?
O1' La1 O1 34.8(3) 28_655 28_655 ?
O1' La1 O1 127.8(3) 42 28_655 ?
O1' La1 O1 73.6(3) . 28_655 ?
O1' La1 O1 94.3(3) 19_655 28_655 ?
O1 La1 O1 139.6(4) 42 28_655 ?
O1' La1 O1 73.6(3) 28_655 . ?
O1' La1 O1 94.3(3) 42 . ?
O1' La1 O1 34.8(3) . . ?
O1' La1 O1 127.8(3) 19_655 . ?
O1 La1 O1 60.4(4) 42 . ?
O1 La1 O1 104.8(3) 28_655 . ?
O1' La1 O1 94.3(3) 28_655 19_655 ?
O1' La1 O1 73.6(3) 42 19_655 ?
O1' La1 O1 127.8(3) . 19_655 ?
O1' La1 O1 34.8(3) 19_655 19_655 ?
O1 La1 O1 104.8(3) 42 19_655 ?
O1 La1 O1 60.4(4) 28_655 19_655 ?
O1 La1 O1 139.6(4) . 19_655 ?
O1' La1 O1W 116.4(2) 28_655 . ?
O1' La1 O1W 81.6(2) 42 . ?
O1' La1 O1W 81.6(2) . . ?
O1' La1 O1W 116.4(2) 19_655 . ?
O1 La1 O1W 58.7(2) 42 . ?
O1 La1 O1W 149.25(19) 28_655 . ?
O1 La1 O1W 58.7(2) . . ?
O1 La1 O1W 149.25(19) 19_655 . ?
O1' La1 O1W 81.6(2) 28_655 28_655 ?
O1' La1 O1W 116.4(2) 42 28_655 ?
O1' La1 O1W 116.4(2) . 28_655 ?
O1' La1 O1W 81.6(2) 19_655 28_655 ?
O1 La1 O1W 149.25(19) 42 28_655 ?
O1 La1 O1W 58.7(2) 28_655 28_655 ?
O1 La1 O1W 149.25(19) . 28_655 ?
O1 La1 O1W 58.7(2) 19_655 28_655 ?
O1W La1 O1W 120.9(4) . 28_655 ?
O1' La1 O2W 141.2(3) 28_655 . ?
O1' La1 O2W 72.5(3) 42 . ?
O1' La1 O2W 141.2(3) . . ?
O1' La1 O2W 72.5(3) 19_655 . ?
O1 La1 O2W 88.3(2) 42 . ?
O1 La1 O2W 125.41(18) 28_655 . ?
O1 La1 O2W 125.41(18) . . ?
O1 La1 O2W 88.3(2) 19_655 . ?
O1W La1 O2W 66.89(17) . . ?
O1W La1 O2W 66.89(17) 28_655 . ?
O1' La1 O2W 72.5(3) 28_655 42 ?
O1' La1 O2W 141.2(3) 42 42 ?
O1' La1 O2W 72.5(3) . 42 ?
O1' La1 O2W 141.2(3) 19_655 42 ?
O1 La1 O2W 125.41(18) 42 42 ?
O1 La1 O2W 88.3(2) 28_655 42 ?
O1 La1 O2W 88.3(2) . 42 ?
O1 La1 O2W 125.41(18) 19_655 42 ?
O1W La1 O2W 66.89(17) . 42 ?
O1W La1 O2W 66.89(17) 28_655 42 ?
O2W La1 O2W 74.6(4) . 42 ?
N1 Ni1 N1 86.1(4) 13 . ?
N1 Ni1 O2 75.4(2) 13 13 ?
N1 Ni1 O2 108.6(2) . 13 ?
N1 Ni1 O2 108.6(2) 13 26 ?
N1 Ni1 O2 75.4(2) . 26 ?
O2 Ni1 O2 49.5(4) 13 26 ?
N1 Ni1 O2 108.6(2) 13 . ?
N1 Ni1 O2 75.4(2) . . ?
O2 Ni1 O2 174.8(5) 13 . ?
O2 Ni1 O2 130.2(4) 26 . ?
N1 Ni1 O2 75.4(2) 13 38 ?
N1 Ni1 O2 108.6(2) . 38 ?
O2 Ni1 O2 130.2(4) 13 38 ?
O2 Ni1 O2 174.8(5) 26 38 ?
O2 Ni1 O2 49.5(4) . 38 ?
N1 Ni1 O2' 84.1(3) 13 13 ?
N1 Ni1 O2' 155.8(2) . 13 ?
O2 Ni1 O2' 47.4(3) 13 13 ?
O2 Ni1 O2' 86.9(3) 26 13 ?
O2 Ni1 O2' 128.8(3) . 13 ?
O2 Ni1 O2' 90.3(3) 38 13 ?
N1 Ni1 O2' 155.8(2) 13 26 ?
N1 Ni1 O2' 84.1(3) . 26 ?
O2 Ni1 O2' 86.9(3) 13 26 ?
O2 Ni1 O2' 47.4(3) 26 26 ?
O2 Ni1 O2' 90.3(3) . 26 ?
O2 Ni1 O2' 128.8(3) 38 26 ?
O2' Ni1 O2' 96.0(5) 13 26 ?
N1 Ni1 O2' 155.8(2) 13 . ?
N1 Ni1 O2' 84.1(3) . . ?
O2 Ni1 O2' 128.8(3) 13 . ?
O2 Ni1 O2' 90.3(3) 26 . ?
O2 Ni1 O2' 47.4(3) . . ?
O2 Ni1 O2' 86.9(3) 38 . ?
O2' Ni1 O2' 112.8(5) 13 . ?
O2' Ni1 O2' 44.2(4) 26 . ?
N1 Ni1 O2' 84.1(3) 13 38 ?
N1 Ni1 O2' 155.8(2) . 38 ?
O2 Ni1 O2' 90.3(3) 13 38 ?
O2 Ni1 O2' 128.8(3) 26 38 ?
O2 Ni1 O2' 86.9(3) . 38 ?
O2 Ni1 O2' 47.4(3) 38 38 ?
O2' Ni1 O2' 44.2(4) 13 38 ?
O2' Ni1 O2' 112.8(5) 26 38 ?
O2' Ni1 O2' 96.0(5) . 38 ?
O4W Ni2 O4W 180.0 . 25_665 ?
O4W Ni2 O5W' 90.000(2) . 37_665 ?
O4W Ni2 O5W' 90.000(2) 25_665 37_665 ?
O4W Ni2 O5W' 90.0 . . ?
O4W Ni2 O5W' 90.0 25_665 . ?
O5W' Ni2 O5W' 90.000(2) 37_665 . ?
O4W Ni2 O5W' 90.0 . 25_665 ?
O4W Ni2 O5W' 90.0 25_665 25_665 ?
O5W' Ni2 O5W' 90.000(2) 37_665 25_665 ?
O5W' Ni2 O5W' 180.000(1) . 25_665 ?
O4W Ni2 O5W' 90.000(1) . 13 ?
O4W Ni2 O5W' 90.000(1) 25_665 13 ?
O5W' Ni2 O5W' 180.0 37_665 13 ?
O5W' Ni2 O5W' 90.0 . 13 ?
O5W' Ni2 O5W' 90.0 25_665 13 ?
O4 Cl1 O3 110.2(5) . 9 ?
O4 Cl1 O3 110.2(5) . . ?
O3 Cl1 O3 108.7(5) 9 . ?
O4 Cl1 O3 110.2(5) . 5 ?
O3 Cl1 O3 108.7(5) 9 5 ?
O3 Cl1 O3 108.7(5) . 5 ?
O6 Cl2 O6 83.2(6) 26 4 ?
O6 Cl2 O6 83.2(6) 26 . ?
O6 Cl2 O6 139.8(19) 4 . ?
O6 Cl2 O6 139.8(19) 26 27 ?
O6 Cl2 O6 83.2(6) 4 27 ?
O6 Cl2 O6 83.2(6) . 27 ?
O6 Cl2 O5 110.1(9) 26 . ?
O6 Cl2 O5 110.1(9) 4 . ?
O6 Cl2 O5 110.1(9) . . ?
O6 Cl2 O5 110.1(9) 27 . ?
C1 N1 C1 91.5(11) 26 . ?
C1 N1 C3 96.0(7) 26 26 ?
C1 N1 C3 125.0(8) . 26 ?
C1 N1 C3 125.0(8) 26 . ?
C1 N1 C3 96.0(7) . . ?
C3 N1 C3 38.1(7) 26 . ?
C1 N1 C1' 24.1(6) 26 26 ?
C1 N1 C1' 110.1(8) . 26 ?
C3 N1 C1' 96.8(6) 26 26 ?
C3 N1 C1' 133.7(6) . 26 ?
C1 N1 C1' 110.1(8) 26 . ?
C1 N1 C1' 24.1(6) . . ?
C3 N1 C1' 133.7(6) 26 . ?
C3 N1 C1' 96.8(6) . . ?
C1' N1 C1' 122.5(9) 26 . ?
C1 N1 Ni1 119.5(6) 26 . ?
C1 N1 Ni1 119.5(6) . . ?
C3 N1 Ni1 103.3(5) 26 . ?
C3 N1 Ni1 103.3(5) . . ?
C1' N1 Ni1 96.2(5) 26 . ?
C1' N1 Ni1 96.2(5) . . ?
N1 C1 C2 109.2(9) . . ?
N1 C1 C1 44.2(5) . 26 ?
C2 C1 C1 134.4(6) . 26 ?
O1 C2 O2 127.4(11) . . ?
O1 C2 C1 115.6(11) . . ?
O2 C2 C1 116.9(9) . . ?
C2 O1 La1 157.2(8) . . ?
C2 O2 O2 151.0(6) . 38 ?
C2 O2 Ni1 115.5(6) . . ?
O2 O2 Ni1 65.2(2) 38 . ?
C2' C1' N1 105.9(8) . . ?
O2' C2' O1' 123.7(10) . . ?
O2' C2' C1' 119.3(9) . . ?
O1' C2' C1' 116.9(10) . . ?
C2' O1' O1' 138.3(7) . 28_655 ?
C2' O1' La1 150.4(8) . . ?
O1' O1' La1 70.1(2) 28_655 . ?
C2' O2' O2' 126.8(6) . 26 ?
C2' O2' Ni1 111.1(7) . . ?
O2' O2' Ni1 67.9(2) 26 . ?
C3 C3 C3 90.000(1) 26 38 ?
C3 C3 C3 47.8(7) 26 13 ?
C3 C3 C3 42.2(7) 38 13 ?
C3 C3 C4 88.1(5) 26 . ?
C3 C3 C4 122.5(7) 38 . ?
C3 C3 C4 112.1(7) 13 . ?
C3 C3 N1 70.9(3) 26 . ?
C3 C3 N1 120.8(4) 38 . ?
C3 C3 N1 99.2(6) 13 . ?
C4 C3 N1 112.6(9) . . ?
C3 C3 C4 57.5(4) 26 26 ?
C3 C3 C4 117.0(6) 38 26 ?
C3 C3 C4 88.6(7) 13 26 ?
C4 C3 C4 30.6(7) . 26 ?
N1 C3 C4 99.1(7) . 26 ?
C4 C4 C5 96.2(6) 26 . ?
C4 C4 C3 91.9(5) 26 . ?
C5 C4 C3 110.8(11) . . ?
C4 C4 C3 57.5(4) 26 26 ?
C5 C4 C3 111.1(10) . 26 ?
C3 C4 C3 34.4(6) . 26 ?
C4 C4 C5 54.1(6) 26 26 ?
C5 C4 C5 42.1(10) . 26 ?
C3 C4 C5 108.1(9) . 26 ?
C3 C4 C5 86.1(7) 26 26 ?
C5 C5 C5 90.000(2) 38 26 ?
C5 C5 C4 126.1(7) 38 . ?
C5 C5 C4 83.8(6) 26 . ?
C5 C5 C5 51.5(10) 38 13 ?
C5 C5 C5 38.5(10) 26 13 ?
C4 C5 C5 106.4(9) . 13 ?
C5 C5 C4 118.7(6) 38 26 ?
C5 C5 C4 54.1(6) 26 26 ?
C4 C5 C4 29.7(7) . 26 ?
C5 C5 C4 80.8(9) 13 26 ?
Cl2 O6 O6 48.4(3) . 26 ?
Cl2 O6 O6 48.4(3) . 27 ?
O6 O6 O6 90.000(2) 26 27 ?
O5W O5W' O5W 163(3) 26 . ?
O5W O5W' Ni2 81.7(17) 26 . ?
O5W O5W' Ni2 81.7(17) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         2.245
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.162

# squeeze RESULTS (APPEND TO CIF)
_platon_complex1_details         
;
SQUEEZE removed 4 disordered ClO4- anions and 30 disordered water molecules
per formula unit. This valueis calculated based upon elemental analysis
data.
;
_vrf_CHEMW03_complex1            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 30 water molecules
omitted by SQUEEZE.
;

_vrf_PLAT043_complex1            
;
PROBLEM: Check Reported Molecular Weight ................ 10391.05
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 30 water molecules
omitted by SQUEEZE.
;

_vrf_PLAT601_complex1            
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 1416.00 A**3
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 30 water molecules
omitted by SQUEEZE.
;

# end Validation Reply Form


####################################################################### 
# 
# 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_complex2
_audit_block_doi                 10.5517/cct73vz
_database_code_depnum_ccdc_archive 'CCDC 751621'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.200903430 2010
_audit_update_record             
;
2009-10-16 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C168 H460 Cl18 Gd12 N24 Ni15 O290'
_chemical_formula_weight         10863.35

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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pm-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   20.9271(3)
_cell_length_b                   20.9271(3)
_cell_length_c                   20.9271(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9164.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1485
_cell_measurement_theta_min      2.3785
_cell_measurement_theta_max      28.8091

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5450
_exptl_absorpt_coefficient_mu    3.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6328
_exptl_absorpt_correction_T_max  0.6328
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Gemini S Ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8533
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_sigmaI/netI    0.1285
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1561
_reflns_number_gt                692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1442P)²+17.4310P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1561
_refine_ls_number_parameters     164
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.2181
_refine_ls_R_factor_gt           0.1069
_refine_ls_wR_factor_ref         0.2964
_refine_ls_wR_factor_gt          0.2436
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.005

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.5000 0.19725(5) -0.19725(5) 0.0808(5) Uani 0.80 4 d SP . .
Gd1' Gd 0.4767(3) 0.2491(3) -0.2131(3) 0.0326(19) Uani 0.05 1 d P . .
Ni1 Ni 0.32794(13) 0.32794(13) 0.0000 0.1161(13) Uani 1 4 d S . .
Ni2 Ni 0.5000 0.5000 0.0000 0.0574(16) Uani 1 16 d S . .
Cl1 Cl 0.2190(3) 0.2190(3) -0.2190(3) 0.162(4) Uani 1 6 d S . .
Cl2 Cl 0.3838(4) 0.0000 0.0000 0.076(2) Uani 1 8 d S . .
N1 N 0.3271(12) 0.2285(12) 0.0000 0.2089(8) Uani 1 2 d SU . .
C1 C 0.3596(10) 0.1931(10) -0.0514(10) 0.0950(8) Uani 0.584(6) 1 d PU . 1
C2 C 0.3678(9) 0.2360(9) -0.0901(7) 0.088(6) Uani 0.584(6) 1 d P . 1
O1 O 0.4070(5) 0.2107(9) -0.1366(7) 0.130(6) Uani 0.584(6) 1 d P . 1
O2 O 0.3609(7) 0.2953(8) -0.0935(11) 0.186(9) Uani 0.584(6) 1 d P . 1
C1' C 0.374(4) 0.227(3) -0.037(3) 0.3029(8) Uani 0.416(6) 1 d PU . 2
C2' C 0.4095(18) 0.2717(17) -0.0756(16) 0.1123(8) Uani 0.416(6) 1 d PU . 2
O1' O 0.4553(8) 0.2450(10) -0.1012(13) 0.140(9) Uani 0.416(6) 1 d P . 2
O2' O 0.4188(9) 0.3122(10) -0.0329(10) 0.142(8) Uani 0.416(6) 1 d P . 2
C3 C 0.2521(9) 0.2212(9) -0.0232(7) 0.0886(8) Uani 0.50 1 d PU . .
C4 C 0.247(2) 0.149(2) 0.0000 0.3157(8) Uani 1 2 d SU . .
C5 C 0.1484(10) 0.1484(10) -0.052(4) 0.52(8) Uani 1 2 d S . .
O3W O 0.5000 0.1154(8) -0.1154(8) 0.155(8) Uani 1 4 d S . .
O3 O 0.1777(8) 0.2478(10) -0.1777(8) 0.317(10) Uani 1 2 d S . .
O4 O 0.2407(13) 0.2407(13) -0.2407(13) 0.59(4) Uani 1 6 d S . .
O5 O 0.309(3) 0.0000 0.0000 0.31(3) Uani 1 8 d S . .
O6 O 0.395(2) 0.0443(9) -0.0443(9) 0.34(2) Uani 0.75 2 d SP . .
O1W O 0.5893(13) 0.2566(9) -0.2566(9) 0.1279(8) Uani 0.50 2 d SPU . .
O4W O 0.6067(13) 0.5000 0.0000 0.120(14) Uani 0.50 4 d SP . .
O5W O 0.6078(14) 0.5000 -0.0855(14) 0.141(11) Uani 0.50 2 d SP . .


_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' 1.234(6) 42 ?
Gd1 Gd1' 1.234(6) 28_655 ?
Gd1 Gd1' 1.234(6) . ?
Gd1 Gd1' 1.234(6) 19_655 ?
Gd1 O1 2.341(12) 42 ?
Gd1 O1 2.341(12) 28_655 ?
Gd1 O1 2.341(12) . ?
Gd1 O1 2.341(12) 19_655 ?
Gd1 O3W 2.42(2) . ?
Gd1 O1' 2.43(3) 42 ?
Gd1 O1' 2.43(3) 28_655 ?
Gd1 O1' 2.43(3) . ?
Gd1' Gd1' 0.974(12) 28_655 ?
Gd1' Gd1' 1.064(12) 42 ?
Gd1' Gd1' 1.443(12) 19_655 ?
Gd1' O1W 1.66(3) 28_655 ?
Gd1' O1 2.311(14) . ?
Gd1' O1' 2.39(3) . ?
Gd1' O1W 2.53(3) . ?
Gd1' O1' 2.74(3) 28_655 ?
Gd1' O1 2.770(14) 42 ?
Ni1 O2' 2.050(18) 13 ?
Ni1 O2' 2.050(18) 26 ?
Ni1 O2' 2.050(18) . ?
Ni1 O2' 2.050(18) 38 ?
Ni1 N1 2.08(3) . ?
Ni1 N1 2.08(3) 13 ?
Ni1 O2 2.19(2) 26 ?
Ni1 O2 2.19(2) 13 ?
Ni1 O2 2.19(2) 38 ?
Ni1 O2 2.19(2) . ?
Ni1 C1' 2.44(7) . ?
Ni1 C1' 2.44(7) 38 ?
Ni2 O4W 2.23(3) 25_665 ?
Ni2 O4W 2.23(3) 37_665 ?
Ni2 O4W 2.23(3) . ?
Ni2 O4W 2.23(3) 13 ?
Cl1 O4 0.79(5) . ?
Cl1 O3 1.36(2) 8 ?
Cl1 O3 1.36(2) . ?
Cl1 O3 1.36(2) 11 ?
Cl2 O6 1.33(3) 26 ?
Cl2 O6 1.33(3) 27 ?
Cl2 O6 1.33(3) 4 ?
Cl2 O6 1.33(3) . ?
Cl2 O5 1.57(7) . ?
N1 C1' 1.25(7) . ?
N1 C1' 1.25(7) 26 ?
N1 C1 1.47(3) . ?
N1 C1 1.47(3) 26 ?
N1 C3 1.65(3) . ?
N1 C3 1.65(3) 26 ?
C1 C2 1.22(3) . ?
C2 O2 1.25(2) . ?
C2 O1 1.38(2) . ?
O1 Gd1' 2.770(14) 42 ?
C1' C2' 1.44(8) . ?
C1' C1' 1.53(14) 26 ?
C2' O1' 1.23(4) . ?
C2' O2' 1.25(4) . ?
O1' Gd1' 2.74(3) 28_655 ?
O2' O2' 1.38(4) 26 ?
C3 C3 0.91(3) 38 ?
C3 C3 0.97(3) 26 ?
C3 C3 1.33(3) 13 ?
C3 C4 1.60(5) . ?
C4 C3 1.60(5) 26 ?
O1W Gd1' 1.66(3) 19_655 ?
O1W Gd1' 1.66(3) 28_655 ?
O1W Gd1' 2.53(3) 42 ?
O4W O5W 1.79(3) 26 ?
O4W O5W 1.79(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Gd1' Gd1 Gd1' 71.5(5) 42 28_655 ?
Gd1' Gd1 Gd1' 51.1(5) 42 . ?
Gd1' Gd1 Gd1' 46.5(5) 28_655 . ?
Gd1' Gd1 Gd1' 46.5(5) 42 19_655 ?
Gd1' Gd1 Gd1' 51.1(5) 28_655 19_655 ?
Gd1' Gd1 Gd1' 71.5(5) . 19_655 ?
Gd1' Gd1 O1 73.3(5) 42 42 ?
Gd1' Gd1 O1 140.5(5) 28_655 42 ?
Gd1' Gd1 O1 96.6(4) . 42 ?
Gd1' Gd1 O1 111.6(5) 19_655 42 ?
Gd1' Gd1 O1 140.5(5) 42 28_655 ?
Gd1' Gd1 O1 73.3(5) 28_655 28_655 ?
Gd1' Gd1 O1 111.6(5) . 28_655 ?
Gd1' Gd1 O1 96.6(4) 19_655 28_655 ?
O1 Gd1 O1 145.3(8) 42 28_655 ?
Gd1' Gd1 O1 96.6(4) 42 . ?
Gd1' Gd1 O1 111.6(5) 28_655 . ?
Gd1' Gd1 O1 73.3(5) . . ?
Gd1' Gd1 O1 140.5(5) 19_655 . ?
O1 Gd1 O1 55.9(8) 42 . ?
O1 Gd1 O1 112.5(7) 28_655 . ?
Gd1' Gd1 O1 111.6(5) 42 19_655 ?
Gd1' Gd1 O1 96.6(4) 28_655 19_655 ?
Gd1' Gd1 O1 140.5(5) . 19_655 ?
Gd1' Gd1 O1 73.3(5) 19_655 19_655 ?
O1 Gd1 O1 112.5(7) 42 19_655 ?
O1 Gd1 O1 55.9(8) 28_655 19_655 ?
O1 Gd1 O1 145.3(8) . 19_655 ?
Gd1' Gd1 O3W 144.2(3) 42 . ?
Gd1' Gd1 O3W 144.2(3) 28_655 . ?
Gd1' Gd1 O3W 144.2(3) . . ?
Gd1' Gd1 O3W 144.2(3) 19_655 . ?
O1 Gd1 O3W 72.7(4) 42 . ?
O1 Gd1 O3W 72.7(4) 28_655 . ?
O1 Gd1 O3W 72.7(4) . . ?
O1 Gd1 O3W 72.7(4) 19_655 . ?
Gd1' Gd1 O1' 73.1(6) 42 42 ?
Gd1' Gd1 O1' 140.1(6) 28_655 42 ?
Gd1' Gd1 O1' 117.6(5) . 42 ?
Gd1' Gd1 O1' 90.7(6) 19_655 42 ?
O1 Gd1 O1' 35.2(6) 42 42 ?
O1 Gd1 O1' 130.0(6) 28_655 42 ?
O1 Gd1 O1' 90.1(6) . 42 ?
O1 Gd1 O1' 79.8(6) 19_655 42 ?
O3W Gd1 O1' 72.9(5) . 42 ?
Gd1' Gd1 O1' 140.1(6) 42 28_655 ?
Gd1' Gd1 O1' 73.1(6) 28_655 28_655 ?
Gd1' Gd1 O1' 90.7(6) . 28_655 ?
Gd1' Gd1 O1' 117.6(5) 19_655 28_655 ?
O1 Gd1 O1' 130.0(6) 42 28_655 ?
O1 Gd1 O1' 35.2(6) 28_655 28_655 ?
O1 Gd1 O1' 79.8(6) . 28_655 ?
O1 Gd1 O1' 90.1(6) 19_655 28_655 ?
O3W Gd1 O1' 72.9(5) . 28_655 ?
O1' Gd1 O1' 145.8(10) 42 28_655 ?
Gd1' Gd1 O1' 117.6(5) 42 . ?
Gd1' Gd1 O1' 90.7(6) 28_655 . ?
Gd1' Gd1 O1' 73.1(6) . . ?
Gd1' Gd1 O1' 140.1(6) 19_655 . ?
O1 Gd1 O1' 90.1(6) 42 . ?
O1 Gd1 O1' 79.8(6) 28_655 . ?
O1 Gd1 O1' 35.2(6) . . ?
O1 Gd1 O1' 130.0(6) 19_655 . ?
O3W Gd1 O1' 72.9(5) . . ?
O1' Gd1 O1' 122.1(10) 42 . ?
O1' Gd1 O1' 45.3(9) 28_655 . ?
Gd1' Gd1' Gd1' 90.000(1) 28_655 42 ?
Gd1' Gd1' Gd1 66.8(3) 28_655 . ?
Gd1' Gd1' Gd1 64.5(3) 42 . ?
Gd1' Gd1' Gd1' 47.5(5) 28_655 19_655 ?
Gd1' Gd1' Gd1' 42.5(5) 42 19_655 ?
Gd1 Gd1' Gd1' 54.2(3) . 19_655 ?
Gd1' Gd1' O1W 146.3(8) 28_655 28_655 ?
Gd1' Gd1' O1W 71.3(4) 42 28_655 ?
Gd1 Gd1' O1W 123.9(7) . 28_655 ?
Gd1' Gd1' O1W 109.0(7) 19_655 28_655 ?
Gd1' Gd1' O1 129.2(4) 28_655 . ?
Gd1' Gd1' O1 104.1(5) 42 . ?
Gd1 Gd1' O1 76.0(5) . . ?
Gd1' Gd1' O1 127.4(5) 19_655 . ?
O1W Gd1' O1 83.5(9) 28_655 . ?
Gd1' Gd1' O1' 100.9(4) 28_655 . ?
Gd1' Gd1' O1' 132.0(5) 42 . ?
Gd1 Gd1' O1' 77.2(5) . . ?
Gd1' Gd1' O1' 128.4(5) 19_655 . ?
O1W Gd1' O1' 112.6(9) 28_655 . ?
O1 Gd1' O1' 35.8(6) . . ?
Gd1' Gd1' O1W 21.4(5) 28_655 . ?
Gd1' Gd1' O1W 77.86(19) 42 . ?
Gd1 Gd1' O1W 77.5(6) . . ?
Gd1' Gd1' O1W 38.4(4) 19_655 . ?
O1W Gd1' O1W 124.9(13) 28_655 . ?
O1 Gd1' O1W 149.2(7) . . ?
O1' Gd1' O1W 122.0(7) . . ?
Gd1' Gd1' O1' 58.7(4) 28_655 28_655 ?
Gd1' Gd1' O1' 125.6(5) 42 28_655 ?
Gd1 Gd1' O1' 62.5(5) . 28_655 ?
Gd1' Gd1' O1' 94.5(6) 19_655 28_655 ?
O1W Gd1' O1' 154.4(9) 28_655 28_655 ?
O1 Gd1' O1' 74.1(5) . 28_655 ?
O1' Gd1' O1' 42.1(8) . 28_655 ?
O1W Gd1' O1' 80.0(6) . 28_655 ?
Gd1' Gd1' O1 121.8(3) 28_655 42 ?
Gd1' Gd1' O1 54.0(4) 42 42 ?
Gd1 Gd1' O1 57.1(4) . 42 ?
Gd1' Gd1' O1 85.5(5) 19_655 42 ?
O1W Gd1' O1 69.6(8) 28_655 42 ?
O1 Gd1' O1 50.2(8) . 42 ?
O1' Gd1' O1 81.5(7) . 42 ?
O1W Gd1' O1 123.4(5) . 42 ?
O1' Gd1' O1 103.4(6) 28_655 42 ?
O2' Ni1 O2' 100.7(12) 13 26 ?
O2' Ni1 O2' 114.3(12) 13 . ?
O2' Ni1 O2' 39.3(12) 26 . ?
O2' Ni1 O2' 39.3(12) 13 38 ?
O2' Ni1 O2' 114.3(12) 26 38 ?
O2' Ni1 O2' 100.7(12) . 38 ?
O2' Ni1 N1 157.9(7) 13 . ?
O2' Ni1 N1 81.2(9) 26 . ?
O2' Ni1 N1 81.2(9) . . ?
O2' Ni1 N1 157.9(7) 38 . ?
O2' Ni1 N1 81.2(9) 13 13 ?
O2' Ni1 N1 157.9(7) 26 13 ?
O2' Ni1 N1 157.9(7) . 13 ?
O2' Ni1 N1 81.2(9) 38 13 ?
N1 Ni1 N1 89.0(14) . 13 ?
O2' Ni1 O2 92.3(7) 13 26 ?
O2' Ni1 O2 49.9(7) 26 26 ?
O2' Ni1 O2 87.6(7) . 26 ?
O2' Ni1 O2 129.9(7) 38 26 ?
N1 Ni1 O2 71.9(5) . 26 ?
N1 Ni1 O2 108.2(5) 13 26 ?
O2' Ni1 O2 49.9(7) 13 13 ?
O2' Ni1 O2 92.3(7) 26 13 ?
O2' Ni1 O2 129.9(7) . 13 ?
O2' Ni1 O2 87.6(7) 38 13 ?
N1 Ni1 O2 108.2(5) . 13 ?
N1 Ni1 O2 71.9(5) 13 13 ?
O2 Ni1 O2 52.8(8) 26 13 ?
O2' Ni1 O2 87.6(7) 13 38 ?
O2' Ni1 O2 129.9(7) 26 38 ?
O2' Ni1 O2 92.3(7) . 38 ?
O2' Ni1 O2 49.9(7) 38 38 ?
N1 Ni1 O2 108.2(5) . 38 ?
N1 Ni1 O2 71.9(5) 13 38 ?
O2 Ni1 O2 179.7(10) 26 38 ?
O2 Ni1 O2 127.2(8) 13 38 ?
O2' Ni1 O2 129.9(7) 13 . ?
O2' Ni1 O2 87.6(7) 26 . ?
O2' Ni1 O2 49.9(7) . . ?
O2' Ni1 O2 92.3(7) 38 . ?
N1 Ni1 O2 71.9(5) . . ?
N1 Ni1 O2 108.2(5) 13 . ?
O2 Ni1 O2 127.2(8) 26 . ?
O2 Ni1 O2 179.7(10) 13 . ?
O2 Ni1 O2 52.8(8) 38 . ?
O2' Ni1 C1' 165.8(19) 13 . ?
O2' Ni1 C1' 66.3(18) 26 . ?
O2' Ni1 C1' 52.2(18) . . ?
O2' Ni1 C1' 139.4(18) 38 . ?
N1 Ni1 C1' 30.8(18) . . ?
N1 Ni1 C1' 112.9(19) 13 . ?
O2 Ni1 C1' 83.4(18) 26 . ?
O2 Ni1 C1' 132.6(17) 13 . ?
O2 Ni1 C1' 96.7(18) 38 . ?
O2 Ni1 C1' 47.5(17) . . ?
O2' Ni1 C1' 66.3(18) 13 38 ?
O2' Ni1 C1' 165.8(19) 26 38 ?
O2' Ni1 C1' 139.4(18) . 38 ?
O2' Ni1 C1' 52.2(18) 38 38 ?
N1 Ni1 C1' 112.9(19) . 38 ?
N1 Ni1 C1' 30.8(18) 13 38 ?
O2 Ni1 C1' 132.6(17) 26 38 ?
O2 Ni1 C1' 83.4(18) 13 38 ?
O2 Ni1 C1' 47.5(17) 38 38 ?
O2 Ni1 C1' 96.7(18) . 38 ?
C1' Ni1 C1' 126(3) . 38 ?
O4W Ni2 O4W 90.000(1) 25_665 37_665 ?
O4W Ni2 O4W 180.0 25_665 . ?
O4W Ni2 O4W 90.0 37_665 . ?
O4W Ni2 O4W 90.000(1) 25_665 13 ?
O4W Ni2 O4W 180.000(2) 37_665 13 ?
O4W Ni2 O4W 90.000(1) . 13 ?
O4 Cl1 O3 118.5(11) . 8 ?
O4 Cl1 O3 118.5(11) . . ?
O3 Cl1 O3 99.2(14) 8 . ?
O4 Cl1 O3 118.4(11) . 11 ?
O3 Cl1 O3 99.2(14) 8 11 ?
O3 Cl1 O3 99.2(14) . 11 ?
O6 Cl2 O6 160(4) 26 27 ?
O6 Cl2 O6 88.2(7) 26 4 ?
O6 Cl2 O6 88.2(7) 27 4 ?
O6 Cl2 O6 88.2(7) 26 . ?
O6 Cl2 O6 88.2(7) 27 . ?
O6 Cl2 O6 160(4) 4 . ?
O6 Cl2 O5 100(2) 26 . ?
O6 Cl2 O5 100(2) 27 . ?
O6 Cl2 O5 100(2) 4 . ?
O6 Cl2 O5 100(2) . . ?
C1' N1 C1' 75(7) . 26 ?
C1' N1 C1 35(3) . . ?
C1' N1 C1 94(4) 26 . ?
C1' N1 C1 94(4) . 26 ?
C1' N1 C1 35(3) 26 26 ?
C1 N1 C1 94(2) . 26 ?
C1' N1 C3 125(3) . . ?
C1' N1 C3 158(4) 26 . ?
C1 N1 C3 100.3(13) . . ?
C1 N1 C3 127.4(18) 26 . ?
C1' N1 C3 158(4) . 26 ?
C1' N1 C3 125(3) 26 26 ?
C1 N1 C3 127.4(18) . 26 ?
C1 N1 C3 100.3(13) 26 26 ?
C3 N1 C3 34.2(12) . 26 ?
C1' N1 Ni1 91(4) . . ?
C1' N1 Ni1 91(4) 26 . ?
C1 N1 Ni1 119.9(14) . . ?
C1 N1 Ni1 119.9(14) 26 . ?
C3 N1 Ni1 95.7(14) . . ?
C3 N1 Ni1 95.7(14) 26 . ?
C2 C1 N1 100.3(18) . . ?
C1 C2 O2 139(2) . . ?
C1 C2 O1 105.7(17) . . ?
O2 C2 O1 114.0(19) . . ?
C2 O1 Gd1' 137.1(14) . . ?
C2 O1 Gd1 157.5(12) . . ?
Gd1' O1 Gd1 30.8(2) . . ?
C2 O1 Gd1' 155.1(13) . 42 ?
Gd1' O1 Gd1' 21.9(3) . 42 ?
Gd1 O1 Gd1' 26.27(19) . 42 ?
C2 O2 Ni1 107.1(15) . . ?
N1 C1' C2' 137(6) . . ?
N1 C1' C1' 52(3) . 26 ?
C2' C1' C1' 124(3) . 26 ?
N1 C1' Ni1 58(3) . . ?
C2' C1' Ni1 80(3) . . ?
C1' C1' Ni1 71.7(17) 26 . ?
O1' C2' O2' 120(3) . . ?
O1' C2' C1' 110(4) . . ?
O2' C2' C1' 97(4) . . ?
C2' O1' Gd1' 124(2) . . ?
C2' O1' Gd1 148(2) . . ?
Gd1' O1' Gd1 29.7(4) . . ?
C2' O1' Gd1' 140(2) . 28_655 ?
Gd1' O1' Gd1' 20.4(3) . 28_655 ?
Gd1 O1' Gd1' 26.7(3) . 28_655 ?
C2' O2' O2' 135.8(19) . 26 ?
C2' O2' Ni1 102(2) . . ?
O2' O2' Ni1 70.4(6) 26 . ?
C3 C3 C3 90.000(3) 38 26 ?
C3 C3 C3 46.7(15) 38 13 ?
C3 C3 C3 43.3(15) 26 13 ?
C3 C3 C4 128.4(16) 38 . ?
C3 C3 C4 72.3(7) 26 . ?
C3 C3 C4 101.9(15) 13 . ?
C3 C3 N1 127.4(11) 38 . ?
C3 C3 N1 72.9(6) 26 . ?
C3 C3 N1 101.7(13) 13 . ?
C4 C3 N1 93.8(19) . . ?
C3 C4 C3 35.3(15) 26 . ?
Gd1' O1W Gd1' 37.4(7) 19_655 28_655 ?
Gd1' O1W Gd1' 12.4(4) 19_655 42 ?
Gd1' O1W Gd1' 32.6(6) 28_655 42 ?
Gd1' O1W Gd1' 32.6(6) 19_655 . ?
Gd1' O1W Gd1' 12.4(4) 28_655 . ?
Gd1' O1W Gd1' 24.3(4) 42 . ?
Gd1' O1W Gd1 23.5(4) 19_655 . ?
Gd1' O1W Gd1 23.5(4) 28_655 . ?
Gd1' O1W Gd1 28.0(3) 42 . ?
Gd1' O1W Gd1 28.0(3) . . ?
O5W O4W O5W 179(3) 26 . ?
O5W O4W Ni2 90.7(13) 26 . ?
O5W O4W Ni2 90.7(13) . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         1.253
_refine_diff_density_min         -2.998
_refine_diff_density_rms         0.133

# squeeze RESULTS (APPEND TO CIF)
_platon_complex2_details         
;
SQUEEZE removed 4 disordered ClO4- anions and 80 disordered water molecules
per formula unit. This valueis calculated based upon elemental analysis
data.
;
_vrf_CHEMW03_complex2            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 80 water molecules
omitted by SQUEEZE.
;

_vrf_PLAT043_complex2            
;
PROBLEM: Check Reported Molecular Weight ................ 10863.35
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 80 water molecules
omitted by SQUEEZE.
;

_vrf_PLAT601_complex2            
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 1209.00 A**3
RESPONSE: This is caused by the given molecular weight being increased from
the atom count to account for 4 ClO4- anions and 80 water molecules
omitted by SQUEEZE.
;

# end Validation Reply Form

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1442140'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H28 La N2 Ni O14, Cl O4, 3(O)'
_chemical_formula_sum            'C14 H30 Cl La N2 Ni O21'
_chemical_formula_weight         795.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   18.7646(7)
_cell_length_b                   9.0729(2)
_cell_length_c                   18.6765(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.804(4)
_cell_angle_gamma                90.00
_cell_volume                     2838.02(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.75
_cell_measurement_theta_min      6.56
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.6527
_exptl_absorpt_correction_T_min  0.5223
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17006
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.13
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4706
_reflns_number_total             5525
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.363
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0566P)²+0.4671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0894
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O8-Ni1 = O8-C14
 0.95 with sigma of 0.02
3.a Rotating group:
 O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O9W(H9WA,H9WB)
3.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C11(H11A,H11B), C13(H13A,H13B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.163596(15) 0.82160(3) 0.012565(15) 0.01410(11) Uani 1 1 d . . .
Ni1 Ni 0.18363(3) 1.34074(6) -0.20370(3) 0.01377(14) Uani 1 1 d D . .
Cl1 Cl 0.40588(10) 1.24049(18) 0.14011(9) 0.0476(4) Uani 1 1 d . . .
O1 O 0.1481(2) 1.5420(3) -0.1802(2) 0.0238(7) Uani 1 1 d . . .
O2 O 0.1978(2) 1.7263(4) -0.0934(2) 0.0291(8) Uani 1 1 d . . .
O3 O 0.2397(2) 1.6022(4) -0.3429(2) 0.0360(9) Uani 1 1 d . . .
O4 O 0.1817(2) 1.4267(4) -0.30422(18) 0.0230(7) Uani 1 1 d . . .
O5 O 0.1862(2) 1.0537(4) -0.0405(2) 0.0252(8) Uani 1 1 d . . .
O6 O 0.1782(2) 1.2618(3) -0.10519(19) 0.0218(7) Uani 1 1 d . . .
O7 O 0.0683(2) 1.0438(4) -0.3733(2) 0.0362(9) Uani 1 1 d . . .
O8 O 0.0897(2) 1.2119(4) -0.2785(2) 0.0221(7) Uani 1 1 d D . .
O9 O 0.4816(6) 1.2876(12) 0.1593(5) 0.151(4) Uani 1 1 d . . .
O10 O 0.3493(7) 1.3274(10) 0.1520(6) 0.150(4) Uani 1 1 d . . .
O11 O 0.4171(5) 1.1295(9) 0.2005(4) 0.107(2) Uani 1 1 d . . .
O12 O 0.3726(3) 1.1662(5) 0.0652(3) 0.0486(12) Uani 1 1 d . . .
O1W O 0.4034(3) 0.6546(6) 0.1813(3) 0.0658(16) Uani 1 1 d . . .
O2W O 0.0169(2) 1.6496(4) -0.3116(2) 0.0355(9) Uani 1 1 d . . .
O3W O 0.1547(3) 0.3257(4) 0.0311(3) 0.0403(10) Uani 1 1 d . . .
O4W O 0.0794(3) 0.7342(4) 0.0811(3) 0.0456(11) Uani 1 1 d . . .
H4WA H 0.0793 0.8021 0.1148 0.068 Uiso 1 1 d R . .
H4WB H 0.0996 0.6521 0.1079 0.068 Uiso 1 1 d R . .
O5W O 0.0861(2) 0.5852(4) -0.0492(3) 0.0452(11) Uani 1 1 d . . .
H5WA H 0.0989 0.5505 -0.0866 0.068 Uiso 1 1 d R . .
H5WB H 0.0338 0.6030 -0.0720 0.068 Uiso 1 1 d R . .
O6W O 0.0374(2) 0.8796(4) -0.1141(2) 0.0325(9) Uani 1 1 d . . .
H6WA H 0.0079 0.9441 -0.1037 0.049 Uiso 1 1 d R . .
H6WB H 0.0091 0.7981 -0.1334 0.049 Uiso 1 1 d R . .
O7W O 0.3167(2) 0.8628(4) 0.0573(2) 0.0270(8) Uani 1 1 d . . .
H7WA H 0.3468 0.8036 0.0990 0.040 Uiso 1 1 d R . .
H7WB H 0.3307 0.9571 0.0728 0.040 Uiso 1 1 d R . .
O8W O 0.0844(2) 1.0361(4) 0.03780(19) 0.0240(7) Uani 1 1 d . . .
O9W O 0.2423(2) 0.5936(4) 0.0846(2) 0.0285(8) Uani 1 1 d . . .
H9WA H 0.2109 0.5173 0.0698 0.043 Uiso 1 1 d R . .
H9WB H 0.2614 0.6057 0.1361 0.043 Uiso 1 1 d R . .
N2 N 0.2442(2) 1.1451(4) -0.1966(2) 0.0165(8) Uani 1 1 d . . .
N1 N 0.2948(2) 1.4399(4) -0.1474(2) 0.0179(8) Uani 1 1 d . . .
C1 C 0.3290(3) 1.1895(5) -0.1727(3) 0.0190(10) Uani 1 1 d . . .
H1 H 0.3301 1.2326 -0.2214 0.023 Uiso 1 1 calc R . .
C2 C 0.3517(3) 1.3131(5) -0.1106(3) 0.0197(10) Uani 1 1 d . . .
H2 H 0.3424 1.2748 -0.0653 0.024 Uiso 1 1 calc R . .
C3 C 0.4391(3) 1.3574(6) -0.0753(4) 0.0320(12) Uani 1 1 d . . .
H3A H 0.4485 1.4112 -0.1164 0.038 Uiso 1 1 calc R . .
H3B H 0.4517 1.4250 -0.0296 0.038 Uiso 1 1 calc R . .
C4 C 0.4945(3) 1.2249(7) -0.0469(4) 0.0356(13) Uani 1 1 d . . .
H4A H 0.4893 1.1760 -0.0021 0.043 Uiso 1 1 calc R . .
H4B H 0.5506 1.2577 -0.0270 0.043 Uiso 1 1 calc R . .
C5 C 0.4737(3) 1.1163(7) -0.1156(4) 0.0351(13) Uani 1 1 d . . .
H5A H 0.4794 1.1650 -0.1601 0.042 Uiso 1 1 calc R . .
H5B H 0.5109 1.0316 -0.0971 0.042 Uiso 1 1 calc R . .
C6 C 0.3889(3) 1.0623(6) -0.1448(3) 0.0296(12) Uani 1 1 d . . .
H6A H 0.3844 1.0084 -0.1010 0.035 Uiso 1 1 calc R . .
H6B H 0.3759 0.9928 -0.1899 0.035 Uiso 1 1 calc R . .
C7 C 0.2875(3) 1.5377(5) -0.0882(3) 0.0230(10) Uani 1 1 d . . .
H7A H 0.3289 1.6154 -0.0720 0.028 Uiso 1 1 calc R . .
H7B H 0.2963 1.4803 -0.0399 0.028 Uiso 1 1 calc R . .
C8 C 0.2046(3) 1.6091(5) -0.1236(3) 0.0213(10) Uani 1 1 d . . .
C9 C 0.3072(3) 1.5234(5) -0.2088(3) 0.0238(10) Uani 1 1 d . . .
H9A H 0.3549 1.4836 -0.2119 0.029 Uiso 1 1 calc R . .
H9B H 0.3184 1.6276 -0.1916 0.029 Uiso 1 1 calc R . .
C10 C 0.2368(3) 1.5179(5) -0.2917(3) 0.0226(10) Uani 1 1 d . . .
C11 C 0.2326(3) 1.0501(5) -0.1385(3) 0.0225(10) Uani 1 1 d . . .
H11A H 0.2849 1.0089 -0.1004 0.027 Uiso 1 1 calc R . .
H11B H 0.1976 0.9666 -0.1678 0.027 Uiso 1 1 calc R . .
C12 C 0.1964(3) 1.1275(5) -0.0917(3) 0.0178(9) Uani 1 1 d . . .
C13 C 0.2022(3) 1.0854(5) -0.2778(3) 0.0219(10) Uani 1 1 d . . .
H13A H 0.2122 0.9781 -0.2767 0.026 Uiso 1 1 calc R . .
H13B H 0.2228 1.1324 -0.3126 0.026 Uiso 1 1 calc R . .
C14 C 0.1121(3) 1.1133(5) -0.3125(3) 0.0218(10) Uani 1 1 d 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
La1 O2 2.495(3) 1_545 ?
La1 O3 2.515(3) 4_586 ?
La1 O5 2.444(3) . ?
La1 O4W 2.566(4) . ?
La1 O5W 2.555(4) . ?
La1 O6W 2.536(3) . ?
La1 O7W 2.631(3) . ?
La1 O8W 2.618(3) . ?
La1 O9W 2.545(3) . ?
Ni1 O1 2.058(3) . ?
Ni1 O4 2.018(3) . ?
Ni1 O6 2.019(3) . ?
Ni1 O8 2.050(3) . ?
Ni1 N2 2.079(4) . ?
Ni1 N1 2.071(4) . ?
Cl1 O9 1.367(8) . ?
Cl1 O10 1.418(8) . ?
Cl1 O11 1.454(7) . ?
Cl1 O12 1.419(4) . ?
O1 C8 1.264(6) . ?
O2 La1 2.495(3) 1_565 ?
O2 C8 1.237(6) . ?
O3 La1 2.515(3) 4_585 ?
O3 C10 1.245(6) . ?
O4 C10 1.261(6) . ?
O5 C12 1.251(5) . ?
O6 C12 1.259(6) . ?
O7 C14 1.233(6) . ?
O8 C14 1.272(6) . ?
O4W H4WA 0.8818 . ?
O4W H4WB 0.8820 . ?
O5W H5WA 0.8920 . ?
O5W H5WB 0.8912 . ?
O6W H6WA 0.8862 . ?
O6W H6WB 0.8864 . ?
O7W H7WA 0.9039 . ?
O7W H7WB 0.9035 . ?
O9W H9WA 0.8704 . ?
O9W H9WB 0.8701 . ?
N2 C1 1.501(6) . ?
N2 C11 1.477(6) . ?
N2 C13 1.462(6) . ?
N1 C2 1.508(6) . ?
N1 C7 1.470(6) . ?
N1 C9 1.479(6) . ?
C1 H1 1.0000 . ?
C1 C2 1.528(6) . ?
C1 C6 1.530(7) . ?
C2 H2 1.0000 . ?
C2 C3 1.521(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.520(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.522(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.511(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.533(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.517(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.501(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.534(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 La1 O3 136.22(13) 1_545 4_586 ?
O2 La1 O4W 136.48(14) 1_545 . ?
O2 La1 O5W 69.41(14) 1_545 . ?
O2 La1 O6W 78.30(13) 1_545 . ?
O2 La1 O7W 70.54(12) 1_545 . ?
O2 La1 O8W 140.42(11) 1_545 . ?
O2 La1 O9W 80.90(12) 1_545 . ?
O3 La1 O4W 74.29(15) 4_586 . ?
O3 La1 O5W 130.34(15) 4_586 . ?
O3 La1 O6W 141.62(12) 4_586 . ?
O3 La1 O7W 67.03(12) 4_586 . ?
O3 La1 O8W 72.32(11) 4_586 . ?
O3 La1 O9W 75.11(12) 4_586 . ?
O5 La1 O2 79.82(11) . 1_545 ?
O5 La1 O3 94.57(13) . 4_586 ?
O5 La1 O4W 136.59(12) . . ?
O5 La1 O5W 135.02(13) . . ?
O5 La1 O6W 72.70(12) . . ?
O5 La1 O7W 69.05(11) . . ?
O5 La1 O8W 69.44(11) . . ?
O5 La1 O9W 138.49(12) . . ?
O4W La1 O7W 135.63(13) . . ?
O4W La1 O8W 67.19(12) . . ?
O5W La1 O4W 67.24(15) . . ?
O5W La1 O7W 125.43(12) . . ?
O5W La1 O8W 116.84(12) . . ?
O6W La1 O4W 90.22(14) . . ?
O6W La1 O5W 69.59(13) . . ?
O6W La1 O7W 133.88(12) . . ?
O6W La1 O8W 69.31(11) . . ?
O6W La1 O9W 137.47(12) . . ?
O8W La1 O7W 117.69(11) . . ?
O9W La1 O4W 80.03(12) . . ?
O9W La1 O5W 68.46(13) . . ?
O9W La1 O7W 69.94(11) . . ?
O9W La1 O8W 138.65(11) . . ?
O1 Ni1 N2 164.58(15) . . ?
O1 Ni1 N1 81.64(14) . . ?
O4 Ni1 O1 89.07(14) . . ?
O4 Ni1 O6 176.02(14) . . ?
O4 Ni1 O8 86.37(13) . . ?
O4 Ni1 N2 99.75(14) . . ?
O4 Ni1 N1 84.05(14) . . ?
O6 Ni1 O1 88.08(13) . . ?
O6 Ni1 O8 92.18(14) . . ?
O6 Ni1 N2 83.64(14) . . ?
O6 Ni1 N1 98.28(14) . . ?
O8 Ni1 O1 112.97(13) . . ?
O8 Ni1 N2 80.43(14) . . ?
O8 Ni1 N1 162.40(14) . . ?
N1 Ni1 N2 86.68(15) . . ?
O9 Cl1 O10 123.2(7) . . ?
O9 Cl1 O11 104.0(6) . . ?
O9 Cl1 O12 110.5(4) . . ?
O10 Cl1 O11 97.0(6) . . ?
O10 Cl1 O12 113.0(5) . . ?
O12 Cl1 O11 106.3(4) . . ?
C8 O1 Ni1 112.0(3) . . ?
C8 O2 La1 140.9(3) . 1_565 ?
C10 O3 La1 142.5(3) . 4_585 ?
C10 O4 Ni1 114.3(3) . . ?
C12 O5 La1 152.3(3) . . ?
C12 O6 Ni1 113.9(3) . . ?
C14 O8 Ni1 111.5(3) . . ?
La1 O4W H4WA 110.0 . . ?
La1 O4W H4WB 109.9 . . ?
H4WA O4W H4WB 108.8 . . ?
La1 O5W H5WA 110.6 . . ?
La1 O5W H5WB 110.1 . . ?
H5WA O5W H5WB 108.4 . . ?
La1 O6W H6WA 110.2 . . ?
La1 O6W H6WB 110.1 . . ?
H6WA O6W H6WB 108.7 . . ?
La1 O7W H7WA 111.0 . . ?
La1 O7W H7WB 110.8 . . ?
H7WA O7W H7WB 107.9 . . ?
La1 O9W H9WA 109.3 . . ?
La1 O9W H9WB 109.5 . . ?
H9WA O9W H9WB 109.5 . . ?
C1 N2 Ni1 105.4(3) . . ?
C11 N2 Ni1 106.7(3) . . ?
C11 N2 C1 115.2(4) . . ?
C13 N2 Ni1 103.1(3) . . ?
C13 N2 C1 114.3(3) . . ?
C13 N2 C11 110.9(4) . . ?
C2 N1 Ni1 104.1(3) . . ?
C7 N1 Ni1 103.3(3) . . ?
C7 N1 C2 113.9(4) . . ?
C7 N1 C9 112.0(4) . . ?
C9 N1 Ni1 107.7(3) . . ?
C9 N1 C2 114.6(4) . . ?
N2 C1 H1 106.9 . . ?
N2 C1 C2 108.5(4) . . ?
N2 C1 C6 114.7(4) . . ?
C2 C1 H1 106.9 . . ?
C2 C1 C6 112.6(4) . . ?
C6 C1 H1 106.9 . . ?
N1 C2 C1 108.5(4) . . ?
N1 C2 H2 106.9 . . ?
N1 C2 C3 113.5(4) . . ?
C1 C2 H2 106.9 . . ?
C3 C2 C1 113.6(4) . . ?
C3 C2 H2 106.9 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 112.1(4) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C3 C4 C5 110.0(5) . . ?
H4A C4 H4B 108.2 . . ?
C5 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 C4 110.1(4) . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C1 C6 H6A 109.3 . . ?
C1 C6 H6B 109.3 . . ?
C5 C6 C1 111.8(4) . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 C8 110.6(4) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
O1 C8 C7 117.5(4) . . ?
O2 C8 O1 125.0(5) . . ?
O2 C8 C7 117.4(4) . . ?
N1 C9 H9A 108.8 . . ?
N1 C9 H9B 108.8 . . ?
N1 C9 C10 113.9(4) . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
O3 C10 O4 125.3(5) . . ?
O3 C10 C9 116.4(4) . . ?
O4 C10 C9 118.3(4) . . ?
N2 C11 H11A 108.7 . . ?
N2 C11 H11B 108.7 . . ?
N2 C11 C12 114.2(4) . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
O5 C12 O6 123.4(4) . . ?
O5 C12 C11 117.4(4) . . ?
O6 C12 C11 119.2(4) . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 C14 110.7(4) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
O7 C14 O8 125.9(5) . . ?
O7 C14 C13 117.0(4) . . ?
O8 C14 C13 117.0(4) . . ?

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1442141'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H18 N2 Nd Ni O14, Cl O4, 3(O)'
_chemical_formula_sum            'C14 H36 Cl N2 Nd Ni O21'
_chemical_formula_weight         806.85
_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'
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'
Nd Nd -0.1943 3.0179 '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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   18.6330(9)
_cell_length_b                   8.9756(4)
_cell_length_c                   18.6370(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.699(3)
_cell_angle_gamma                90.00
_cell_volume                     2784.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.01
_cell_measurement_theta_min      6.11
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.6414
_exptl_absorpt_correction_T_min  0.4423
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6969
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4101
_reflns_number_total             4505
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0335P)²+13.8337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0786
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C11(H11A,H11B), C13(H13A,H13B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.18207(3) -0.34224(6) -0.20549(3) 0.00969(13) Uani 1 1 d . . .
Nd1 Nd 0.163252(13) 0.17625(2) 0.010931(13) 0.01045(9) Uani 1 1 d . . .
Cl1 Cl 0.40623(9) -0.24312(17) 0.14013(9) 0.0415(4) Uani 1 1 d . . .
N1 N 0.2933(2) -0.4424(4) -0.1497(2) 0.0123(7) Uani 1 1 d . . .
N2 N 0.2430(2) -0.1441(4) -0.1980(2) 0.0126(7) Uani 1 1 d . . .
C1 C 0.3504(3) -0.3152(5) -0.1127(3) 0.0157(9) Uani 1 1 d . . .
H1 H 0.3414 -0.2777 -0.0668 0.019 Uiso 1 1 calc R . .
C2 C 0.3281(3) -0.1886(5) -0.1738(3) 0.0148(9) Uani 1 1 d . . .
H2 H 0.3299 -0.2305 -0.2227 0.018 Uiso 1 1 calc R . .
C3 C 0.3880(3) -0.0608(6) -0.1447(3) 0.0250(11) Uani 1 1 d . . .
H3A H 0.3833 -0.0084 -0.1002 0.030 Uiso 1 1 calc R . .
H3B H 0.3750 0.0113 -0.1890 0.030 Uiso 1 1 calc R . .
C4 C 0.4739(3) -0.1154(6) -0.1157(3) 0.0286(12) Uani 1 1 d . . .
H4A H 0.4799 -0.1620 -0.1609 0.034 Uiso 1 1 calc R . .
H4B H 0.5114 -0.0300 -0.0960 0.034 Uiso 1 1 calc R . .
C5 C 0.4943(3) -0.2277(6) -0.0489(3) 0.0317(13) Uani 1 1 d . . .
H5A H 0.4894 -0.1804 -0.0033 0.038 Uiso 1 1 calc R . .
H5B H 0.5505 -0.2613 -0.0296 0.038 Uiso 1 1 calc R . .
C6 C 0.4385(3) -0.3606(6) -0.0783(3) 0.0279(12) Uani 1 1 d . . .
H6A H 0.4512 -0.4305 -0.0331 0.033 Uiso 1 1 calc R . .
H6B H 0.4475 -0.4132 -0.1202 0.033 Uiso 1 1 calc R . .
C7 C 0.2865(3) -0.5421(5) -0.0904(3) 0.0195(10) Uani 1 1 d . . .
H7A H 0.2964 -0.4849 -0.0414 0.023 Uiso 1 1 calc R . .
H7B H 0.3277 -0.6214 -0.0752 0.023 Uiso 1 1 calc R . .
C8 C 0.2029(3) -0.6125(5) -0.1249(3) 0.0170(9) Uani 1 1 d . . .
C9 C 0.3054(3) -0.5269(5) -0.2119(3) 0.0186(10) Uani 1 1 d . . .
H9A H 0.3161 -0.6325 -0.1951 0.022 Uiso 1 1 calc R . .
H9B H 0.3536 -0.4874 -0.2149 0.022 Uiso 1 1 calc R . .
C10 C 0.2348(3) -0.5199(5) -0.2949(3) 0.0162(9) Uani 1 1 d . . .
C11 C 0.2302(3) -0.0488(5) -0.1400(3) 0.0180(10) Uani 1 1 d . . .
H11A H 0.1941 0.0342 -0.1697 0.022 Uiso 1 1 calc R . .
H11B H 0.2824 -0.0049 -0.1023 0.022 Uiso 1 1 calc R . .
C12 C 0.1951(3) -0.1274(5) -0.0921(3) 0.0148(9) Uani 1 1 d . . .
C13 C 0.2009(3) -0.0838(5) -0.2797(3) 0.0176(10) Uani 1 1 d . . .
H13A H 0.2224 -0.1307 -0.3141 0.021 Uiso 1 1 calc R . .
H13B H 0.2106 0.0248 -0.2785 0.021 Uiso 1 1 calc R . .
C14 C 0.1112(3) -0.1132(5) -0.3148(3) 0.0188(10) Uani 1 1 d . . .
O1 O 0.1957(2) -0.7299(4) -0.0936(2) 0.0250(8) Uani 1 1 d . . .
O2 O 0.14658(19) -0.5463(3) -0.1823(2) 0.0191(7) Uani 1 1 d . . .
O3 O 0.2377(2) -0.6032(4) -0.3464(2) 0.0292(8) Uani 1 1 d . . .
O4 O 0.17999(18) -0.4282(4) -0.30630(18) 0.0180(7) Uani 1 1 d . . .
O5 O 0.18560(19) -0.0552(4) -0.04049(19) 0.0201(7) Uani 1 1 d . . .
O6 O 0.1763(2) -0.2630(3) -0.10679(19) 0.0193(7) Uani 1 1 d . . .
O7 O 0.0671(2) -0.0448(4) -0.3766(2) 0.0303(9) Uani 1 1 d . . .
O8 O 0.08678(18) -0.2103(3) -0.28096(19) 0.0180(7) Uani 1 1 d . . .
O9 O 0.3717(3) -0.1723(5) 0.0641(2) 0.0436(11) Uani 1 1 d . . .
O10 O 0.4165(4) -0.1294(8) 0.1999(3) 0.0795(18) Uani 1 1 d . . .
O11 O 0.4843(5) -0.2887(11) 0.1591(4) 0.125(4) Uani 1 1 d . . .
O12 O 0.3514(7) -0.3394(10) 0.1514(6) 0.152(4) Uani 1 1 d . . .
O1W O 0.4016(3) 0.3379(5) 0.1828(3) 0.0556(14) Uani 1 1 d . . .
O2W O 0.0155(2) -0.6530(4) -0.3157(2) 0.0318(9) Uani 1 1 d . . .
O3W O 0.1557(3) 0.6724(4) 0.0323(3) 0.0398(10) Uani 1 1 d . . .
O4W O 0.0795(3) 0.2651(4) 0.0774(3) 0.0406(10) Uani 1 1 d . . .
O5W O 0.08465(19) -0.0332(4) 0.03611(19) 0.0206(7) Uani 1 1 d . . .
O6W O 0.0385(2) 0.1198(4) -0.1125(2) 0.0281(8) Uani 1 1 d . . .
O7W O 0.2402(2) 0.3995(4) 0.0827(2) 0.0235(7) Uani 1 1 d . . .
O8W O 0.0877(2) 0.4124(4) -0.0499(3) 0.0389(10) Uani 1 1 d . . .
O9W O 0.31397(19) 0.1342(4) 0.0546(2) 0.0231(7) 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
Ni1 N1 2.062(4) . ?
Ni1 N2 2.080(4) . ?
Ni1 O2 2.058(3) . ?
Ni1 O4 2.015(3) . ?
Ni1 O6 2.020(3) . ?
Ni1 O8 2.071(3) . ?
Nd1 O1 2.435(3) 1_565 ?
Nd1 O3 2.472(3) 4_556 ?
Nd1 O5 2.401(3) . ?
Nd1 O4W 2.518(4) . ?
Nd1 O5W 2.553(3) . ?
Nd1 O6W 2.479(3) . ?
Nd1 O7W 2.477(3) . ?
Nd1 O8W 2.515(4) . ?
Nd1 O9W 2.576(3) . ?
Cl1 O9 1.416(4) . ?
Cl1 O10 1.458(6) . ?
Cl1 O11 1.396(7) . ?
Cl1 O12 1.424(8) . ?
N1 C1 1.500(6) . ?
N1 C7 1.472(6) . ?
N1 C9 1.485(6) . ?
N2 C2 1.495(6) . ?
N2 C11 1.479(6) . ?
N2 C13 1.467(6) . ?
C1 H1 1.0000 . ?
C1 C2 1.528(6) . ?
C1 C6 1.525(6) . ?
C2 H2 1.0000 . ?
C2 C3 1.520(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.522(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.512(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.514(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.529(7) . ?
C8 O1 1.240(6) . ?
C8 O2 1.262(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.517(6) . ?
C10 O3 1.236(6) . ?
C10 O4 1.254(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.498(6) . ?
C12 O5 1.238(5) . ?
C12 O6 1.262(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.520(6) . ?
C14 O7 1.236(6) . ?
C14 O8 1.274(6) . ?
O1 Nd1 2.435(3) 1_545 ?
O3 Nd1 2.472(3) 4 ?

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
N1 Ni1 N2 86.79(14) . . ?
N1 Ni1 O8 162.33(14) . . ?
O2 Ni1 N1 81.45(13) . . ?
O2 Ni1 N2 164.53(14) . . ?
O2 Ni1 O8 113.16(12) . . ?
O4 Ni1 N1 84.10(13) . . ?
O4 Ni1 N2 99.85(14) . . ?
O4 Ni1 O2 88.95(13) . . ?
O4 Ni1 O6 175.84(13) . . ?
O4 Ni1 O8 86.22(13) . . ?
O6 Ni1 N1 98.46(14) . . ?
O6 Ni1 N2 83.61(14) . . ?
O6 Ni1 O2 88.19(13) . . ?
O6 Ni1 O8 92.12(13) . . ?
O8 Ni1 N2 80.33(13) . . ?
O1 Nd1 O3 137.02(12) 1_565 4_556 ?
O1 Nd1 O4W 135.68(13) 1_565 . ?
O1 Nd1 O5W 140.44(11) 1_565 . ?
O1 Nd1 O6W 78.13(12) 1_565 . ?
O1 Nd1 O7W 82.02(12) 1_565 . ?
O1 Nd1 O8W 68.76(13) 1_565 . ?
O1 Nd1 O9W 71.12(12) 1_565 . ?
O3 Nd1 O4W 74.14(14) 4_556 . ?
O3 Nd1 O5W 72.42(11) 4_556 . ?
O3 Nd1 O6W 141.54(12) 4_556 . ?
O3 Nd1 O7W 74.01(12) 4_556 . ?
O3 Nd1 O8W 129.65(14) 4_556 . ?
O3 Nd1 O9W 67.43(12) 4_556 . ?
O5 Nd1 O1 80.21(11) . 1_565 ?
O5 Nd1 O3 94.93(12) . 4_556 ?
O5 Nd1 O4W 136.65(12) . . ?
O5 Nd1 O5W 69.70(11) . . ?
O5 Nd1 O6W 73.23(12) . . ?
O5 Nd1 O7W 138.88(11) . . ?
O5 Nd1 O8W 135.37(13) . . ?
O5 Nd1 O9W 68.87(11) . . ?
O4W Nd1 O5W 67.00(12) . . ?
O4W Nd1 O9W 135.99(13) . . ?
O5W Nd1 O9W 117.91(11) . . ?
O6W Nd1 O4W 89.51(14) . . ?
O6W Nd1 O5W 69.15(11) . . ?
O6W Nd1 O8W 69.66(12) . . ?
O6W Nd1 O9W 134.24(12) . . ?
O7W Nd1 O4W 79.28(12) . . ?
O7W Nd1 O5W 137.46(11) . . ?
O7W Nd1 O6W 137.74(11) . . ?
O7W Nd1 O8W 68.44(12) . . ?
O7W Nd1 O9W 70.36(11) . . ?
O8W Nd1 O4W 67.04(15) . . ?
O8W Nd1 O5W 116.90(12) . . ?
O8W Nd1 O9W 125.15(12) . . ?
O9 Cl1 O10 107.1(3) . . ?
O9 Cl1 O12 112.7(5) . . ?
O11 Cl1 O9 109.8(4) . . ?
O11 Cl1 O10 104.3(5) . . ?
O11 Cl1 O12 121.4(7) . . ?
O12 Cl1 O10 99.7(5) . . ?
C1 N1 Ni1 104.1(3) . . ?
C7 N1 Ni1 103.7(3) . . ?
C7 N1 C1 113.6(3) . . ?
C7 N1 C9 111.7(3) . . ?
C9 N1 Ni1 107.4(3) . . ?
C9 N1 C1 115.0(4) . . ?
C2 N2 Ni1 105.4(3) . . ?
C11 N2 Ni1 106.4(3) . . ?
C11 N2 C2 115.5(3) . . ?
C13 N2 Ni1 103.0(3) . . ?
C13 N2 C2 114.3(3) . . ?
C13 N2 C11 111.0(4) . . ?
N1 C1 H1 107.0 . . ?
N1 C1 C2 108.9(3) . . ?
N1 C1 C6 113.4(4) . . ?
C2 C1 H1 107.0 . . ?
C6 C1 H1 107.0 . . ?
C6 C1 C2 113.1(4) . . ?
N2 C2 C1 108.6(4) . . ?
N2 C2 H2 106.9 . . ?
N2 C2 C3 114.5(4) . . ?
C1 C2 H2 106.9 . . ?
C3 C2 C1 112.6(4) . . ?
C3 C2 H2 106.9 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C2 C3 C4 111.7(4) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 C4 C3 110.0(4) . . ?
C5 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C4 C5 C6 110.4(4) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C1 C6 H6A 109.2 . . ?
C1 C6 H6B 109.2 . . ?
C5 C6 C1 112.1(4) . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 C8 110.6(4) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
O1 C8 C7 117.3(4) . . ?
O1 C8 O2 125.0(4) . . ?
O2 C8 C7 117.6(4) . . ?
N1 C9 H9A 108.7 . . ?
N1 C9 H9B 108.7 . . ?
N1 C9 C10 114.1(4) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
O3 C10 C9 116.5(4) . . ?
O3 C10 O4 125.6(4) . . ?
O4 C10 C9 117.8(4) . . ?
N2 C11 H11A 108.6 . . ?
N2 C11 H11B 108.6 . . ?
N2 C11 C12 114.8(4) . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
O5 C12 C11 118.0(4) . . ?
O5 C12 O6 123.4(4) . . ?
O6 C12 C11 118.6(4) . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 C14 110.8(4) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
O7 C14 C13 117.2(4) . . ?
O7 C14 O8 124.5(4) . . ?
O8 C14 C13 118.3(4) . . ?
C8 O1 Nd1 142.0(3) . 1_545 ?
C8 O2 Ni1 112.0(3) . . ?
C10 O3 Nd1 142.8(3) . 4 ?
C10 O4 Ni1 114.9(3) . . ?
C12 O5 Nd1 151.0(3) . . ?
C12 O6 Ni1 114.4(3) . . ?
C14 O8 Ni1 109.9(3) . . ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1442142'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C28 H52 N6 Nd2 Ni2 O30, 8(H2 O)'
_chemical_formula_sum            'C28 H68 N6 Nd2 Ni2 O38'
_chemical_formula_weight         1502.78
_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'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.2011(18)
_cell_length_b                   12.234(2)
_cell_length_c                   12.510(3)
_cell_angle_alpha                85.62(3)
_cell_angle_beta                 80.05(3)
_cell_angle_gamma                68.91(3)
_cell_volume                     1294.0(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.75
_cell_measurement_theta_min      6.56
_exptl_absorpt_coefficient_mu    2.802
_exptl_absorpt_correction_T_max  0.7480
_exptl_absorpt_correction_T_min  0.4869
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11125
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.12
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4785
_reflns_number_total             5071
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0209P)²+1.4636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0572
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1W(H,HA), O3W(HB,HC), O4W(HD,HE), O2W(HF,HG)
2.b Rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O10(H10A,H10B), O13(H13A,H13B)
2.c Ternary CH refined with riding coordinates:
 C2(H2), C1(H1)
2.d Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13C,H13D), C7(H7A,H7B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,
 H11B), C6(H6C,H6D), C5(H5C,H5D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.992078(15) 0.717313(11) 0.636553(10) 0.01401(6) Uani 1 1 d . . .
Ni1 Ni 1.31487(4) 0.77479(3) 0.33932(2) 0.01273(8) Uani 1 1 d . . .
O1 O 0.9739(2) 0.64028(16) 0.45149(14) 0.0189(4) Uani 1 1 d . . .
O2 O 1.4295(2) 0.60114(16) 0.30806(15) 0.0187(4) Uani 1 1 d . . .
O3 O 1.1494(2) 0.72464(16) 0.44954(14) 0.0164(4) Uani 1 1 d . . .
O4 O 1.6041(2) 0.48167(16) 0.18270(16) 0.0226(4) Uani 1 1 d . . .
O5 O 1.2611(2) 0.68880(17) 0.66922(16) 0.0214(4) Uani 1 1 d . . .
H5A H 1.2830 0.6438 0.7277 0.032 Uiso 1 1 d R . .
H5B H 1.2689 0.7574 0.6796 0.032 Uiso 1 1 d R . .
O6 O 1.1523(2) 0.50433(16) 0.63283(16) 0.0213(4) Uani 1 1 d . . .
H6A H 1.1810 0.4806 0.6970 0.032 Uiso 1 1 d R . .
H6B H 1.2379 0.4906 0.5836 0.032 Uiso 1 1 d R . .
O7 O 1.1977(2) 0.94696(16) 0.36834(15) 0.0186(4) Uani 1 1 d . . .
O8 O 1.6582(2) 0.89382(19) 0.37209(17) 0.0277(5) Uani 1 1 d . . .
O9 O 1.4958(2) 0.79186(16) 0.40615(14) 0.0180(4) Uani 1 1 d . . .
O10 O 0.7867(2) 0.86280(18) 0.55143(17) 0.0285(5) Uani 1 1 d . . .
H10A H 0.7734 0.9324 0.5731 0.043 Uiso 1 1 d R . .
H10B H 0.6987 0.8493 0.5696 0.043 Uiso 1 1 d R . .
N2 N 1.4538(2) 0.80004(18) 0.19802(17) 0.0139(4) Uani 1 1 d . . .
O12 O 0.9796(2) 1.09530(17) 0.34157(17) 0.0254(4) Uani 1 1 d . . .
O13 O 0.8022(2) 0.61834(19) 0.66893(16) 0.0265(5) Uani 1 1 d . . .
H13A H 0.7347 0.6434 0.6218 0.040 Uiso 1 1 d R . .
H13B H 0.7483 0.6326 0.7355 0.040 Uiso 1 1 d R . .
N3 N 1.1408(2) 0.79625(18) 0.24300(16) 0.0133(4) Uani 1 1 d . . .
O15 O 0.9731(3) 0.6656(2) 0.83670(17) 0.0344(5) Uani 1 1 d . . .
O1W O 0.6420(3) 0.5988(2) 0.86243(18) 0.0331(5) Uani 1 1 d G . .
H H 0.5582 0.5821 0.8603 0.050 Uiso 1 1 d G . .
HA H 0.7017 0.5474 0.9032 0.050 Uiso 1 1 d G . .
O17 O 0.7929(3) 0.8280(2) 0.80275(18) 0.0383(6) Uani 1 1 d . . .
O3W O 1.6136(2) 0.56914(19) 0.53889(17) 0.0280(5) Uani 1 1 d G . .
HB H 1.5761 0.5232 0.5821 0.042 Uiso 1 1 d G . .
HC H 1.5401 0.6375 0.5351 0.042 Uiso 1 1 d G . .
C9 C 1.0152(3) 0.9109(2) 0.2736(2) 0.0168(5) Uani 1 1 d . . .
H9A H 0.9258 0.8965 0.3211 0.020 Uiso 1 1 calc R . .
H9B H 0.9764 0.9516 0.2071 0.020 Uiso 1 1 calc R . .
C14 C 1.5321(3) 0.5815(2) 0.2231(2) 0.0167(5) Uani 1 1 d . . .
O4W O 1.4033(3) 0.8513(2) 0.63228(19) 0.0375(5) Uani 1 1 d G . .
HD H 1.3797 0.9234 0.6510 0.056 Uiso 1 1 d G . .
HE H 1.4488 0.8425 0.5649 0.056 Uiso 1 1 d G . .
C13 C 1.5747(3) 0.6831(2) 0.1683(2) 0.0182(5) Uani 1 1 d . . .
H13C H 1.6761 0.6794 0.1880 0.022 Uiso 1 1 calc R . .
H13D H 1.5902 0.6745 0.0887 0.022 Uiso 1 1 calc R . .
C2 C 1.3428(3) 0.8530(2) 0.1172(2) 0.0141(5) Uani 1 1 d . . .
H2 H 1.2814 0.9359 0.1392 0.017 Uiso 1 1 calc R . .
C10 C 1.0688(3) 0.9907(2) 0.3318(2) 0.0162(5) Uani 1 1 d . . .
C7 C 1.0809(3) 0.7000(2) 0.2774(2) 0.0157(5) Uani 1 1 d . . .
H7A H 1.1541 0.6262 0.2425 0.019 Uiso 1 1 calc R . .
H7B H 0.9765 0.7182 0.2551 0.019 Uiso 1 1 calc R . .
N1 N 0.8584(3) 0.7564(3) 0.8726(2) 0.0302(6) Uani 1 1 d . . .
C8 C 1.0669(3) 0.6859(2) 0.4004(2) 0.0156(5) Uani 1 1 d . . .
O21 O 0.8159(3) 0.7715(3) 0.97022(18) 0.0507(8) Uani 1 1 d . . .
C1 C 1.2238(3) 0.7892(2) 0.12798(19) 0.0139(5) Uani 1 1 d . . .
H1 H 1.2861 0.7046 0.1132 0.017 Uiso 1 1 calc R . .
C12 C 1.5649(3) 0.8524(2) 0.3447(2) 0.0179(5) Uani 1 1 d . . .
C3 C 1.4245(3) 0.8570(2) 0.0003(2) 0.0194(5) Uani 1 1 d . . .
H3A H 1.4878 0.9081 -0.0036 0.023 Uiso 1 1 calc R . .
H3B H 1.4976 0.7772 -0.0207 0.023 Uiso 1 1 calc R . .
O2W O 0.8286(3) 0.4508(3) 0.9955(2) 0.0498(7) Uani 1 1 d G . .
HF H 0.7691 0.4541 1.0582 0.075 Uiso 1 1 d G . .
HG H 0.9266 0.4291 1.0048 0.075 Uiso 1 1 d G . .
C4 C 1.3075(4) 0.9026(3) -0.0801(2) 0.0244(6) Uani 1 1 d . . .
H4A H 1.2406 0.9852 -0.0641 0.029 Uiso 1 1 calc R . .
H4B H 1.3656 0.8996 -0.1549 0.029 Uiso 1 1 calc R . .
C11 C 1.5277(3) 0.8801(2) 0.2286(2) 0.0174(5) Uani 1 1 d . . .
H11A H 1.4553 0.9622 0.2237 0.021 Uiso 1 1 calc R . .
H11B H 1.6262 0.8712 0.1775 0.021 Uiso 1 1 calc R . .
C6 C 1.1129(3) 0.8331(3) 0.0430(2) 0.0201(6) Uani 1 1 d . . .
H6C H 1.0461 0.7845 0.0475 0.024 Uiso 1 1 calc R . .
H6D H 1.0426 0.9149 0.0590 0.024 Uiso 1 1 calc R . .
C5 C 1.2042(3) 0.8278(3) -0.0715(2) 0.0230(6) Uani 1 1 d . . .
H5C H 1.1295 0.8568 -0.1243 0.028 Uiso 1 1 calc R . .
H5D H 1.2711 0.7456 -0.0892 0.028 Uiso 1 1 calc 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
Nd1 O1 2.6184(18) . ?
Nd1 O3 2.5432(19) . ?
Nd1 O5 2.4746(19) . ?
Nd1 O6 2.489(2) . ?
Nd1 O10 2.420(2) . ?
Nd1 O12 2.4391(19) 2_776 ?
Nd1 O13 2.426(2) . ?
Nd1 O15 2.527(2) . ?
Nd1 O17 2.616(2) . ?
Nd1 N1 3.000(3) . ?
Nd1 C8 2.938(3) . ?
Ni1 O2 2.0374(19) . ?
Ni1 O3 2.1007(19) . ?
Ni1 O7 2.0194(19) . ?
Ni1 O9 2.0672(18) . ?
Ni1 N2 2.067(2) . ?
Ni1 N3 2.098(2) . ?
O1 C8 1.246(3) . ?
O2 C14 1.268(3) . ?
O3 C8 1.283(3) . ?
O4 C14 1.258(3) . ?
O7 C10 1.263(3) . ?
O8 C12 1.245(3) . ?
O9 C12 1.276(3) . ?
N2 C13 1.488(3) . ?
N2 C2 1.505(3) . ?
N2 C11 1.481(3) . ?
O12 Nd1 2.4391(19) 2_776 ?
O12 C10 1.249(3) . ?
N3 C9 1.487(3) . ?
N3 C7 1.477(3) . ?
N3 C1 1.501(3) . ?
O15 N1 1.273(4) . ?
O17 N1 1.256(4) . ?
C9 C10 1.519(3) . ?
C14 C13 1.515(4) . ?
C2 C1 1.541(3) . ?
C2 C3 1.530(3) . ?
C7 C8 1.523(3) . ?
N1 O21 1.223(3) . ?
C1 C6 1.534(3) . ?
C12 C11 1.535(4) . ?
C3 C4 1.529(4) . ?
C4 C5 1.526(4) . ?
C6 C5 1.523(4) . ?

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 Nd1 N1 146.95(6) . . ?
O1 Nd1 C8 25.07(6) . . ?
O3 Nd1 O1 50.51(6) . . ?
O3 Nd1 O17 149.24(7) . . ?
O3 Nd1 N1 162.25(6) . . ?
O3 Nd1 C8 25.80(6) . . ?
O5 Nd1 O1 115.79(7) . . ?
O5 Nd1 O3 74.69(6) . . ?
O5 Nd1 O6 70.69(7) . . ?
O5 Nd1 O15 78.54(7) . . ?
O5 Nd1 O17 107.78(8) . . ?
O5 Nd1 N1 92.41(7) . . ?
O5 Nd1 C8 97.48(7) . . ?
O6 Nd1 O1 73.50(7) . . ?
O6 Nd1 O3 84.94(7) . . ?
O6 Nd1 O15 78.58(8) . . ?
O6 Nd1 O17 125.32(8) . . ?
O6 Nd1 N1 102.52(8) . . ?
O6 Nd1 C8 81.05(8) . . ?
O10 Nd1 O1 69.83(7) . . ?
O10 Nd1 O3 81.09(7) . . ?
O10 Nd1 O5 137.51(7) . . ?
O10 Nd1 O6 141.40(6) . . ?
O10 Nd1 O12 74.10(7) . 2_776 ?
O10 Nd1 O13 82.54(8) . . ?
O10 Nd1 O15 125.34(8) . . ?
O10 Nd1 O17 77.26(8) . . ?
O10 Nd1 N1 101.57(8) . . ?
O10 Nd1 C8 70.87(8) . . ?
O12 Nd1 O1 124.33(7) 2_776 . ?
O12 Nd1 O3 83.52(7) 2_776 . ?
O12 Nd1 O5 68.96(7) 2_776 . ?
O12 Nd1 O6 139.64(6) 2_776 . ?
O12 Nd1 O15 94.51(8) 2_776 . ?
O12 Nd1 O17 69.74(8) 2_776 . ?
O12 Nd1 N1 80.43(8) 2_776 . ?
O12 Nd1 C8 102.95(8) 2_776 . ?
O13 Nd1 O1 71.33(6) . . ?
O13 Nd1 O3 121.74(6) . . ?
O13 Nd1 O5 139.95(7) . . ?
O13 Nd1 O6 74.65(7) . . ?
O13 Nd1 O12 142.49(7) . 2_776 ?
O13 Nd1 O15 75.45(7) . . ?
O13 Nd1 O17 76.83(8) . . ?
O13 Nd1 N1 75.96(7) . . ?
O13 Nd1 C8 96.36(7) . . ?
O15 Nd1 O1 141.03(7) . . ?
O15 Nd1 O3 152.01(7) . . ?
O15 Nd1 O17 49.38(8) . . ?
O15 Nd1 N1 24.78(8) . . ?
O15 Nd1 C8 159.42(8) . . ?
O17 Nd1 O1 136.39(7) . . ?
O17 Nd1 N1 24.66(8) . . ?
O17 Nd1 C8 148.04(8) . . ?
C8 Nd1 N1 170.11(7) . . ?
O2 Ni1 O3 86.81(8) . . ?
O2 Ni1 O9 94.22(8) . . ?
O2 Ni1 N2 84.65(8) . . ?
O2 Ni1 N3 95.04(8) . . ?
O7 Ni1 O2 178.76(7) . . ?
O7 Ni1 O3 92.90(8) . . ?
O7 Ni1 O9 86.99(8) . . ?
O7 Ni1 N2 95.31(9) . . ?
O7 Ni1 N3 83.73(8) . . ?
O9 Ni1 O3 114.97(7) . . ?
O9 Ni1 N2 81.06(8) . . ?
O9 Ni1 N3 163.71(8) . . ?
N2 Ni1 O3 162.39(7) . . ?
N2 Ni1 N3 86.50(8) . . ?
N3 Ni1 O3 78.94(8) . . ?
C8 O1 Nd1 91.96(14) . . ?
C14 O2 Ni1 113.53(17) . . ?
Ni1 O3 Nd1 153.33(8) . . ?
C8 O3 Nd1 94.56(15) . . ?
C8 O3 Ni1 111.47(16) . . ?
C10 O7 Ni1 115.20(15) . . ?
C12 O9 Ni1 111.52(16) . . ?
C13 N2 Ni1 106.33(16) . . ?
C13 N2 C2 114.80(19) . . ?
C2 N2 Ni1 105.71(15) . . ?
C11 N2 Ni1 104.68(15) . . ?
C11 N2 C13 110.85(19) . . ?
C11 N2 C2 113.5(2) . . ?
C10 O12 Nd1 136.51(17) . 2_776 ?
C9 N3 Ni1 105.86(14) . . ?
C9 N3 C1 115.2(2) . . ?
C7 N3 Ni1 104.84(16) . . ?
C7 N3 C9 109.96(19) . . ?
C7 N3 C1 114.65(18) . . ?
C1 N3 Ni1 105.23(14) . . ?
N1 O15 Nd1 98.89(18) . . ?
N1 O17 Nd1 95.06(17) . . ?
N3 C9 C10 113.9(2) . . ?
O2 C14 C13 118.5(2) . . ?
O4 C14 O2 123.8(3) . . ?
O4 C14 C13 117.7(2) . . ?
N2 C13 C14 113.8(2) . . ?
N2 C2 C1 108.7(2) . . ?
N2 C2 C3 114.3(2) . . ?
C3 C2 C1 112.58(19) . . ?
O7 C10 C9 118.3(2) . . ?
O12 C10 O7 124.8(2) . . ?
O12 C10 C9 116.9(2) . . ?
N3 C7 C8 108.83(19) . . ?
O15 N1 Nd1 56.33(14) . . ?
O17 N1 Nd1 60.29(14) . . ?
O17 N1 O15 116.4(2) . . ?
O21 N1 Nd1 174.77(19) . . ?
O21 N1 O15 120.8(3) . . ?
O21 N1 O17 122.8(3) . . ?
O1 C8 Nd1 62.97(13) . . ?
O1 C8 O3 121.3(2) . . ?
O1 C8 C7 120.2(2) . . ?
O3 C8 Nd1 59.64(13) . . ?
O3 C8 C7 118.5(2) . . ?
C7 C8 Nd1 166.41(17) . . ?
N3 C1 C2 109.39(18) . . ?
N3 C1 C6 114.2(2) . . ?
C6 C1 C2 111.8(2) . . ?
O8 C12 O9 125.1(3) . . ?
O8 C12 C11 116.8(2) . . ?
O9 C12 C11 118.0(2) . . ?
C4 C3 C2 112.5(2) . . ?
C5 C4 C3 109.7(2) . . ?
N2 C11 C12 110.2(2) . . ?
C5 C6 C1 111.6(2) . . ?
C6 C5 C4 110.1(2) . . ?

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1442143'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C28 H36 Dy2 N6 Ni2 O30, 8(O)'
_chemical_formula_sum            'C28 H36 Dy2 N6 Ni2 O38'
_chemical_formula_weight         1507.05
_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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.1672(18)
_cell_length_b                   12.170(2)
_cell_length_c                   12.442(3)
_cell_angle_alpha                85.92(3)
_cell_angle_beta                 79.65(3)
_cell_angle_gamma                68.68(3)
_cell_volume                     1272.1(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.75
_cell_measurement_theta_min      6.22
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.7058
_exptl_absorpt_correction_T_min  0.4545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8897
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.15
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4057
_reflns_number_total             4400
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.438
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0477P)²+4.6426P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0985
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2A,H2B), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B), C5(H5A,
 H5B), C4(H4A,H4B), C11(H11A,H11B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.50847(3) -0.21642(2) -0.136052(19) 0.01281(11) Uani 1 1 d . . .
Ni1 Ni 0.18704(8) -0.27551(6) 0.15682(5) 0.01172(17) Uani 1 1 d . . .
O1 O 0.2463(5) -0.1892(4) -0.1667(3) 0.0232(9) Uani 1 1 d . . .
O4 O 0.3568(4) -0.2273(3) 0.0461(3) 0.0153(8) Uani 1 1 d . . .
N2 N 0.3608(5) -0.2985(4) 0.2535(4) 0.0132(9) Uani 1 1 d . . .
O7 O 0.7051(6) -0.3249(4) -0.3020(4) 0.0350(11) Uani 1 1 d . . .
O8 O 0.7159(5) -0.3566(4) -0.0585(3) 0.0238(9) Uani 1 1 d . . .
O9 O 0.5170(5) -0.1635(4) -0.3285(3) 0.0282(10) Uani 1 1 d . . .
O10 O 0.6930(5) -0.1207(4) -0.1695(3) 0.0232(9) Uani 1 1 d . . .
C9 C -0.0748(7) -0.1822(5) 0.3297(5) 0.0164(12) Uani 1 1 d . . .
H9A H -0.0896 -0.1736 0.4099 0.020 Uiso 1 1 calc R . .
H9B H -0.1773 -0.1780 0.3111 0.020 Uiso 1 1 calc R . .
C1 C 0.1556(6) -0.3528(5) 0.3795(4) 0.0129(11) Uani 1 1 d . . .
H1 H 0.2165 -0.4365 0.3565 0.016 Uiso 1 1 calc R . .
C2 C 0.0724(7) -0.3570(6) 0.4972(5) 0.0224(13) Uani 1 1 d . . .
H2A H -0.0010 -0.2767 0.5196 0.027 Uiso 1 1 calc R . .
H2B H 0.0086 -0.4080 0.5006 0.027 Uiso 1 1 calc R . .
C14 C 0.4370(6) -0.1873(5) 0.0964(4) 0.0120(11) Uani 1 1 d . . .
O17 O 0.3525(5) -0.0116(3) -0.1312(3) 0.0196(9) Uani 1 1 d . . .
N3 N 0.6354(6) -0.2527(5) -0.3695(4) 0.0265(13) Uani 1 1 d . . .
C3 C 0.1901(7) -0.4041(5) 0.5768(5) 0.0195(12) Uani 1 1 d . . .
H3A H 0.1316 -0.4023 0.6521 0.023 Uiso 1 1 calc R . .
H3B H 0.2578 -0.4870 0.5588 0.023 Uiso 1 1 calc R . .
C10 C -0.0329(6) -0.0792(5) 0.2746(5) 0.0153(12) Uani 1 1 d . . .
O23 O 0.6772(6) -0.2653(6) -0.4678(4) 0.0433(14) Uani 1 1 d . . .
C6 C 0.2771(6) -0.2913(5) 0.3689(4) 0.0113(11) Uani 1 1 d . . .
H6 H 0.2157 -0.2059 0.3848 0.014 Uiso 1 1 calc R . .
C13 C 0.4216(7) -0.2015(5) 0.2209(4) 0.0157(12) Uani 1 1 d . . .
H13A H 0.5264 -0.2204 0.2434 0.019 Uiso 1 1 calc R . .
H13B H 0.3475 -0.1273 0.2568 0.019 Uiso 1 1 calc R . .
C8 C -0.0665(7) -0.3497(5) 0.1512(5) 0.0199(13) Uani 1 1 d . . .
C12 C 0.4315(6) -0.4944(5) 0.1654(4) 0.0169(12) Uani 1 1 d . . .
C7 C -0.0310(7) -0.3771(5) 0.2680(5) 0.0181(12) Uani 1 1 d . . .
H7A H -0.1310 -0.3665 0.3193 0.022 Uiso 1 1 calc R . .
H7B H 0.0404 -0.4602 0.2729 0.022 Uiso 1 1 calc R . .
C5 C 0.3880(7) -0.3374(5) 0.4545(5) 0.0181(12) Uani 1 1 d . . .
H5A H 0.4570 -0.4203 0.4381 0.022 Uiso 1 1 calc R . .
H5B H 0.4570 -0.2902 0.4503 0.022 Uiso 1 1 calc R . .
C4 C 0.2933(7) -0.3300(5) 0.5702(4) 0.0194(12) Uani 1 1 d . . .
H4A H 0.3669 -0.3593 0.6238 0.023 Uiso 1 1 calc R . .
H4B H 0.2259 -0.2470 0.5879 0.023 Uiso 1 1 calc R . .
O36 O 0.0055(4) -0.2903(3) 0.0893(3) 0.0161(8) Uani 1 1 d . . .
O22 O 0.5175(5) -0.6015(3) 0.1590(3) 0.0211(9) Uani 1 1 d . . .
O26 O 0.5276(5) -0.1391(4) 0.0461(3) 0.0190(9) Uani 1 1 d . . .
O12 O 0.0722(5) -0.1004(3) 0.1895(3) 0.0181(9) Uani 1 1 d . . .
O15 O -0.1062(5) 0.0219(4) 0.3153(3) 0.0218(9) Uani 1 1 d . . .
O24 O 0.3030(5) -0.4496(3) 0.1279(3) 0.0173(8) Uani 1 1 d . . .
O21 O -0.1618(5) -0.3882(4) 0.1229(4) 0.0282(10) Uani 1 1 d . . .
N1 N 0.0443(5) -0.2987(4) 0.2990(4) 0.0143(10) Uani 1 1 d . . .
C11 C 0.4875(6) -0.4142(5) 0.2205(5) 0.0156(12) Uani 1 1 d . . .
H11A H 0.5298 -0.4547 0.2863 0.019 Uiso 1 1 calc R . .
H11B H 0.5756 -0.3999 0.1702 0.019 Uiso 1 1 calc R . .
O1W O 0.1152(5) 0.0712(4) 0.0409(3) 0.0229(9) Uiso 1 1 d . . .
O2W O 0.8562(5) -0.0966(4) -0.3621(4) 0.0303(10) Uiso 1 1 d . . .
O3W O 0.1064(6) -0.3567(4) -0.1356(4) 0.0347(11) Uiso 1 1 d . . .
O4W O -0.3321(6) 0.0526(5) 0.5052(4) 0.0460(13) Uiso 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 O1 2.401(4) . ?
Dy1 O4 2.459(4) . ?
Dy1 O7 2.565(5) . ?
Dy1 O8 2.350(4) . ?
Dy1 O9 2.430(4) . ?
Dy1 O10 2.346(4) . ?
Dy1 C14 2.867(5) . ?
Dy1 O17 2.379(4) . ?
Dy1 N3 2.929(5) . ?
Dy1 O22 2.355(4) 2_645 ?
Dy1 O26 2.572(4) . ?
Ni1 O4 2.107(4) . ?
Ni1 N2 2.093(4) . ?
Ni1 O36 2.061(4) . ?
Ni1 O12 2.038(4) . ?
Ni1 O24 2.021(4) . ?
Ni1 N1 2.070(5) . ?
O4 C14 1.279(7) . ?
N2 C6 1.494(7) . ?
N2 C13 1.482(7) . ?
N2 C11 1.491(7) . ?
O7 N3 1.251(7) . ?
O9 N3 1.281(7) . ?
C9 C10 1.524(8) . ?
C9 N1 1.467(7) . ?
C1 C2 1.532(8) . ?
C1 C6 1.536(7) . ?
C1 N1 1.505(7) . ?
C2 C3 1.525(8) . ?
C14 C13 1.533(7) . ?
C14 O26 1.242(7) . ?
N3 O23 1.217(7) . ?
C3 C4 1.516(8) . ?
C10 O12 1.268(7) . ?
C10 O15 1.259(7) . ?
C6 C5 1.539(7) . ?
C8 C7 1.533(8) . ?
C8 O36 1.279(7) . ?
C8 O21 1.240(7) . ?
C12 O22 1.254(7) . ?
C12 O24 1.264(7) . ?
C12 C11 1.507(8) . ?
C7 N1 1.470(7) . ?
C5 C4 1.533(8) . ?
O22 Dy1 2.355(4) 2_645 ?

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 O4 74.74(14) . . ?
O1 Dy1 O7 107.53(16) . . ?
O1 Dy1 O9 76.71(15) . . ?
O1 Dy1 C14 97.90(15) . . ?
O1 Dy1 N3 91.54(15) . . ?
O1 Dy1 O26 116.33(14) . . ?
O4 Dy1 O7 148.45(15) . . ?
O4 Dy1 C14 26.40(14) . . ?
O4 Dy1 N3 161.22(13) . . ?
O4 Dy1 O26 51.71(12) . . ?
O7 Dy1 C14 147.77(16) . . ?
O7 Dy1 N3 25.22(16) . . ?
O7 Dy1 O26 136.12(15) . . ?
O8 Dy1 O1 139.05(14) . . ?
O8 Dy1 O4 82.15(14) . . ?
O8 Dy1 O7 76.32(16) . . ?
O8 Dy1 O9 125.71(15) . . ?
O8 Dy1 C14 71.50(15) . . ?
O8 Dy1 O17 141.37(14) . . ?
O8 Dy1 N3 101.14(16) . . ?
O8 Dy1 O22 75.21(14) . 2_645 ?
O8 Dy1 O26 70.18(14) . . ?
O9 Dy1 O4 150.38(14) . . ?
O9 Dy1 O7 50.73(16) . . ?
O9 Dy1 C14 158.88(15) . . ?
O9 Dy1 N3 25.55(16) . . ?
O9 Dy1 O26 140.72(14) . . ?
O10 Dy1 O1 139.97(15) . . ?
O10 Dy1 O4 122.91(13) . . ?
O10 Dy1 O7 76.29(15) . . ?
O10 Dy1 O8 80.97(15) . . ?
O10 Dy1 O9 76.24(15) . . ?
O10 Dy1 C14 96.84(15) . . ?
O10 Dy1 O17 75.01(14) . . ?
O10 Dy1 N3 75.82(14) . . ?
O10 Dy1 O22 142.05(14) . 2_645 ?
O10 Dy1 O26 71.25(13) . . ?
C14 Dy1 N3 170.56(14) . . ?
O17 Dy1 O1 70.62(14) . . ?
O17 Dy1 O4 86.02(14) . . ?
O17 Dy1 O7 124.95(15) . . ?
O17 Dy1 O9 77.20(15) . . ?
O17 Dy1 C14 81.74(15) . . ?
O17 Dy1 N3 101.71(16) . . ?
O17 Dy1 O26 73.63(14) . . ?
O22 Dy1 O1 68.77(14) 2_645 . ?
O22 Dy1 O4 82.77(14) 2_645 . ?
O22 Dy1 O7 69.68(15) 2_645 . ?
O22 Dy1 O9 94.19(16) 2_645 . ?
O22 Dy1 C14 102.93(15) 2_645 . ?
O22 Dy1 O17 139.38(13) 2_645 . ?
O22 Dy1 N3 80.28(15) 2_645 . ?
O22 Dy1 O26 125.04(14) 2_645 . ?
O26 Dy1 C14 25.67(14) . . ?
O26 Dy1 N3 146.84(13) . . ?
N2 Ni1 O4 78.76(16) . . ?
O36 Ni1 O4 115.01(15) . . ?
O36 Ni1 N2 163.90(16) . . ?
O36 Ni1 N1 81.06(16) . . ?
O12 Ni1 O4 87.14(16) . . ?
O12 Ni1 N2 95.12(17) . . ?
O12 Ni1 O36 93.94(16) . . ?
O12 Ni1 N1 84.30(17) . . ?
O24 Ni1 O4 93.17(16) . . ?
O24 Ni1 N2 83.63(17) . . ?
O24 Ni1 O36 87.15(16) . . ?
O24 Ni1 O12 178.62(16) . . ?
O24 Ni1 N1 95.04(18) . . ?
N1 Ni1 O4 162.33(16) . . ?
N1 Ni1 N2 86.63(17) . . ?
Ni1 O4 Dy1 153.78(18) . . ?
C14 O4 Dy1 94.9(3) . . ?
C14 O4 Ni1 111.1(3) . . ?
C6 N2 Ni1 105.5(3) . . ?
C13 N2 Ni1 105.2(3) . . ?
C13 N2 C6 114.0(4) . . ?
C13 N2 C11 110.0(4) . . ?
C11 N2 Ni1 105.6(3) . . ?
C11 N2 C6 115.6(4) . . ?
N3 O7 Dy1 93.9(4) . . ?
N3 O9 Dy1 99.5(3) . . ?
N1 C9 C10 114.4(5) . . ?
C2 C1 C6 113.0(4) . . ?
N1 C1 C2 114.2(5) . . ?
N1 C1 C6 109.2(4) . . ?
C3 C2 C1 112.1(5) . . ?
O4 C14 Dy1 58.7(3) . . ?
O4 C14 C13 118.8(5) . . ?
C13 C14 Dy1 167.0(4) . . ?
O26 C14 Dy1 63.8(3) . . ?
O26 C14 O4 121.2(5) . . ?
O26 C14 C13 120.0(5) . . ?
O7 N3 Dy1 60.9(3) . . ?
O7 N3 O9 115.7(5) . . ?
O9 N3 Dy1 54.9(3) . . ?
O23 N3 Dy1 175.4(4) . . ?
O23 N3 O7 122.6(6) . . ?
O23 N3 O9 121.7(6) . . ?
C4 C3 C2 110.2(5) . . ?
O12 C10 C9 117.8(5) . . ?
O15 C10 C9 118.2(5) . . ?
O15 C10 O12 124.0(5) . . ?
N2 C6 C1 109.6(4) . . ?
N2 C6 C5 114.5(4) . . ?
C1 C6 C5 111.7(4) . . ?
N2 C13 C14 108.1(4) . . ?
O36 C8 C7 117.9(5) . . ?
O21 C8 C7 117.5(5) . . ?
O21 C8 O36 124.6(5) . . ?
O22 C12 O24 124.4(5) . . ?
O22 C12 C11 117.3(5) . . ?
O24 C12 C11 118.3(5) . . ?
N1 C7 C8 110.5(5) . . ?
C4 C5 C6 111.3(4) . . ?
C3 C4 C5 109.2(5) . . ?
C8 O36 Ni1 111.5(3) . . ?
C12 O22 Dy1 138.3(4) . 2_645 ?
C14 O26 Dy1 90.5(3) . . ?
C10 O12 Ni1 113.9(4) . . ?
C12 O24 Ni1 114.9(4) . . ?
C9 N1 Ni1 106.8(3) . . ?
C9 N1 C1 114.7(4) . . ?
C9 N1 C7 110.7(4) . . ?
C1 N1 Ni1 105.2(3) . . ?
C7 N1 Ni1 104.7(3) . . ?
C7 N1 C1 113.9(4) . . ?
N2 C11 C12 113.7(4) . . ?

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1442144'
_audit_update_record             
;
2015-12-14 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_audit_creation_date             2015-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C14 H30 Dy N2 Ni O14, Cl, 2(H2 O)'
_chemical_formula_sum            'C14 H34 Cl Dy N2 Ni O16'
_chemical_formula_weight         743.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   7.558(2)
_cell_length_b                   11.269(3)
_cell_length_c                   15.561(4)
_cell_angle_alpha                100.694(5)
_cell_angle_beta                 103.838(4)
_cell_angle_gamma                105.732(5)
_cell_volume                     1193.4(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.69
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_T_max  0.6853
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5977
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3968
_reflns_number_total             4085
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0221P)²+3.9207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B)
2.b Rotating group:
 O10(H10A,H10B), O14(H14A,H14B), O12(H12A,H12B), O11(H11A,H11B), O13(H13A,
 H13B), O9(H9A,H9B)
2.c Ternary CH refined with riding coordinates:
 C5(H5), C10(H10)
2.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C11(H11C,H11D), C6(H6A,H6B), C2(H2A,H2B), C13(H13C,H13D), C9(H9C,
 H9D), C7(H7A,H7B), C8(H8A,H8B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.58493(3) 0.750846(17) 0.331017(13) 0.01371(8) Uani 1 1 d . . .
Ni1 Ni 1.08403(7) 1.23840(5) 0.30663(4) 0.01240(12) Uani 1 1 d . . .
Cl1 Cl 0.93550(16) 0.66118(11) 0.11959(8) 0.0257(2) Uani 1 1 d . . .
O10 O 0.3426(4) 0.8262(3) 0.2581(2) 0.0180(6) Uani 1 1 d . . .
H10A H 0.2431 0.7614 0.2193 0.027 Uiso 1 1 d R . .
H10B H 0.3885 0.8792 0.2272 0.027 Uiso 1 1 d R . .
O4 O 0.2880(4) 0.5996(3) 0.2963(2) 0.0180(6) Uani 1 1 d . . .
O7 O 0.7230(4) 0.8782(3) 0.2444(2) 0.0185(6) Uani 1 1 d . . .
O1 O 1.0961(4) 1.3246(3) 0.43822(19) 0.0168(6) Uani 1 1 d . . .
O3 O 1.2730(4) 1.4019(3) 0.3018(2) 0.0160(6) Uani 1 1 d . . .
O8 O 0.9025(4) 1.0776(3) 0.3205(2) 0.0166(6) Uani 1 1 d . . .
O14 O 0.5672(4) 0.6134(3) 0.1964(2) 0.0200(7) Uani 1 1 d . . .
H14A H 0.6453 0.6536 0.1688 0.030 Uiso 1 1 d R . .
H14B H 0.4477 0.5844 0.1584 0.030 Uiso 1 1 d R . .
O5 O 1.2800(4) 1.1441(3) 0.3008(2) 0.0198(7) Uani 1 1 d . . .
O12 O 0.6413(4) 0.5835(3) 0.3942(2) 0.0237(7) Uani 1 1 d . . .
H12A H 0.5303 0.5231 0.3858 0.036 Uiso 1 1 d R . .
H12B H 0.7023 0.6137 0.4541 0.036 Uiso 1 1 d R . .
O15 O 1.2502(5) 0.9746(3) 0.4001(2) 0.0273(8) Uani 1 1 d G . .
H15A H 1.3155 0.9291 0.3800 0.041 Uiso 1 1 d G . .
H15B H 1.2369 1.0279 0.3672 0.041 Uiso 1 1 d G . .
N1 N 0.8804(5) 1.3270(3) 0.2773(2) 0.0124(7) Uani 1 1 d . . .
O6 O 1.3832(5) 1.0390(3) 0.1981(2) 0.0235(7) Uani 1 1 d . . .
O2 O 0.8745(4) 1.3303(3) 0.5083(2) 0.0214(7) Uani 1 1 d . . .
N2 N 0.9778(5) 1.1412(3) 0.1682(2) 0.0132(7) Uani 1 1 d . . .
O16 O 1.2042(5) 1.4746(3) 0.0917(2) 0.0269(7) Uani 1 1 d G . .
H16A H 1.1800 1.4441 0.0330 0.040 Uiso 1 1 d G . .
H16B H 1.1311 1.5203 0.1011 0.040 Uiso 1 1 d G . .
O11 O 0.4703(5) 0.7814(3) 0.4640(2) 0.0338(9) Uani 1 1 d . . .
H11A H 0.5622 0.7900 0.5136 0.051 Uiso 1 1 d R . .
H11B H 0.3708 0.7148 0.4570 0.051 Uiso 1 1 d R . .
O13 O 0.9147(5) 0.7825(4) 0.3826(3) 0.0362(9) Uani 1 1 d . . .
H13A H 0.9389 0.7459 0.4270 0.054 Uiso 1 1 d R . .
H13B H 0.9790 0.8647 0.4033 0.054 Uiso 1 1 d R . .
C5 C 0.7522(6) 1.2578(4) 0.1822(3) 0.0123(8) Uani 1 1 d . . .
H5 H 0.6645 1.1758 0.1858 0.015 Uiso 1 1 calc R . .
C14 C 0.8246(6) 0.9870(4) 0.2482(3) 0.0141(8) Uani 1 1 d . . .
C4 C 1.1977(6) 1.4882(4) 0.2957(3) 0.0145(8) Uani 1 1 d . . .
O9 O 0.7013(5) 0.9669(3) 0.4190(2) 0.0331(9) Uani 1 1 d . . .
H9A H 0.6050 0.9908 0.4293 0.050 Uiso 1 1 d R . .
H9B H 0.7580 1.0161 0.3889 0.050 Uiso 1 1 d R . .
C10 C 0.8776(6) 1.2220(4) 0.1244(3) 0.0125(8) Uani 1 1 d . . .
H10 H 0.9794 1.3031 0.1290 0.015 Uiso 1 1 calc R . .
C3 C 0.9884(6) 1.4629(4) 0.2895(3) 0.0142(8) Uani 1 1 d . . .
H3A H 0.9804 1.5150 0.3462 0.017 Uiso 1 1 calc R . .
H3B H 0.9258 1.4911 0.2372 0.017 Uiso 1 1 calc R . .
C12 C 1.2848(6) 1.1025(4) 0.2188(3) 0.0178(9) Uani 1 1 d . . .
C11 C 1.1519(6) 1.1368(4) 0.1435(3) 0.0172(9) Uani 1 1 d . . .
H11C H 1.2202 1.2210 0.1365 0.021 Uiso 1 1 calc R . .
H11D H 1.1156 1.0720 0.0842 0.021 Uiso 1 1 calc R . .
C6 C 0.6245(6) 1.3269(4) 0.1384(3) 0.0176(9) Uani 1 1 d . . .
H6A H 0.7058 1.4127 0.1394 0.021 Uiso 1 1 calc R . .
H6B H 0.5360 1.3386 0.1744 0.021 Uiso 1 1 calc R . .
C2 C 0.7835(6) 1.3142(4) 0.3486(3) 0.0147(8) Uani 1 1 d . . .
H2A H 0.6791 1.2304 0.3285 0.018 Uiso 1 1 calc R . .
H2B H 0.7247 1.3823 0.3574 0.018 Uiso 1 1 calc R . .
C1 C 0.9282(6) 1.3245(4) 0.4388(3) 0.0163(9) Uani 1 1 d . . .
C13 C 0.8512(6) 1.0114(4) 0.1592(3) 0.0168(9) Uani 1 1 d . . .
H13C H 0.9055 0.9485 0.1320 0.020 Uiso 1 1 calc R . .
H13D H 0.7228 0.9965 0.1159 0.020 Uiso 1 1 calc R . .
C9 C 0.7663(6) 1.1609(4) 0.0222(3) 0.0175(9) Uani 1 1 d . . .
H9C H 0.8589 1.1550 -0.0126 0.021 Uiso 1 1 calc R . .
H9D H 0.6809 1.0731 0.0140 0.021 Uiso 1 1 calc R . .
C7 C 0.5068(6) 1.2525(4) 0.0396(3) 0.0216(10) Uani 1 1 d . . .
H7A H 0.4229 1.2986 0.0127 0.026 Uiso 1 1 calc R . .
H7B H 0.4237 1.1670 0.0380 0.026 Uiso 1 1 calc R . .
C8 C 0.6453(7) 1.2384(4) -0.0160(3) 0.0202(9) Uani 1 1 d . . .
H8A H 0.5708 1.1947 -0.0812 0.024 Uiso 1 1 calc R . .
H8B H 0.7308 1.3240 -0.0128 0.024 Uiso 1 1 calc 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 O10 2.360(3) . ?
Dy1 O4 2.289(3) . ?
Dy1 O7 2.355(3) . ?
Dy1 O14 2.314(3) . ?
Dy1 O12 2.372(3) . ?
Dy1 O11 2.430(3) . ?
Dy1 O13 2.332(3) . ?
Dy1 O9 2.367(3) . ?
Ni1 O1 2.066(3) . ?
Ni1 O3 2.028(3) . ?
Ni1 O8 2.037(3) . ?
Ni1 O5 2.053(3) . ?
Ni1 N1 2.060(3) . ?
Ni1 N2 2.075(4) . ?
O4 C4 1.253(5) 1_445 ?
O7 C14 1.240(5) . ?
O1 C1 1.271(5) . ?
O3 C4 1.260(5) . ?
O8 C14 1.259(5) . ?
O5 C12 1.287(5) . ?
N1 C5 1.487(5) . ?
N1 C3 1.479(5) . ?
N1 C2 1.476(5) . ?
O6 C12 1.219(5) . ?
O2 C1 1.240(5) . ?
N2 C10 1.491(5) . ?
N2 C11 1.466(5) . ?
N2 C13 1.475(5) . ?
C5 C10 1.534(5) . ?
C5 C6 1.514(6) . ?
C14 C13 1.509(6) . ?
C4 O4 1.253(5) 1_665 ?
C4 C3 1.505(6) . ?
C10 C9 1.533(6) . ?
C12 C11 1.532(6) . ?
C6 C7 1.523(6) . ?
C2 C1 1.522(6) . ?
C9 C8 1.522(6) . ?
C7 C8 1.530(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Dy1 O12 144.13(11) . . ?
O10 Dy1 O11 86.80(12) . . ?
O10 Dy1 O9 79.23(12) . . ?
O4 Dy1 O10 70.21(10) . . ?
O4 Dy1 O7 131.56(10) . . ?
O4 Dy1 O14 77.92(11) . . ?
O4 Dy1 O12 74.18(11) . . ?
O4 Dy1 O11 71.81(11) . . ?
O4 Dy1 O13 142.32(11) . . ?
O4 Dy1 O9 129.55(12) . . ?
O7 Dy1 O10 74.19(11) . . ?
O7 Dy1 O12 136.61(11) . . ?
O7 Dy1 O11 137.54(11) . . ?
O7 Dy1 O9 72.04(11) . . ?
O14 Dy1 O10 94.01(11) . . ?
O14 Dy1 O7 72.89(10) . . ?
O14 Dy1 O12 82.56(11) . . ?
O14 Dy1 O11 147.49(11) . . ?
O14 Dy1 O13 88.56(13) . . ?
O14 Dy1 O9 144.81(11) . . ?
O12 Dy1 O11 78.12(13) . . ?
O13 Dy1 O10 146.58(11) . . ?
O13 Dy1 O7 74.81(11) . . ?
O13 Dy1 O12 69.25(11) . . ?
O13 Dy1 O11 108.30(13) . . ?
O13 Dy1 O9 79.65(14) . . ?
O9 Dy1 O12 122.45(12) . . ?
O9 Dy1 O11 67.23(12) . . ?
O1 Ni1 N2 161.47(13) . . ?
O3 Ni1 O1 90.56(12) . . ?
O3 Ni1 O8 176.28(12) . . ?
O3 Ni1 O5 91.24(12) . . ?
O3 Ni1 N1 85.10(13) . . ?
O3 Ni1 N2 100.05(13) . . ?
O8 Ni1 O1 86.19(12) . . ?
O8 Ni1 O5 88.46(12) . . ?
O8 Ni1 N1 96.11(13) . . ?
O8 Ni1 N2 83.57(12) . . ?
O5 Ni1 O1 114.37(12) . . ?
O5 Ni1 N1 165.29(13) . . ?
O5 Ni1 N2 80.80(13) . . ?
N1 Ni1 O1 79.96(13) . . ?
N1 Ni1 N2 85.81(13) . . ?
C4 O4 Dy1 145.9(3) 1_445 . ?
C14 O7 Dy1 143.9(3) . . ?
C1 O1 Ni1 109.0(3) . . ?
C4 O3 Ni1 112.1(3) . . ?
C14 O8 Ni1 114.7(3) . . ?
C12 O5 Ni1 113.6(3) . . ?
C5 N1 Ni1 106.7(2) . . ?
C3 N1 Ni1 106.4(2) . . ?
C3 N1 C5 114.5(3) . . ?
C2 N1 Ni1 103.8(2) . . ?
C2 N1 C5 114.0(3) . . ?
C2 N1 C3 110.5(3) . . ?
C10 N2 Ni1 104.1(2) . . ?
C11 N2 Ni1 103.5(3) . . ?
C11 N2 C10 114.7(3) . . ?
C11 N2 C13 110.9(3) . . ?
C13 N2 Ni1 107.8(2) . . ?
C13 N2 C10 114.7(3) . . ?
N1 C5 C10 108.1(3) . . ?
N1 C5 C6 115.0(3) . . ?
C6 C5 C10 112.7(3) . . ?
O7 C14 O8 124.4(4) . . ?
O7 C14 C13 116.9(4) . . ?
O8 C14 C13 118.7(4) . . ?
O4 C4 O3 124.0(4) 1_665 . ?
O4 C4 C3 115.2(4) 1_665 . ?
O3 C4 C3 120.7(4) . . ?
N2 C10 C5 107.7(3) . . ?
N2 C10 C9 113.7(3) . . ?
C9 C10 C5 113.6(3) . . ?
N1 C3 C4 113.8(3) . . ?
O5 C12 C11 115.2(4) . . ?
O6 C12 O5 125.3(4) . . ?
O6 C12 C11 119.5(4) . . ?
N2 C11 C12 109.5(3) . . ?
C5 C6 C7 111.4(4) . . ?
N1 C2 C1 110.2(3) . . ?
O1 C1 C2 118.1(4) . . ?
O2 C1 O1 123.8(4) . . ?
O2 C1 C2 118.1(4) . . ?
N2 C13 C14 114.7(3) . . ?
C8 C9 C10 111.6(3) . . ?
C6 C7 C8 108.8(4) . . ?
C9 C8 C7 109.8(4) . . ?

