# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_p20160601e
_database_code_depnum_ccdc_archive 'CCDC 1522433'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C31 H24 Dy F15 N2 Ni O12'
_chemical_formula_sum            'C31 H24 Dy F15 N2 Ni O12'
_chemical_formula_weight         1122.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         NiDyCHONFCl
_chemical_oxdiff_usercomment     JiangNiDy
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'
F F 0.0171 0.0103 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.2854(7)
_cell_length_b                   12.6822(4)
_cell_length_c                   16.6662(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.946(4)
_cell_angle_gamma                90
_cell_volume                     3827.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    128.45(10)
_cell_measurement_theta_max      27.9180
_cell_measurement_theta_min      3.4220
_exptl_absorpt_coefficient_mu    2.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   0.2
_exptl_transmission_factor_min   0.1
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16229
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.945
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      128.45(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  14.00   1.00    5.50    --   18.94 -57.00 -30.00   64
  2  ω    -47.00  54.00   1.00    5.50    --  -19.25  19.00 150.00  101
  3  ω     63.00  95.00   1.00    5.50    --   18.94 178.00  30.00   32
  4  ω     54.00  87.00   1.00    5.50    --   18.94 178.00-180.00   33
  5  ω    -83.00 -51.00   1.00    5.50    --  -19.25 -57.00  30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0320519000
_diffrn_orient_matrix_UB_12      -0.0284926000
_diffrn_orient_matrix_UB_13      0.0161325000
_diffrn_orient_matrix_UB_21      0.0207862000
_diffrn_orient_matrix_UB_22      0.0272755000
_diffrn_orient_matrix_UB_23      -0.0264098000
_diffrn_orient_matrix_UB_31      0.0088042000
_diffrn_orient_matrix_UB_32      0.0395845000
_diffrn_orient_matrix_UB_33      0.0297961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5068
_reflns_number_total             6729
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+40.4167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1188
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H9A,H9B} of C9, H5 of C5, H4 of C4, H8 of C8, H15 of C15, H10 of C10, H29
  of C29, {H11A,H11B} of C11, H14 of C14, H12 of C12, H16 of C16, H6 of C6, H24
  of C24
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H12A,H12B} of O12, {H19A,H19B,H19C} of C19, H3 of O3
2.a Rotating group:
 O12(H12A,H12B)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B)
2.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C16(H16), C6(H6), C24(H24), C5(H5), C4(H4), C8(H8),
 C15(H15), C29(H29)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.73050(2) 0.49785(4) 0.86576(2) 0.03240(12) Uani 1 1 d . . . . .
Ni1 Ni 0.88668(5) 0.49054(9) 0.77466(6) 0.0300(2) Uani 1 1 d . . . . .
O4 O 0.7769(3) 0.4844(4) 0.7433(3) 0.0285(12) Uani 1 1 d . . . . .
O5 O 0.6371(3) 0.5064(5) 0.7339(3) 0.0365(13) Uani 1 1 d . . . . .
N1 N 0.9943(4) 0.4969(6) 0.8222(4) 0.0370(16) Uani 1 1 d . . . . .
C13 C 0.7770(5) 0.4982(7) 0.5998(5) 0.0356(19) Uani 1 1 d . . . . .
C18 C 0.7420(4) 0.4977(7) 0.6697(4) 0.0305(17) Uani 1 1 d . . . . .
C17 C 0.6653(4) 0.5132(7) 0.6616(5) 0.0324(18) Uani 1 1 d . . . . .
O2 O 0.8559(3) 0.5286(4) 0.8831(3) 0.0312(13) Uani 1 1 d . . . . .
C19 C 0.5583(4) 0.4919(9) 0.7287(5) 0.049(2) Uani 1 1 d . . . . .
H19A H 0.5464 0.4678 0.7799 0.073 Uiso 1 1 calc R U . . .
H19B H 0.5423 0.4406 0.6876 0.073 Uiso 1 1 calc R U . . .
H19C H 0.5338 0.5578 0.7150 0.073 Uiso 1 1 calc R U . . .
O12 O 0.8774(3) 0.6553(4) 0.7444(3) 0.0379(14) Uani 1 1 d . . . . .
H12A H 0.9139 0.6883 0.7699 0.057 Uiso 1 1 d R U . . .
H12B H 0.8375 0.6798 0.7578 0.057 Uiso 1 1 d R U . . .
O1 O 0.7827(3) 0.6350(4) 0.9771(3) 0.0374(14) Uani 1 1 d . . . . .
C14 C 0.7331(5) 0.5162(8) 0.5245(5) 0.047(2) Uani 1 1 d . . . . .
H14 H 0.7551 0.5157 0.4774 0.056 Uiso 1 1 calc R U . . .
N2 N 0.9050(4) 0.4673(5) 0.6591(4) 0.0385(18) Uani 1 1 d . . . . .
O11 O 0.7315(3) 0.6772(4) 0.8118(3) 0.0343(13) Uani 1 1 d . . . . .
F5 F 0.5515(3) 0.1446(5) 0.9262(4) 0.0677(18) Uani 1 1 d . . . . .
O8 O 0.6404(3) 0.3656(5) 0.8648(3) 0.0428(15) Uani 1 1 d . . . . .
O9 O 0.7391(3) 0.4300(4) 0.9981(3) 0.0352(14) Uani 1 1 d . . . . .
F13 F 0.7711(4) 0.8558(5) 0.7533(4) 0.079(2) Uani 1 1 d . . . . .
F7 F 0.7148(4) 0.2564(5) 1.1533(3) 0.0717(19) Uani 1 1 d . . . . .
O7 O 0.7852(3) 0.3295(5) 0.8652(4) 0.0436(15) Uani 1 1 d . . . . .
O10 O 0.6271(3) 0.5840(5) 0.9013(4) 0.0441(15) Uani 1 1 d . . . . .
O6 O 0.8862(3) 0.3294(4) 0.8002(3) 0.0353(13) Uani 1 1 d . . . . .
F4 F 0.5139(3) 0.2553(5) 0.8367(4) 0.074(2) Uani 1 1 d . . . . .
C12 C 0.8541(5) 0.4788(7) 0.5992(5) 0.040(2) Uani 1 1 d . . . . .
H12 H 0.8691 0.4739 0.5482 0.049 Uiso 1 1 calc R U . . .
O3 O 1.0020(5) 0.2876(7) 0.7163(6) 0.081(3) Uani 1 1 d . . . . .
H3 H 0.9653 0.2936 0.7391 0.122 Uiso 1 1 calc R U . . .
F6 F 0.6019(4) 0.1532(6) 0.8199(5) 0.093(2) Uani 1 1 d . . . . .
F8 F 0.8183(4) 0.2936(7) 1.1177(4) 0.097(3) Uani 1 1 d . . . . .
C16 C 0.6243(5) 0.5313(7) 0.5866(5) 0.042(2) Uani 1 1 d . . . . .
H16 H 0.5735 0.5412 0.5819 0.051 Uiso 1 1 calc R U . . .
C6 C 1.0083(6) 0.6832(8) 0.9908(6) 0.049(3) Uani 1 1 d . . . . .
H6 H 1.0592 0.6917 0.9945 0.059 Uiso 1 1 calc R U . . .
C20 C 0.8369(5) 0.2893(7) 0.8366(5) 0.035(2) Uani 1 1 d . . . . .
C2 C 0.8951(5) 0.5964(6) 0.9315(4) 0.0310(19) Uani 1 1 d . . . . .
C23 C 0.6300(4) 0.2924(7) 0.9117(5) 0.034(2) Uani 1 1 d . . . . .
F9 F 0.7536(5) 0.4151(5) 1.1578(3) 0.104(3) Uani 1 1 d . . . . .
C25 C 0.7153(5) 0.3486(7) 1.0277(5) 0.036(2) Uani 1 1 d . . . . .
C3 C 0.8576(5) 0.6564(7) 0.9841(5) 0.038(2) Uani 1 1 d . . . . .
F15 F 0.6823(5) 0.9359(5) 0.7964(5) 0.116(3) Uani 1 1 d . . . . .
F14 F 0.6660(4) 0.8510(8) 0.6908(4) 0.114(3) Uani 1 1 d . . . . .
C7 C 0.9720(4) 0.6101(7) 0.9352(5) 0.0333(19) Uani 1 1 d . . . . .
F11 F 0.5324(4) 0.6653(7) 0.9988(4) 0.104(3) Uani 1 1 d . . . . .
C21 C 0.8415(6) 0.1732(7) 0.8475(6) 0.047(3) Uani 1 1 d . . . . .
C24 C 0.6635(5) 0.2776(7) 0.9913(5) 0.037(2) Uani 1 1 d . . . . .
H24 H 0.6510 0.2192 1.0202 0.044 Uiso 1 1 calc R U . . .
C26 C 0.7501(7) 0.3284(8) 1.1151(5) 0.052(3) Uani 1 1 d . . . . .
C9 C 1.0527(5) 0.4429(9) 0.7850(6) 0.054(3) Uani 1 1 d . . . . .
H9A H 1.0753 0.3910 0.8233 0.065 Uiso 1 1 calc R U . . .
H9B H 1.0903 0.4945 0.7777 0.065 Uiso 1 1 calc R U . . .
C5 C 0.9696(6) 0.7413(8) 1.0391(6) 0.051(3) Uani 1 1 d . . . . .
H5 H 0.9945 0.7904 1.0742 0.061 Uiso 1 1 calc R U . . .
C4 C 0.8945(6) 0.7294(7) 1.0373(5) 0.047(2) Uani 1 1 d . . . . .
H4 H 0.8689 0.7695 1.0710 0.057 Uiso 1 1 calc R U . . .
F12 F 0.4927(5) 0.7761(7) 0.9097(5) 0.120(3) Uani 1 1 d . . . . .
C8 C 1.0180(5) 0.5518(7) 0.8851(5) 0.043(2) Uani 1 1 d . . . . .
H8 H 1.0689 0.5548 0.9003 0.052 Uiso 1 1 calc R U . . .
C30 C 0.6850(5) 0.7500(7) 0.8102(5) 0.040(2) Uani 1 1 d . . . . .
F10 F 0.4745(4) 0.6129(9) 0.8890(6) 0.124(3) Uani 1 1 d . . . . .
C15 C 0.6598(7) 0.5343(8) 0.5193(5) 0.060(3) Uani 1 1 d . . . . .
H15 H 0.6328 0.5490 0.4691 0.072 Uiso 1 1 calc R U . . .
C10 C 1.0301(6) 0.3869(9) 0.7032(6) 0.056(3) Uani 1 1 d . . . . .
H10 H 1.0758 0.3754 0.6798 0.068 Uiso 1 1 calc R U . . .
C31 C 0.7047(7) 0.8515(8) 0.7679(7) 0.062(3) Uani 1 1 d . . . . .
C22 C 0.5742(5) 0.2106(8) 0.8732(6) 0.045(2) Uani 1 1 d . . . . .
C28 C 0.5956(5) 0.6694(9) 0.8859(5) 0.048(2) Uani 1 1 d . . . . .
C29 C 0.6193(6) 0.7528(8) 0.8436(5) 0.050(3) Uani 1 1 d . . . . .
H29 H 0.5904 0.8133 0.8369 0.060 Uiso 1 1 calc R U . . .
C1 C 0.7462(5) 0.6643(8) 1.0444(5) 0.049(3) Uani 1 1 d . . . . .
H1A H 0.6981 0.6326 1.0386 0.074 Uiso 1 1 calc R U . . .
H1B H 0.7415 0.7396 1.0459 0.074 Uiso 1 1 calc R U . . .
H1C H 0.7746 0.6402 1.0938 0.074 Uiso 1 1 calc R U . . .
C11 C 0.9802(5) 0.4524(9) 0.6420(5) 0.051(3) Uani 1 1 d . . . . .
H11A H 1.0026 0.5213 0.6384 0.061 Uiso 1 1 calc R U . . .
H11B H 0.9781 0.4192 0.5893 0.061 Uiso 1 1 calc R U . . .
C27 C 0.5218(7) 0.6807(11) 0.9211(8) 0.072(3) Uani 1 1 d . . . . .
F2 F 0.7772(4) 0.1221(5) 0.8344(4) 0.080(2) Uani 1 1 d . . . . .
F3 F 0.8649(4) 0.1467(6) 0.9258(4) 0.095(2) Uani 1 1 d . . . . .
F1 F 0.8853(5) 0.1265(6) 0.8044(5) 0.102(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.4159(11) . ?
Dy1 O4 2.321(5) . ?
Dy1 O5 2.593(5) . ?
Dy1 O2 2.304(5) . ?
Dy1 O1 2.625(5) . ?
Dy1 O11 2.447(6) . ?
Dy1 O8 2.349(6) . ?
Dy1 O9 2.352(5) . ?
Dy1 O7 2.358(7) . ?
Dy1 O10 2.329(6) . ?
Ni1 O4 2.005(5) . ?
Ni1 N1 2.019(7) . ?
Ni1 O2 2.025(5) . ?
Ni1 O12 2.151(6) . ?
Ni1 N2 2.021(7) . ?
Ni1 O6 2.087(6) . ?
O4 C18 1.314(8) . ?
O5 C17 1.378(9) . ?
O5 C19 1.443(9) . ?
N1 C9 1.474(11) . ?
N1 C8 1.284(11) . ?
C13 C18 1.405(11) . ?
C13 C14 1.412(11) . ?
C13 C12 1.432(12) . ?
C18 C17 1.404(11) . ?
C17 C16 1.385(11) . ?
O2 C2 1.321(9) . ?
O1 C3 1.384(10) . ?
O1 C1 1.432(9) . ?
C14 C15 1.351(14) . ?
N2 C12 1.275(10) . ?
N2 C11 1.455(11) . ?
O11 C30 1.253(10) . ?
F5 C22 1.324(10) . ?
O8 C23 1.245(10) . ?
O9 C25 1.248(10) . ?
F13 C31 1.273(12) . ?
F7 C26 1.330(11) . ?
O7 C20 1.228(10) . ?
O10 C28 1.238(11) . ?
O6 C20 1.261(10) . ?
F4 C22 1.312(10) . ?
O3 C10 1.389(13) . ?
F6 C22 1.303(11) . ?
F8 C26 1.317(13) . ?
C16 C15 1.372(13) . ?
C6 C7 1.411(12) . ?
C6 C5 1.359(13) . ?
C20 C21 1.485(12) . ?
C2 C3 1.409(12) . ?
C2 C7 1.410(11) . ?
C23 C24 1.394(11) . ?
C23 C22 1.534(12) . ?
F9 C26 1.306(11) . ?
C25 C24 1.385(11) . ?
C25 C26 1.528(12) . ?
C3 C4 1.390(12) . ?
F15 C31 1.261(12) . ?
F14 C31 1.379(13) . ?
C7 C8 1.464(13) . ?
F11 C27 1.296(14) . ?
C21 F2 1.335(11) . ?
C21 F3 1.358(10) . ?
C21 F1 1.290(11) . ?
C9 C10 1.543(14) . ?
C5 C4 1.379(13) . ?
F12 C27 1.325(14) . ?
C30 C31 1.534(13) . ?
C30 C29 1.392(12) . ?
F10 C27 1.282(15) . ?
C10 C11 1.519(13) . ?
C28 C29 1.374(14) . ?
C28 C27 1.551(14) . ?

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
O4 Dy1 Ni1 34.72(12) . . ?
O4 Dy1 O5 62.35(17) . . ?
O4 Dy1 O1 121.90(18) . . ?
O4 Dy1 O11 73.93(18) . . ?
O4 Dy1 O8 106.39(19) . . ?
O4 Dy1 O9 144.29(19) . . ?
O4 Dy1 O7 74.0(2) . . ?
O4 Dy1 O10 131.74(19) . . ?
O5 Dy1 Ni1 96.76(12) . . ?
O5 Dy1 O1 134.78(19) . . ?
O2 Dy1 Ni1 35.10(12) . . ?
O2 Dy1 O4 69.20(17) . . ?
O2 Dy1 O5 128.83(17) . . ?
O2 Dy1 O1 62.64(18) . . ?
O2 Dy1 O11 80.27(19) . . ?
O2 Dy1 O8 143.7(2) . . ?
O2 Dy1 O9 90.45(18) . . ?
O2 Dy1 O7 74.9(2) . . ?
O2 Dy1 O10 135.8(2) . . ?
O1 Dy1 Ni1 95.00(13) . . ?
O11 Dy1 Ni1 79.21(13) . . ?
O11 Dy1 O5 71.78(19) . . ?
O11 Dy1 O1 67.87(17) . . ?
O8 Dy1 Ni1 127.29(15) . . ?
O8 Dy1 O5 69.19(19) . . ?
O8 Dy1 O1 131.63(19) . . ?
O8 Dy1 O11 134.6(2) . . ?
O8 Dy1 O9 72.61(19) . . ?
O8 Dy1 O7 69.5(2) . . ?
O9 Dy1 Ni1 117.08(14) . . ?
O9 Dy1 O5 139.52(18) . . ?
O9 Dy1 O1 67.00(18) . . ?
O9 Dy1 O11 132.99(18) . . ?
O9 Dy1 O7 72.5(2) . . ?
O7 Dy1 Ni1 65.98(15) . . ?
O7 Dy1 O5 105.3(2) . . ?
O7 Dy1 O1 119.3(2) . . ?
O7 Dy1 O11 144.65(19) . . ?
O10 Dy1 Ni1 152.06(16) . . ?
O10 Dy1 O5 74.5(2) . . ?
O10 Dy1 O1 74.8(2) . . ?
O10 Dy1 O11 72.9(2) . . ?
O10 Dy1 O8 75.2(2) . . ?
O10 Dy1 O9 83.4(2) . . ?
O10 Dy1 O7 141.7(2) . . ?
O4 Ni1 Dy1 41.24(13) . . ?
O4 Ni1 N1 172.1(2) . . ?
O4 Ni1 O2 81.3(2) . . ?
O4 Ni1 O12 86.1(2) . . ?
O4 Ni1 N2 92.2(3) . . ?
O4 Ni1 O6 89.0(2) . . ?
N1 Ni1 Dy1 130.86(19) . . ?
N1 Ni1 O2 91.0(2) . . ?
N1 Ni1 O12 95.4(3) . . ?
N1 Ni1 N2 95.7(3) . . ?
N1 Ni1 O6 89.5(3) . . ?
O2 Ni1 Dy1 40.86(14) . . ?
O2 Ni1 O12 87.4(2) . . ?
O2 Ni1 O6 92.4(2) . . ?
O12 Ni1 Dy1 91.93(16) . . ?
N2 Ni1 Dy1 133.3(2) . . ?
N2 Ni1 O2 171.3(3) . . ?
N2 Ni1 O12 86.4(2) . . ?
N2 Ni1 O6 93.3(3) . . ?
O6 Ni1 Dy1 84.74(16) . . ?
O6 Ni1 O12 175.1(2) . . ?
Ni1 O4 Dy1 104.0(2) . . ?
C18 O4 Dy1 128.5(5) . . ?
C18 O4 Ni1 125.3(5) . . ?
C17 O5 Dy1 117.5(4) . . ?
C17 O5 C19 116.5(6) . . ?
C19 O5 Dy1 125.5(5) . . ?
C9 N1 Ni1 122.7(6) . . ?
C8 N1 Ni1 122.9(6) . . ?
C8 N1 C9 114.4(8) . . ?
C18 C13 C14 118.0(8) . . ?
C18 C13 C12 124.6(7) . . ?
C14 C13 C12 117.4(8) . . ?
O4 C18 C13 123.9(7) . . ?
O4 C18 C17 117.2(7) . . ?
C17 C18 C13 118.9(7) . . ?
O5 C17 C18 113.4(7) . . ?
O5 C17 C16 125.4(8) . . ?
C16 C17 C18 121.3(8) . . ?
Ni1 O2 Dy1 104.0(2) . . ?
C2 O2 Dy1 129.3(5) . . ?
C2 O2 Ni1 120.4(5) . . ?
C3 O1 Dy1 116.7(5) . . ?
C3 O1 C1 116.4(7) . . ?
C1 O1 Dy1 124.2(5) . . ?
C15 C14 C13 121.4(8) . . ?
C12 N2 Ni1 122.0(6) . . ?
C12 N2 C11 117.9(7) . . ?
C11 N2 Ni1 119.4(5) . . ?
C30 O11 Dy1 130.8(5) . . ?
C23 O8 Dy1 134.1(5) . . ?
C25 O9 Dy1 133.8(5) . . ?
C20 O7 Dy1 136.7(6) . . ?
C28 O10 Dy1 136.8(6) . . ?
C20 O6 Ni1 121.1(6) . . ?
N2 C12 C13 128.7(8) . . ?
C15 C16 C17 119.0(9) . . ?
C5 C6 C7 120.6(9) . . ?
O7 C20 O6 131.3(8) . . ?
O7 C20 C21 113.5(9) . . ?
O6 C20 C21 115.3(9) . . ?
O2 C2 C3 117.5(8) . . ?
O2 C2 C7 124.1(8) . . ?
C3 C2 C7 118.4(8) . . ?
O8 C23 C24 127.8(8) . . ?
O8 C23 C22 113.1(7) . . ?
C24 C23 C22 119.1(8) . . ?
O9 C25 C24 128.2(8) . . ?
O9 C25 C26 113.3(8) . . ?
C24 C25 C26 118.6(8) . . ?
O1 C3 C2 113.7(7) . . ?
O1 C3 C4 124.9(8) . . ?
C4 C3 C2 121.4(9) . . ?
C6 C7 C8 116.8(8) . . ?
C2 C7 C6 119.0(8) . . ?
C2 C7 C8 124.2(8) . . ?
F2 C21 C20 115.3(8) . . ?
F2 C21 F3 100.9(9) . . ?
F3 C21 C20 111.5(8) . . ?
F1 C21 C20 114.6(10) . . ?
F1 C21 F2 106.7(8) . . ?
F1 C21 F3 106.5(8) . . ?
C25 C24 C23 120.9(8) . . ?
F7 C26 C25 114.0(8) . . ?
F8 C26 F7 105.9(9) . . ?
F8 C26 C25 110.8(8) . . ?
F9 C26 F7 107.9(8) . . ?
F9 C26 F8 106.8(9) . . ?
F9 C26 C25 111.1(8) . . ?
N1 C9 C10 117.7(8) . . ?
C6 C5 C4 121.8(9) . . ?
C5 C4 C3 118.8(9) . . ?
N1 C8 C7 125.7(8) . . ?
O11 C30 C31 115.3(8) . . ?
O11 C30 C29 129.0(9) . . ?
C29 C30 C31 115.7(9) . . ?
C14 C15 C16 121.4(8) . . ?
O3 C10 C9 109.8(9) . . ?
O3 C10 C11 113.6(10) . . ?
C11 C10 C9 113.8(9) . . ?
F13 C31 F14 101.7(9) . . ?
F13 C31 C30 114.5(9) . . ?
F15 C31 F13 113.8(11) . . ?
F15 C31 F14 101.7(10) . . ?
F15 C31 C30 115.5(9) . . ?
F14 C31 C30 107.5(10) . . ?
F5 C22 C23 113.5(8) . . ?
F4 C22 F5 105.2(8) . . ?
F4 C22 C23 111.7(8) . . ?
F6 C22 F5 106.8(9) . . ?
F6 C22 F4 107.9(9) . . ?
F6 C22 C23 111.3(8) . . ?
O10 C28 C29 127.5(9) . . ?
O10 C28 C27 114.0(10) . . ?
C29 C28 C27 118.4(10) . . ?
C28 C29 C30 122.5(9) . . ?
N2 C11 C10 115.9(8) . . ?
F11 C27 F12 106.4(11) . . ?
F11 C27 C28 110.2(10) . . ?
F12 C27 C28 112.5(11) . . ?
F10 C27 F11 108.4(12) . . ?
F10 C27 F12 108.5(12) . . ?
F10 C27 C28 110.6(11) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.891
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_niybde_sq
_database_code_depnum_ccdc_archive 'CCDC 1555626'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 N4 Ni2 O22 Yb2'
_chemical_formula_sum            'C48 H58 N4 Ni2 O22 Yb2'
_chemical_formula_weight         1506.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.856(3)
_cell_length_b                   14.164(3)
_cell_length_c                   17.346(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.55(3)
_cell_angle_gamma                90
_cell_volume                     3155.4(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6317
_cell_measurement_temperature    127.1(4)
_cell_measurement_theta_max      28.8390
_cell_measurement_theta_min      3.1050
_exptl_absorpt_coefficient_mu    3.595
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13347
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.876
_diffrn_ambient_temperature      128.60(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4737
_reflns_number_total             5563
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         0.774
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+0.6015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0755
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H9a,H9b} of C9, H6 of C6, H5 of C5, H12 of C12, {H11a,H11b} of C11, H4 of
  C4, {H22a,H22b} of C22, H14 of C14, H10 of C10, H15 of C15, H8 of C8, H16 of
  C16
 At 1.5 times of:
  {H21a,H21b,H21c} of C21, {H23a,H23b,H23c} of C23, H11 of O11, H3 of O3,
  {H1a,H1b,H1c} of C1, {H19a,H19b,H19c} of C19
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 Ni1-H11
 2.733709 with sigma of 0.02
 C22-H11
 1.913868 with sigma of 0.02
3. Rigid bond restraints
 O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O8, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O7, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C11(H11a,H11b), C9(H9a,H9b)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C8(H8), C15(H15), C14(H14), C6(H6), C5(H5), C12(H12), C4(H4)
4.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C23(H23a,H23b,H23c), C21(H21a,H21b,H21c)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 1.2428(2) -0.0092(2) 0.42733(18) 0.0208(7) Uani 1 1 d . U . . .
Yb1 Yb 0.99428(2) 0.13782(2) 0.49473(2) 0.01451(8) Uani 1 1 d . . . . .
Ni1 Ni 0.75573(5) 0.15828(4) 0.56524(3) 0.01751(15) Uani 1 1 d D . . . .
C20 C 1.0158(4) 0.3606(3) 0.5436(3) 0.0220(11) Uani 1 1 d . . . . .
O4 O 0.9070(2) 0.1648(2) 0.60204(16) 0.0174(7) Uani 1 1 d . . . . .
O8 O 1.1640(2) 0.1308(2) 0.44338(18) 0.0200(7) Uani 1 1 d . U . . .
O5 O 1.1061(2) 0.1424(2) 0.61438(17) 0.0193(7) Uani 1 1 d . . . . .
O1 O 0.9520(2) 0.1248(2) 0.35506(17) 0.0189(7) Uani 1 1 d . . . . .
O2 O 0.8240(2) 0.1598(2) 0.46154(17) 0.0189(7) Uani 1 1 d . . . . .
C2 C 0.7808(4) 0.1340(3) 0.3943(3) 0.0164(11) Uani 1 1 d . . . . .
C17 C 1.0555(4) 0.1458(3) 0.6832(3) 0.0169(10) Uani 1 1 d . . . . .
O10 O 0.9419(3) 0.3811(2) 0.5836(2) 0.0324(9) Uani 1 1 d . . . . .
C16 C 1.1041(4) 0.1376(3) 0.7555(3) 0.0219(11) Uani 1 1 d . . . . .
H16 H 1.1759 0.1301 0.7608 0.026 Uiso 1 1 calc R U . . .
N1 N 0.6121(3) 0.1484(3) 0.5112(2) 0.0238(10) Uani 1 1 d . . . . .
C8 C 0.5957(4) 0.1305(3) 0.4396(3) 0.0201(11) Uani 1 1 d . . . . .
H8 H 0.5266 0.1225 0.4228 0.024 Uiso 1 1 calc R U . . .
N2 N 0.7122(3) 0.1657(3) 0.6770(2) 0.0203(9) Uani 1 1 d . . . . .
C15 C 1.0446(4) 0.1406(3) 0.8202(3) 0.0277(13) Uani 1 1 d . . . . .
H15 H 1.0766 0.1367 0.8692 0.033 Uiso 1 1 calc R U . . .
C24 C 1.1681(4) 0.0400(3) 0.4484(2) 0.0174(9) Uani 1 1 d . U . . .
C19 C 1.2184(4) 0.1408(3) 0.6211(3) 0.0279(13) Uani 1 1 d . . . . .
H19A H 1.2413 0.0815 0.6426 0.042 Uiso 1 1 calc R U . . .
H19B H 1.2426 0.1913 0.6541 0.042 Uiso 1 1 calc R U . . .
H19C H 1.2459 0.1484 0.5709 0.042 Uiso 1 1 calc R U . . .
C10 C 0.5303(4) 0.1195(4) 0.6378(3) 0.0375(14) Uani 1 1 d . . . . .
H10 H 0.4612 0.1217 0.6594 0.045 Uiso 1 1 calc R U . . .
O6 O 1.0865(2) 0.0032(2) 0.47892(19) 0.0242(8) Uani 1 1 d . U . . .
C14 C 0.9382(4) 0.1495(3) 0.8118(3) 0.0245(12) Uani 1 1 d . . . . .
H14 H 0.8991 0.1507 0.8556 0.029 Uiso 1 1 calc R U . . .
C18 C 0.9471(4) 0.1558(3) 0.6735(2) 0.0147(10) Uani 1 1 d . . . . .
C7 C 0.6730(4) 0.1213(3) 0.3814(3) 0.0194(11) Uani 1 1 d . . . . .
C22 C 0.7171(4) 0.3595(3) 0.4939(3) 0.0373(14) Uani 1 1 d D . . . .
H22A H 0.6772 0.3176 0.4596 0.045 Uiso 1 1 calc R U . . .
H22B H 0.7756 0.3833 0.4663 0.045 Uiso 1 1 calc R U . . .
C3 C 0.8469(4) 0.1165(3) 0.3337(3) 0.0177(10) Uani 1 1 d . . . . .
C13 C 0.8872(4) 0.1568(3) 0.7393(3) 0.0195(11) Uani 1 1 d . . . . .
C1 C 1.0230(4) 0.1153(3) 0.2928(3) 0.0237(12) Uani 1 1 d . . . . .
H1A H 1.0924 0.1303 0.3116 0.036 Uiso 1 1 calc R U . . .
H1B H 1.0026 0.1578 0.2517 0.036 Uiso 1 1 calc R U . . .
H1C H 1.0211 0.0516 0.2739 0.036 Uiso 1 1 calc R U . . .
O11 O 0.7555(2) 0.3071(2) 0.56190(17) 0.0228(8) Uani 1 1 d D . . . .
H11 H 0.810(2) 0.3383(14) 0.5795(19) 0.034 Uiso 1 1 d D U . . .
O3 O 0.5619(3) 0.0202(3) 0.6386(3) 0.0512(12) Uani 1 1 d . . . . .
H3 H 0.6060 0.0118 0.6066 0.077 Uiso 1 1 calc R U . . .
C6 C 0.6356(4) 0.0973(3) 0.3054(3) 0.0240(11) Uani 1 1 d . . . . .
H6 H 0.5644 0.0892 0.2957 0.029 Uiso 1 1 calc R U . . .
C5 C 0.7013(4) 0.0858(3) 0.2465(3) 0.0283(12) Uani 1 1 d . . . . .
H5 H 0.6747 0.0724 0.1970 0.034 Uiso 1 1 calc R U . . .
C12 C 0.7753(4) 0.1667(3) 0.7362(3) 0.0225(11) Uani 1 1 d . . . . .
H12 H 0.7451 0.1748 0.7835 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6009(4) 0.1774(4) 0.6907(3) 0.0344(14) Uani 1 1 d . . . . .
H11A H 0.5827 0.2435 0.6844 0.041 Uiso 1 1 calc R U . . .
H11B H 0.5889 0.1600 0.7437 0.041 Uiso 1 1 calc R U . . .
C4 C 0.8080(4) 0.0943(3) 0.2606(3) 0.0248(12) Uani 1 1 d . . . . .
H4 H 0.8531 0.0851 0.2208 0.030 Uiso 1 1 calc R U . . .
O9 O 1.0199(3) 0.2902(2) 0.49779(16) 0.0237(8) Uani 1 1 d . . . . .
C9 C 0.5172(4) 0.1552(4) 0.5567(3) 0.0377(14) Uani 1 1 d . . . . .
H9A H 0.4618 0.1198 0.5303 0.045 Uiso 1 1 calc R U . . .
H9B H 0.4956 0.2208 0.5582 0.045 Uiso 1 1 calc R U . . .
C23 C 0.6516(6) 0.4383(5) 0.5163(4) 0.073(2) Uani 1 1 d . . . . .
H23A H 0.6894 0.4770 0.5534 0.109 Uiso 1 1 calc R U . . .
H23B H 0.5900 0.4144 0.5388 0.109 Uiso 1 1 calc R U . . .
H23C H 0.6323 0.4754 0.4716 0.109 Uiso 1 1 calc R U . . .
C21 C 1.1096(4) 0.4233(4) 0.5466(3) 0.0426(15) Uani 1 1 d . . . . .
H21A H 1.1083 0.4628 0.5016 0.064 Uiso 1 1 calc R U . . .
H21B H 1.1715 0.3853 0.5481 0.064 Uiso 1 1 calc R U . . .
H21C H 1.1092 0.4620 0.5920 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Ni1 2.116(3) 3_756 ?
O7 C24 1.254(5) . ?
Yb1 Yb1 3.9110(9) 3_756 ?
Yb1 Ni1 3.3645(10) . ?
Yb1 O4 2.248(3) . ?
Yb1 O8 2.395(3) . ?
Yb1 O5 2.473(3) . ?
Yb1 O1 2.466(3) . ?
Yb1 O2 2.260(3) . ?
Yb1 C24 2.778(5) . ?
Yb1 O6 2.268(3) . ?
Yb1 O6 2.307(3) 3_756 ?
Yb1 C18 3.197(4) . ?
Yb1 O9 2.184(3) . ?
Ni1 O7 2.116(3) 3_756 ?
Ni1 O4 2.022(3) . ?
Ni1 O2 2.036(3) . ?
Ni1 N1 2.038(4) . ?
Ni1 N2 2.043(4) . ?
Ni1 O11 2.108(3) . ?
C20 O10 1.236(6) . ?
C20 O9 1.278(5) . ?
C20 C21 1.497(7) . ?
O4 C18 1.328(5) . ?
O8 C24 1.290(5) . ?
O5 C17 1.386(5) . ?
O5 C19 1.443(5) . ?
O1 C3 1.390(5) . ?
O1 C1 1.451(5) . ?
O2 C2 1.321(5) . ?
C2 C7 1.406(6) . ?
C2 C3 1.403(7) . ?
C17 C16 1.380(6) . ?
C17 C18 1.405(6) . ?
C16 C15 1.387(7) . ?
N1 C8 1.276(6) . ?
N1 C9 1.485(6) . ?
C8 C7 1.454(6) . ?
N2 C12 1.281(6) . ?
N2 C11 1.471(6) . ?
C15 C14 1.374(7) . ?
C24 O6 1.305(5) . ?
C10 O3 1.464(6) . ?
C10 C11 1.505(7) . ?
C10 C9 1.497(7) . ?
O6 Yb1 2.307(3) 3_756 ?
C14 C13 1.397(6) . ?
C18 C13 1.404(6) . ?
C7 C6 1.423(6) . ?
C22 O11 1.461(6) . ?
C22 C23 1.463(7) . ?
C3 C4 1.379(6) . ?
C13 C12 1.443(6) . ?
C6 C5 1.364(7) . ?
C5 C4 1.387(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
C24 O7 Ni1 122.8(3) . 3_756 ?
Ni1 Yb1 Yb1 95.852(12) . 3_756 ?
O4 Yb1 Yb1 98.63(8) . 3_756 ?
O4 Yb1 Ni1 35.70(8) . . ?
O4 Yb1 O8 144.22(11) . . ?
O4 Yb1 O5 66.02(10) . . ?
O4 Yb1 O1 136.86(11) . . ?
O4 Yb1 O2 70.98(11) . . ?
O4 Yb1 C24 139.62(12) . . ?
O4 Yb1 O6 74.78(11) . 3_756 ?
O4 Yb1 O6 121.71(11) . . ?
O4 Yb1 C18 19.95(11) . . ?
O8 Yb1 Yb1 86.73(7) . 3_756 ?
O8 Yb1 Ni1 177.40(7) . . ?
O8 Yb1 O5 78.92(10) . . ?
O8 Yb1 O1 78.25(11) . . ?
O8 Yb1 C24 27.62(11) . . ?
O8 Yb1 C18 125.42(11) . . ?
O5 Yb1 Yb1 88.14(7) . 3_756 ?
O5 Yb1 Ni1 101.43(7) . . ?
O5 Yb1 C24 79.09(11) . . ?
O5 Yb1 C18 46.53(11) . . ?
O1 Yb1 Yb1 88.70(7) . 3_756 ?
O1 Yb1 Ni1 101.47(8) . . ?
O1 Yb1 O5 157.09(11) . . ?
O1 Yb1 C24 79.82(12) . . ?
O1 Yb1 C18 156.33(11) . . ?
O2 Yb1 Yb1 100.57(8) . 3_756 ?
O2 Yb1 Ni1 36.15(8) . . ?
O2 Yb1 O8 143.04(11) . . ?
O2 Yb1 O5 136.95(10) . . ?
O2 Yb1 O1 65.88(11) . . ?
O2 Yb1 C24 141.01(12) . . ?
O2 Yb1 O6 74.35(11) . 3_756 ?
O2 Yb1 O6 126.19(11) . . ?
O2 Yb1 C18 90.72(11) . . ?
C24 Yb1 Yb1 59.11(10) . 3_756 ?
C24 Yb1 Ni1 154.96(10) . . ?
C24 Yb1 C18 120.69(12) . . ?
O6 Yb1 Yb1 31.54(8) . 3_756 ?
O6 Yb1 Yb1 30.96(8) 3_756 3_756 ?
O6 Yb1 Ni1 64.96(8) 3_756 . ?
O6 Yb1 Ni1 127.31(8) . . ?
O6 Yb1 O8 117.61(10) 3_756 . ?
O6 Yb1 O8 55.28(10) . . ?
O6 Yb1 O5 96.11(11) 3_756 . ?
O6 Yb1 O5 80.55(11) . . ?
O6 Yb1 O1 84.94(11) . . ?
O6 Yb1 O1 92.76(11) 3_756 . ?
O6 Yb1 C24 90.03(13) 3_756 . ?
O6 Yb1 C24 27.67(12) . . ?
O6 Yb1 O6 62.51(14) . 3_756 ?
O6 Yb1 C18 76.70(11) 3_756 . ?
O6 Yb1 C18 107.87(12) . . ?
C18 Yb1 Yb1 92.42(8) . 3_756 ?
C18 Yb1 Ni1 54.90(9) . . ?
O9 Yb1 Yb1 168.59(8) . 3_756 ?
O9 Yb1 Ni1 92.58(9) . . ?
O9 Yb1 O4 83.81(11) . . ?
O9 Yb1 O8 84.90(11) . . ?
O9 Yb1 O5 82.66(10) . . ?
O9 Yb1 O1 97.15(10) . . ?
O9 Yb1 O2 90.77(11) . . ?
O9 Yb1 C24 112.18(13) . . ?
O9 Yb1 O6 138.99(12) . . ?
O9 Yb1 O6 156.93(12) . 3_756 ?
O9 Yb1 C18 86.15(11) . . ?
O7 Ni1 Yb1 86.01(9) 3_756 . ?
O4 Ni1 O7 91.17(12) . 3_756 ?
O4 Ni1 Yb1 40.46(8) . . ?
O4 Ni1 O2 80.33(12) . . ?
O4 Ni1 N1 170.90(14) . . ?
O4 Ni1 N2 89.90(14) . . ?
O4 Ni1 O11 87.89(12) . . ?
O2 Ni1 O7 93.52(12) . 3_756 ?
O2 Ni1 Yb1 40.90(9) . . ?
O2 Ni1 N1 90.67(14) . . ?
O2 Ni1 N2 169.75(14) . . ?
O2 Ni1 O11 88.01(12) . . ?
N1 Ni1 O7 87.98(14) . 3_756 ?
N1 Ni1 Yb1 130.45(12) . . ?
N1 Ni1 N2 99.16(16) . . ?
N1 Ni1 O11 93.21(14) . . ?
N2 Ni1 O7 89.75(14) . 3_756 ?
N2 Ni1 Yb1 129.90(11) . . ?
N2 Ni1 O11 88.55(14) . . ?
O11 Ni1 O7 178.06(13) . 3_756 ?
O11 Ni1 Yb1 94.37(9) . . ?
O10 C20 O9 125.9(5) . . ?
O10 C20 C21 118.6(4) . . ?
O9 C20 C21 115.4(5) . . ?
Ni1 O4 Yb1 103.84(12) . . ?
C18 O4 Yb1 124.8(3) . . ?
C18 O4 Ni1 128.2(3) . . ?
C24 O8 Yb1 93.0(3) . . ?
C17 O5 Yb1 116.5(3) . . ?
C17 O5 C19 115.9(3) . . ?
C19 O5 Yb1 127.5(3) . . ?
C3 O1 Yb1 116.0(3) . . ?
C3 O1 C1 115.5(3) . . ?
C1 O1 Yb1 128.2(3) . . ?
Ni1 O2 Yb1 102.95(12) . . ?
C2 O2 Yb1 123.4(3) . . ?
C2 O2 Ni1 126.6(3) . . ?
O2 C2 C7 123.3(4) . . ?
O2 C2 C3 117.8(4) . . ?
C3 C2 C7 118.9(4) . . ?
O5 C17 C18 113.7(4) . . ?
C16 C17 O5 124.7(4) . . ?
C16 C17 C18 121.5(4) . . ?
C17 C16 C15 119.3(5) . . ?
C8 N1 Ni1 124.6(3) . . ?
C8 N1 C9 115.2(4) . . ?
C9 N1 Ni1 120.0(3) . . ?
N1 C8 C7 127.3(4) . . ?
C12 N2 Ni1 124.9(3) . . ?
C12 N2 C11 117.0(4) . . ?
C11 N2 Ni1 118.0(3) . . ?
C14 C15 C16 119.9(5) . . ?
O7 C24 Yb1 176.1(3) . . ?
O7 C24 O8 124.3(4) . . ?
O7 C24 O6 122.5(4) . . ?
O8 C24 Yb1 59.4(2) . . ?
O8 C24 O6 113.2(4) . . ?
O6 C24 Yb1 53.8(2) . . ?
O3 C10 C11 111.0(5) . . ?
O3 C10 C9 110.7(4) . . ?
C9 C10 C11 115.4(5) . . ?
Yb1 O6 Yb1 117.49(14) . 3_756 ?
C24 O6 Yb1 143.5(3) . 3_756 ?
C24 O6 Yb1 98.5(3) . . ?
C15 C14 C13 121.9(5) . . ?
O4 C18 Yb1 35.30(19) . . ?
O4 C18 C17 117.6(4) . . ?
O4 C18 C13 123.6(4) . . ?
C17 C18 Yb1 83.0(3) . . ?
C13 C18 Yb1 157.4(3) . . ?
C13 C18 C17 118.8(4) . . ?
C2 C7 C8 125.2(4) . . ?
C2 C7 C6 117.9(4) . . ?
C6 C7 C8 116.8(4) . . ?
O11 C22 C23 110.5(5) . . ?
O1 C3 C2 113.5(4) . . ?
C4 C3 O1 124.9(4) . . ?
C4 C3 C2 121.6(5) . . ?
C14 C13 C18 118.5(4) . . ?
C14 C13 C12 117.9(4) . . ?
C18 C13 C12 123.6(4) . . ?
C22 O11 Ni1 122.0(3) . . ?
C5 C6 C7 121.8(5) . . ?
C6 C5 C4 119.9(4) . . ?
N2 C12 C13 128.5(4) . . ?
N2 C11 C10 113.9(4) . . ?
C3 C4 C5 119.8(5) . . ?
C20 O9 Yb1 140.9(3) . . ?
N1 C9 C10 114.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 C24 O6 Yb1 -8.2(8) . . . 3_756 ?
O7 C24 O6 Yb1 -178.4(4) . . . . ?
Yb1 O4 C18 C17 12.3(5) . . . . ?
Yb1 O4 C18 C13 -168.5(3) . . . . ?
Yb1 O8 C24 O7 178.6(4) . . . . ?
Yb1 O8 C24 O6 -2.3(4) . . . . ?
Yb1 O5 C17 C16 172.1(3) . . . . ?
Yb1 O5 C17 C18 -6.1(5) . . . . ?
Yb1 O1 C3 C2 10.9(5) . . . . ?
Yb1 O1 C3 C4 -169.8(4) . . . . ?
Yb1 O2 C2 C7 160.5(3) . . . . ?
Yb1 O2 C2 C3 -18.0(5) . . . . ?
Yb1 C24 O6 Yb1 170.2(6) . . . 3_756 ?
Yb1 C18 C13 C14 164.4(6) . . . . ?
Yb1 C18 C13 C12 -16.6(11) . . . . ?
Ni1 O7 C24 O8 -178.8(3) 3_756 . . . ?
Ni1 O7 C24 O6 2.3(6) 3_756 . . . ?
Ni1 O4 C18 Yb1 156.3(5) . . . . ?
Ni1 O4 C18 C17 168.6(3) . . . . ?
Ni1 O4 C18 C13 -12.2(6) . . . . ?
Ni1 O2 C2 C7 14.9(6) . . . . ?
Ni1 O2 C2 C3 -163.6(3) . . . . ?
Ni1 N1 C8 C7 -5.4(7) . . . . ?
Ni1 N1 C9 C10 -30.4(6) . . . . ?
Ni1 N2 C12 C13 -4.4(7) . . . . ?
Ni1 N2 C11 C10 40.6(6) . . . . ?
O4 C18 C13 C14 -178.1(4) . . . . ?
O4 C18 C13 C12 0.8(7) . . . . ?
O8 C24 O6 Yb1 172.7(3) . . . 3_756 ?
O8 C24 O6 Yb1 2.5(4) . . . . ?
O5 C17 C16 C15 -179.0(4) . . . . ?
O5 C17 C18 Yb1 4.3(3) . . . . ?
O5 C17 C18 O4 -2.9(6) . . . . ?
O5 C17 C18 C13 177.9(4) . . . . ?
O1 C3 C4 C5 178.5(4) . . . . ?
O2 C2 C7 C8 -2.8(7) . . . . ?
O2 C2 C7 C6 177.3(4) . . . . ?
O2 C2 C3 O1 3.0(6) . . . . ?
O2 C2 C3 C4 -176.3(4) . . . . ?
C2 C7 C6 C5 0.6(7) . . . . ?
C2 C3 C4 C5 -2.2(7) . . . . ?
C17 C16 C15 C14 1.5(7) . . . . ?
C17 C18 C13 C14 1.1(7) . . . . ?
C17 C18 C13 C12 -180.0(4) . . . . ?
O10 C20 O9 Yb1 -50.0(8) . . . . ?
C16 C17 C18 Yb1 -174.0(4) . . . . ?
C16 C17 C18 O4 178.9(4) . . . . ?
C16 C17 C18 C13 -0.4(7) . . . . ?
C16 C15 C14 C13 -0.8(7) . . . . ?
N1 C8 C7 C2 -2.3(8) . . . . ?
N1 C8 C7 C6 177.6(4) . . . . ?
C8 N1 C9 C10 145.4(5) . . . . ?
C8 C7 C6 C5 -179.3(4) . . . . ?
C15 C14 C13 C18 -0.5(7) . . . . ?
C15 C14 C13 C12 -179.5(4) . . . . ?
C19 O5 C17 C16 -7.2(6) . . . . ?
C19 O5 C17 C18 174.6(4) . . . . ?
C14 C13 C12 N2 -172.9(5) . . . . ?
C18 C17 C16 C15 -0.9(7) . . . . ?
C18 C13 C12 N2 8.1(8) . . . . ?
C7 C2 C3 O1 -175.6(4) . . . . ?
C7 C2 C3 C4 5.0(7) . . . . ?
C7 C6 C5 C4 2.3(8) . . . . ?
C3 C2 C7 C8 175.7(4) . . . . ?
C3 C2 C7 C6 -4.1(6) . . . . ?
C1 O1 C3 C2 -174.9(4) . . . . ?
C1 O1 C3 C4 4.4(6) . . . . ?
O3 C10 C11 N2 52.2(6) . . . . ?
O3 C10 C9 N1 -59.0(6) . . . . ?
C6 C5 C4 C3 -1.5(8) . . . . ?
C12 N2 C11 C10 -143.5(5) . . . . ?
C11 N2 C12 C13 -180.0(5) . . . . ?
C11 C10 C9 N1 68.1(6) . . . . ?
C9 N1 C8 C7 179.0(5) . . . . ?
C9 C10 C11 N2 -74.7(6) . . . . ?
C23 C22 O11 Ni1 135.9(4) . . . . ?
C21 C20 O9 Yb1 131.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_nitm_sq
_database_code_depnum_ccdc_archive 'CCDC 1555625'

_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 N4 Ni2 O22 Tm2'
_chemical_formula_sum            'C48 H58 N4 Ni2 O22 Tm2'
_chemical_formula_weight         1498.26
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.970(3)
_cell_length_b                   14.473(3)
_cell_length_c                   17.537(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.72(3)
_cell_angle_gamma                90
_cell_volume                     3291.6(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9115
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      1.4069
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6379
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ASDABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.109
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.4000
_diffrn_measured_fraction_theta_max 27.8864
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1864
	          2theta: -29.8131
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1864
	          2theta: -29.8131
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1864
	          2theta: -29.8131
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             8132
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0678
_diffrn_orient_matrix_UB_12      -0.0103
_diffrn_orient_matrix_UB_13      -0.0353
_diffrn_orient_matrix_UB_21      -0.0318
_diffrn_orient_matrix_UB_22      -0.0013
_diffrn_orient_matrix_UB_23      0.0613
_diffrn_orient_matrix_UB_31      -0.0078
_diffrn_orient_matrix_UB_32      0.0564
_diffrn_orient_matrix_UB_33      -0.0029
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5049
_reflns_number_total             5794
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.080
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0363
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0955
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H20a,H20b} of C20, {H9a,H9b} of C9, {H11a,H11b} of C11, H4 of C4, H5 of C5,
   H8 of C8, H14 of C14, H10 of C10, H6 of C6, H15 of C15, H16 of C16, H12 of
  C12
 At 1.5 times of:
  {H22a,H22b,H22c} of C221, {H23a,H23b,H23c} of C23, H3 of O3, {H1a,H1b,H1c}
  of C1, H11 of O11, {H19a,H19b,H19c} of C19
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C221-C20
 1.52 with sigma of 0.02
 C23-C22
 1.52 with sigma of 0.02
 C20-H11
 1.896421 with sigma of 0.02
 Ni1-H11
 2.738164 with sigma of 0.02
3. Rigid bond restraints
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O8, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C9(H9a,H9b), C20(H20a,H20b)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C6(H6), C15(H15), C16(H16), C12(H12), C5(H5), C4(H4)
4.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C23(H23a,H23b,H23c), C221(H22a,H22b,H22c)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.2577(3) 0.49036(19) 1.0754(2) 0.0456(8) Uani 1 1 d . U . . .
Tm1 Tm 0.50598(2) 0.63628(2) 1.00542(2) 0.03313(10) Uani 1 1 d . . . . .
Ni1 Ni 0.74626(4) 0.65566(4) 0.93403(3) 0.03863(16) Uani 1 1 d D . . . .
O1 O 0.5451(3) 0.6307(2) 1.14477(18) 0.0429(8) Uani 1 1 d . . . . .
O5 O 0.4012(2) 0.6362(2) 0.88735(19) 0.0442(8) Uani 1 1 d . . . . .
C17 C 0.4549(4) 0.6363(3) 0.8182(3) 0.0409(11) Uani 1 1 d . . . . .
O4 O 0.5972(2) 0.6662(2) 0.89812(16) 0.0387(7) Uani 1 1 d . . . . .
O2 O 0.6740(2) 0.6548(2) 1.03637(17) 0.0416(7) Uani 1 1 d . . . . .
O8 O 0.3354(2) 0.62775(19) 1.05769(19) 0.0448(8) Uani 1 1 d . U . . .
C2 C 0.7152(4) 0.6340(3) 1.1043(3) 0.0349(10) Uani 1 1 d . . . . .
N1 N 0.8865(3) 0.6430(3) 0.9856(3) 0.0485(10) Uani 1 1 d . . . . .
N2 N 0.7943(3) 0.6632(3) 0.8234(2) 0.0466(10) Uani 1 1 d . . . . .
C24 C 0.3326(3) 0.5392(3) 1.0551(2) 0.0391(9) Uani 1 1 d . U . . .
O6 O 0.4168(3) 0.50220(17) 1.0282(2) 0.0500(9) Uani 1 1 d . U . . .
C18 C 0.5611(4) 0.6512(3) 0.8291(3) 0.0353(10) Uani 1 1 d . . . . .
C8 C 0.9012(4) 0.6278(3) 1.0581(3) 0.0480(12) Uani 1 1 d . . . . .
H8 H 0.9692 0.6194 1.0741 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6234(4) 0.6502(3) 0.7633(3) 0.0427(11) Uani 1 1 d . . . . .
C3 C 0.6482(4) 0.6222(3) 1.1657(3) 0.0406(11) Uani 1 1 d . . . . .
C14 C 0.5752(5) 0.6384(4) 0.6913(3) 0.0602(15) Uani 1 1 d . . . . .
H14 H 0.6158 0.6397 0.6480 0.072 Uiso 1 1 calc R U . . .
C10 C 0.9708(4) 0.6131(4) 0.8599(3) 0.0650(15) Uani 1 1 d . . . . .
H10 H 1.0398 0.6141 0.8378 0.078 Uiso 1 1 calc R U . . .
C6 C 0.8570(4) 0.6030(3) 1.1915(3) 0.0548(13) Uani 1 1 d . . . . .
H6 H 0.9271 0.5943 1.2010 0.066 Uiso 1 1 calc R U . . .
C15 C 0.4724(5) 0.6251(4) 0.6827(3) 0.0658(16) Uani 1 1 d . . . . .
H15 H 0.4432 0.6165 0.6345 0.079 Uiso 1 1 calc R U . . .
C7 C 0.8233(4) 0.6225(3) 1.1171(3) 0.0436(11) Uani 1 1 d . . . . .
C1 C 0.4721(4) 0.6255(4) 1.2067(3) 0.0549(14) Uani 1 1 d . . . . .
H1A H 0.4039 0.6380 1.1874 0.082 Uiso 1 1 calc R U . . .
H1B H 0.4901 0.6703 1.2450 0.082 Uiso 1 1 calc R U . . .
H1C H 0.4741 0.5648 1.2286 0.082 Uiso 1 1 calc R U . . .
C16 C 0.4106(4) 0.6246(3) 0.7479(3) 0.0539(13) Uani 1 1 d . . . . .
H16 H 0.3397 0.6162 0.7431 0.065 Uiso 1 1 calc R U . . .
O11 O 0.7477(3) 0.8024(2) 0.9390(2) 0.0555(9) Uani 1 1 d D . . . .
H11 H 0.697(3) 0.8345(15) 0.921(2) 0.083 Uiso 1 1 d D U . . .
C19 C 0.2885(4) 0.6359(4) 0.8811(4) 0.0607(16) Uani 1 1 d . . . . .
H19A H 0.2661 0.5797 0.8570 0.091 Uiso 1 1 calc R U . . .
H19B H 0.2661 0.6878 0.8511 0.091 Uiso 1 1 calc R U . . .
H19C H 0.2595 0.6400 0.9311 0.091 Uiso 1 1 calc R U . . .
C12 C 0.7332(4) 0.6611(3) 0.7653(3) 0.0491(12) Uani 1 1 d . . . . .
H12 H 0.7644 0.6674 0.7182 0.059 Uiso 1 1 calc R U . . .
O9 O 0.4785(3) 0.7862(2) 1.00244(17) 0.0546(9) Uani 1 1 d . . . . .
C5 C 0.7898(5) 0.5964(4) 1.2503(3) 0.0621(14) Uani 1 1 d . . . . .
H5 H 0.8152 0.5861 1.2994 0.075 Uiso 1 1 calc R U . . .
O3 O 0.9389(4) 0.5179(3) 0.8590(3) 0.0879(14) Uani 1 1 d . . . . .
H3 H 0.8784 0.5146 0.8451 0.132 Uiso 1 1 calc R U . . .
C4 C 0.6851(4) 0.6048(3) 1.2386(3) 0.0545(13) Uani 1 1 d . . . . .
H4 H 0.6398 0.5989 1.2790 0.065 Uiso 1 1 calc R U . . .
C11 C 0.9045(4) 0.6750(4) 0.8094(3) 0.0646(15) Uani 1 1 d . . . . .
H11A H 0.9233 0.7389 0.8186 0.078 Uiso 1 1 calc R U . . .
H11B H 0.9182 0.6612 0.7564 0.078 Uiso 1 1 calc R U . . .
C9 C 0.9838(4) 0.6457(4) 0.9413(4) 0.0771(19) Uani 1 1 d . . . . .
H9A H 1.0350 0.6073 0.9668 0.093 Uiso 1 1 calc R U . . .
H9B H 1.0098 0.7086 0.9411 0.093 Uiso 1 1 calc R U . . .
O10 O 0.5637(3) 0.8789(3) 0.9239(3) 0.0819(13) Uani 1 1 d . . . . .
C22 C 0.4868(4) 0.8557(3) 0.9583(3) 0.0497(13) Uani 1 1 d D . . . .
C23 C 0.3931(5) 0.9132(5) 0.9495(5) 0.100(3) Uani 1 1 d D . . . .
H23A H 0.3420 0.8800 0.9205 0.150 Uiso 1 1 calc R U . . .
H23B H 0.4101 0.9694 0.9234 0.150 Uiso 1 1 calc R U . . .
H23C H 0.3665 0.9277 0.9989 0.150 Uiso 1 1 calc R U . . .
C20 C 0.7849(6) 0.8539(4) 1.0032(5) 0.095(2) Uani 1 1 d D . . . .
H20A H 0.7269 0.8795 1.0305 0.114 Uiso 1 1 calc R U . . .
H20B H 0.8220 0.8129 1.0376 0.114 Uiso 1 1 calc R U . . .
C221 C 0.8452(11) 0.9202(9) 0.9823(8) 0.233(7) Uani 1 1 d D . . . .
H22A H 0.9001 0.8954 0.9522 0.350 Uiso 1 1 calc R U . . .
H22B H 0.8737 0.9502 1.0266 0.350 Uiso 1 1 calc R U . . .
H22C H 0.8067 0.9642 0.9525 0.350 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Ni1 2.120(3) 3_667 ?
O7 C24 1.257(5) . ?
Tm1 Ni1 3.3845(10) . ?
Tm1 O1 2.491(3) . ?
Tm1 O5 2.463(3) . ?
Tm1 O4 2.277(3) . ?
Tm1 O2 2.255(3) . ?
Tm1 O8 2.409(3) . ?
Tm1 C24 2.800(4) . ?
Tm1 O6 2.296(3) . ?
Tm1 O6 2.320(3) 3_667 ?
Tm1 O9 2.199(3) . ?
Ni1 O7 2.120(3) 3_667 ?
Ni1 O4 2.031(3) . ?
Ni1 O2 2.035(3) . ?
Ni1 N1 2.029(4) . ?
Ni1 N2 2.049(4) . ?
Ni1 O11 2.126(3) . ?
O1 C3 1.388(6) . ?
O1 C1 1.451(6) . ?
O5 C17 1.406(6) . ?
O5 C19 1.464(6) . ?
C17 C18 1.405(7) . ?
C17 C16 1.365(7) . ?
O4 C18 1.311(5) . ?
O2 C2 1.335(5) . ?
O8 C24 1.283(5) . ?
C2 C3 1.402(7) . ?
C2 C7 1.427(7) . ?
N1 C8 1.303(7) . ?
N1 C9 1.490(7) . ?
N2 C12 1.282(6) . ?
N2 C11 1.463(6) . ?
C24 O6 1.310(5) . ?
O6 Tm1 2.320(3) 3_667 ?
C18 C13 1.416(6) . ?
C8 C7 1.457(7) . ?
C13 C14 1.412(7) . ?
C13 C12 1.433(7) . ?
C3 C4 1.381(7) . ?
C14 C15 1.354(8) . ?
C10 O3 1.438(7) . ?
C10 C11 1.518(7) . ?
C10 C9 1.512(9) . ?
C6 C7 1.398(7) . ?
C6 C5 1.362(7) . ?
C15 C16 1.404(8) . ?
O11 C20 1.428(8) . ?
O9 C22 1.275(6) . ?
C5 C4 1.377(7) . ?
O10 C22 1.219(6) . ?
C22 C23 1.479(7) . ?
C20 C221 1.294(9) . ?

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
C24 O7 Ni1 123.8(3) . 3_667 ?
O1 Tm1 Ni1 100.85(8) . . ?
O1 Tm1 C24 80.40(12) . . ?
O5 Tm1 Ni1 100.96(8) . . ?
O5 Tm1 O1 158.19(12) . . ?
O5 Tm1 C24 79.89(12) . . ?
O4 Tm1 Ni1 35.71(7) . . ?
O4 Tm1 O1 135.65(11) . . ?
O4 Tm1 O5 65.94(10) . . ?
O4 Tm1 O8 144.45(12) . . ?
O4 Tm1 C24 141.30(12) . . ?
O4 Tm1 O6 124.92(12) . . ?
O4 Tm1 O6 74.00(11) . 3_667 ?
O2 Tm1 Ni1 35.68(8) . . ?
O2 Tm1 O1 65.37(11) . . ?
O2 Tm1 O5 136.37(11) . . ?
O2 Tm1 O4 70.46(11) . . ?
O2 Tm1 O8 143.52(12) . . ?
O2 Tm1 C24 139.67(12) . . ?
O2 Tm1 O6 75.24(12) . 3_667 ?
O2 Tm1 O6 123.10(12) . . ?
O8 Tm1 Ni1 178.09(7) . . ?
O8 Tm1 O1 78.58(12) . . ?
O8 Tm1 O5 79.63(11) . . ?
O8 Tm1 C24 27.22(11) . . ?
C24 Tm1 Ni1 154.62(9) . . ?
O6 Tm1 Ni1 64.87(8) 3_667 . ?
O6 Tm1 Ni1 127.03(8) . . ?
O6 Tm1 O1 84.22(12) . . ?
O6 Tm1 O1 97.93(12) 3_667 . ?
O6 Tm1 O5 91.25(13) 3_667 . ?
O6 Tm1 O5 82.64(12) . . ?
O6 Tm1 O8 54.81(10) . . ?
O6 Tm1 O8 116.98(10) 3_667 . ?
O6 Tm1 C24 89.78(12) 3_667 . ?
O6 Tm1 C24 27.59(12) . . ?
O6 Tm1 O6 62.21(14) . 3_667 ?
O9 Tm1 Ni1 93.38(9) . . ?
O9 Tm1 O1 94.94(10) . . ?
O9 Tm1 O5 83.84(11) . . ?
O9 Tm1 O4 83.00(11) . . ?
O9 Tm1 O2 92.52(12) . . ?
O9 Tm1 O8 84.86(12) . . ?
O9 Tm1 C24 111.85(13) . . ?
O9 Tm1 O6 156.44(13) . 3_667 ?
O9 Tm1 O6 139.12(12) . . ?
O7 Ni1 Tm1 85.70(9) 3_667 . ?
O7 Ni1 O11 177.71(15) 3_667 . ?
O4 Ni1 O7 91.66(13) . 3_667 ?
O4 Ni1 Tm1 40.88(8) . . ?
O4 Ni1 O2 80.04(12) . . ?
O4 Ni1 N2 90.11(14) . . ?
O4 Ni1 O11 86.85(13) . . ?
O2 Ni1 O7 93.00(13) . 3_667 ?
O2 Ni1 Tm1 40.28(9) . . ?
O2 Ni1 N2 169.95(14) . . ?
O2 Ni1 O11 88.46(13) . . ?
N1 Ni1 O7 88.02(15) . 3_667 ?
N1 Ni1 Tm1 130.70(12) . . ?
N1 Ni1 O4 171.53(15) . . ?
N1 Ni1 O2 91.53(15) . . ?
N1 Ni1 N2 98.35(17) . . ?
N1 Ni1 O11 93.71(15) . . ?
N2 Ni1 O7 89.22(14) . 3_667 ?
N2 Ni1 Tm1 130.34(12) . . ?
N2 Ni1 O11 89.04(15) . . ?
O11 Ni1 Tm1 94.30(10) . . ?
C3 O1 Tm1 116.5(3) . . ?
C3 O1 C1 115.6(4) . . ?
C1 O1 Tm1 127.5(3) . . ?
C17 O5 Tm1 116.8(3) . . ?
C17 O5 C19 116.1(4) . . ?
C19 O5 Tm1 127.1(3) . . ?
C18 C17 O5 112.3(4) . . ?
C16 C17 O5 124.9(5) . . ?
C16 C17 C18 122.9(5) . . ?
Ni1 O4 Tm1 103.41(12) . . ?
C18 O4 Tm1 123.2(3) . . ?
C18 O4 Ni1 127.0(3) . . ?
Ni1 O2 Tm1 104.04(13) . . ?
C2 O2 Tm1 124.2(3) . . ?
C2 O2 Ni1 127.3(3) . . ?
C24 O8 Tm1 93.6(2) . . ?
O2 C2 C3 117.9(4) . . ?
O2 C2 C7 123.3(4) . . ?
C3 C2 C7 118.8(4) . . ?
C8 N1 Ni1 124.7(3) . . ?
C8 N1 C9 113.5(5) . . ?
C9 N1 Ni1 121.7(4) . . ?
C12 N2 Ni1 123.9(3) . . ?
C12 N2 C11 117.7(4) . . ?
C11 N2 Ni1 118.3(3) . . ?
O7 C24 Tm1 175.8(3) . . ?
O7 C24 O8 125.0(4) . . ?
O7 C24 O6 121.6(4) . . ?
O8 C24 Tm1 59.2(2) . . ?
O8 C24 O6 113.5(4) . . ?
O6 C24 Tm1 54.3(2) . . ?
Tm1 O6 Tm1 117.79(14) . 3_667 ?
C24 O6 Tm1 144.0(3) . 3_667 ?
C24 O6 Tm1 98.1(2) . . ?
C17 C18 C13 117.1(4) . . ?
O4 C18 C17 119.3(4) . . ?
O4 C18 C13 123.5(4) . . ?
N1 C8 C7 127.5(4) . . ?
C18 C13 C12 123.8(4) . . ?
C14 C13 C18 118.6(5) . . ?
C14 C13 C12 117.6(5) . . ?
O1 C3 C2 113.0(4) . . ?
C4 C3 O1 125.6(5) . . ?
C4 C3 C2 121.4(5) . . ?
C15 C14 C13 122.7(5) . . ?
O3 C10 C11 113.5(5) . . ?
O3 C10 C9 109.8(5) . . ?
C9 C10 C11 114.9(5) . . ?
C5 C6 C7 121.6(5) . . ?
C14 C15 C16 118.8(5) . . ?
C2 C7 C8 124.8(4) . . ?
C6 C7 C2 117.7(5) . . ?
C6 C7 C8 117.5(5) . . ?
C17 C16 C15 119.8(5) . . ?
C20 O11 Ni1 123.8(4) . . ?
N2 C12 C13 128.8(4) . . ?
C22 O9 Tm1 141.1(3) . . ?
C6 C5 C4 121.4(5) . . ?
C5 C4 C3 118.9(5) . . ?
N2 C11 C10 112.4(4) . . ?
N1 C9 C10 113.4(5) . . ?
O9 C22 C23 115.6(5) . . ?
O10 C22 O9 126.4(5) . . ?
O10 C22 C23 118.0(5) . . ?
C221 C20 O11 111.3(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 C24 O6 Tm1 2.9(9) . . . 3_667 ?
O7 C24 O6 Tm1 179.2(4) . . . . ?
Tm1 O1 C3 C2 10.4(4) . . . . ?
Tm1 O1 C3 C4 -170.3(4) . . . . ?
Tm1 O5 C17 C18 -9.5(4) . . . . ?
Tm1 O5 C17 C16 171.3(4) . . . . ?
Tm1 O4 C18 C17 15.1(5) . . . . ?
Tm1 O4 C18 C13 -165.8(3) . . . . ?
Tm1 O2 C2 C3 -16.7(5) . . . . ?
Tm1 O2 C2 C7 162.7(3) . . . . ?
Tm1 O8 C24 O7 -179.2(4) . . . . ?
Tm1 O8 C24 O6 0.4(4) . . . . ?
Tm1 C24 O6 Tm1 -176.3(6) . . . 3_667 ?
Tm1 O9 C22 O10 -52.0(9) . . . . ?
Tm1 O9 C22 C23 128.7(6) . . . . ?
Ni1 O7 C24 O8 177.4(3) 3_667 . . . ?
Ni1 O7 C24 O6 -2.2(6) 3_667 . . . ?
Ni1 O4 C18 C17 162.3(3) . . . . ?
Ni1 O4 C18 C13 -18.5(6) . . . . ?
Ni1 O2 C2 C3 -169.2(3) . . . . ?
Ni1 O2 C2 C7 10.3(5) . . . . ?
Ni1 N1 C8 C7 -4.0(7) . . . . ?
Ni1 N1 C9 C10 -27.7(7) . . . . ?
Ni1 N2 C12 C13 -2.3(7) . . . . ?
Ni1 N2 C11 C10 43.8(6) . . . . ?
Ni1 O11 C20 C221 133.4(9) . . . . ?
O1 C3 C4 C5 178.8(4) . . . . ?
O5 C17 C18 O4 -2.4(5) . . . . ?
O5 C17 C18 C13 178.4(3) . . . . ?
O5 C17 C16 C15 -179.4(4) . . . . ?
C17 C18 C13 C14 2.6(6) . . . . ?
C17 C18 C13 C12 -177.7(4) . . . . ?
O4 C18 C13 C14 -176.6(4) . . . . ?
O4 C18 C13 C12 3.1(7) . . . . ?
O2 C2 C3 O1 2.5(5) . . . . ?
O2 C2 C3 C4 -176.9(4) . . . . ?
O2 C2 C7 C8 -2.8(7) . . . . ?
O2 C2 C7 C6 178.4(4) . . . . ?
O8 C24 O6 Tm1 -176.7(4) . . . 3_667 ?
O8 C24 O6 Tm1 -0.4(4) . . . . ?
C2 C3 C4 C5 -1.9(7) . . . . ?
N1 C8 C7 C2 -0.4(8) . . . . ?
N1 C8 C7 C6 178.4(5) . . . . ?
C18 C17 C16 C15 1.4(7) . . . . ?
C18 C13 C14 C15 -2.1(8) . . . . ?
C18 C13 C12 N2 8.2(8) . . . . ?
C8 N1 C9 C10 149.4(5) . . . . ?
C13 C14 C15 C16 1.1(9) . . . . ?
C3 C2 C7 C8 176.6(4) . . . . ?
C3 C2 C7 C6 -2.2(6) . . . . ?
C14 C13 C12 N2 -172.1(5) . . . . ?
C14 C15 C16 C17 -0.7(8) . . . . ?
C6 C5 C4 C3 -1.4(8) . . . . ?
C7 C2 C3 O1 -177.0(3) . . . . ?
C7 C2 C3 C4 3.6(6) . . . . ?
C7 C6 C5 C4 2.8(9) . . . . ?
C1 O1 C3 C2 -176.0(4) . . . . ?
C1 O1 C3 C4 3.4(6) . . . . ?
C16 C17 C18 O4 176.8(4) . . . . ?
C16 C17 C18 C13 -2.4(6) . . . . ?
C19 O5 C17 C18 170.7(4) . . . . ?
C19 O5 C17 C16 -8.5(6) . . . . ?
C12 N2 C11 C10 -138.2(5) . . . . ?
C12 C13 C14 C15 178.2(5) . . . . ?
C5 C6 C7 C2 -1.0(7) . . . . ?
C5 C6 C7 C8 -179.8(5) . . . . ?
O3 C10 C11 N2 50.2(7) . . . . ?
O3 C10 C9 N1 -62.4(6) . . . . ?
C11 N2 C12 C13 179.9(5) . . . . ?
C11 C10 C9 N1 66.9(7) . . . . ?
C9 N1 C8 C7 178.9(5) . . . . ?
C9 C10 C11 N2 -77.3(6) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_p160411y_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 1484049'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H57 Cl4 N2 Ni O11 Tb'
_chemical_formula_weight         1413.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2890(4)
_cell_length_b                   12.7006(4)
_cell_length_c                   23.3948(8)
_cell_angle_alpha                82.054(3)
_cell_angle_beta                 83.489(3)
_cell_angle_gamma                76.859(3)
_cell_volume                     3223.38(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    127.60(10)
_cell_measurement_reflns_used    9543
_cell_measurement_theta_min      3.3620
_cell_measurement_theta_max      28.7670
_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    1.605
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1
_exptl_absorpt_correction_T_max  0.5
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      127.60(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24297
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.873
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_full        25.008
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11365
_reflns_number_gt                9790
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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.
;
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0283P)²+0.4541P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11365
_refine_ls_number_parameters     779
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.72627(2) 0.78609(2) 0.21995(2) 0.01398(7) Uani 1 1 d . . . . .
Ni1 Ni 0.58348(4) 0.70896(4) 0.34457(2) 0.01707(13) Uani 1 1 d . . . . .
O11 O 0.9251(2) 0.6950(2) 0.21494(11) 0.0165(6) Uani 1 1 d . . . . .
O3 O 0.3491(3) 0.6525(3) 0.45659(13) 0.0383(9) Uani 1 1 d . . . . .
H3 H 0.3700 0.6335 0.4242 0.057 Uiso 1 1 calc R U . . .
O5 O 0.8742(2) 0.8870(2) 0.26289(11) 0.0181(6) Uani 1 1 d . . . . .
O4 O 0.7148(2) 0.7969(2) 0.32147(11) 0.0172(6) Uani 1 1 d . . . . .
O10 O 0.7392(2) 0.6509(2) 0.16151(11) 0.0177(6) Uani 1 1 d . . . . .
O9 O 0.7942(2) 0.8663(2) 0.13157(11) 0.0181(6) Uani 1 1 d . . . . .
O1 O 0.5233(2) 0.8415(2) 0.15877(11) 0.0196(6) Uani 1 1 d . . . . .
O2 O 0.5339(2) 0.7775(2) 0.26563(11) 0.0155(6) Uani 1 1 d . . . . .
O6 O 0.7083(2) 0.6038(2) 0.29736(11) 0.0188(6) Uani 1 1 d . . . . .
O7 O 0.4691(2) 0.6028(2) 0.35375(12) 0.0220(7) Uani 1 1 d . . . . .
O8 O 0.6441(2) 0.9719(2) 0.21695(11) 0.0161(6) Uani 1 1 d . . . . .
N2 N 0.6500(3) 0.6608(3) 0.42295(14) 0.0225(8) Uani 1 1 d . . . . .
N1 N 0.4441(3) 0.8180(3) 0.38250(14) 0.0222(8) Uani 1 1 d . . . . .
C25 C 0.9302(5) 0.2944(4) 0.2115(2) 0.0393(13) Uani 1 1 d . . . . .
H25 H 0.9295 0.2399 0.1888 0.047 Uiso 1 1 calc R U . . .
C43 C 0.7716(3) 0.9579(3) 0.10214(17) 0.0155(9) Uani 1 1 d . . . . .
C44 C 0.8180(3) 0.9617(3) 0.03903(17) 0.0160(9) Uani 1 1 d . . . . .
C35 C 0.6413(3) 1.0545(3) 0.17951(16) 0.0137(9) Uani 1 1 d . . . . .
C45 C 0.8271(4) 1.0581(3) 0.00383(17) 0.0227(10) Uani 1 1 d . . . . .
H45 H 0.8028 1.1241 0.0193 0.027 Uiso 1 1 calc R U . . .
C16 C 1.0201(4) 0.8237(4) 0.33688(18) 0.0260(10) Uani 1 1 d . . . . .
H16 H 1.0789 0.8575 0.3157 0.031 Uiso 1 1 calc R U . . .
C52 C 0.8758(4) 0.4445(4) 0.0657(2) 0.0310(12) Uani 1 1 d . . . . .
H52 H 0.9587 0.4363 0.0692 0.037 Uiso 1 1 calc R U . . .
C37 C 0.5815(4) 1.2609(3) 0.17201(18) 0.0209(10) Uani 1 1 d . . . . .
H37 H 0.6489 1.2657 0.1457 0.025 Uiso 1 1 calc R U . . .
C19 C 0.9589(4) 0.9417(4) 0.22798(18) 0.0268(11) Uani 1 1 d . . . . .
H19A H 1.0307 0.8893 0.2168 0.040 Uiso 1 1 calc R U . . .
H19B H 0.9810 0.9922 0.2496 0.040 Uiso 1 1 calc R U . . .
H19C H 0.9222 0.9803 0.1939 0.040 Uiso 1 1 calc R U . . .
C57 C 0.9500(3) 0.5975(3) 0.13332(17) 0.0191(9) Uani 1 1 d . . . . .
H57 H 1.0064 0.5651 0.1053 0.023 Uiso 1 1 calc R U . . .
C42 C 0.7019(3) 1.0526(3) 0.12352(17) 0.0174(9) Uani 1 1 d . . . . .
H42 H 0.6953 1.1179 0.0994 0.021 Uiso 1 1 calc R U . . .
C8 C 0.3588(4) 0.8826(3) 0.35601(18) 0.0228(10) Uani 1 1 d . . . . .
H8 H 0.2951 0.9202 0.3792 0.027 Uiso 1 1 calc R U . . .
C31 C 0.1937(5) 0.4295(6) 0.3909(2) 0.0595(19) Uani 1 1 d . . . . .
H31 H 0.1119 0.4646 0.3950 0.071 Uiso 1 1 calc R U . . .
C38 C 0.5025(4) 1.3553(4) 0.18759(18) 0.0257(10) Uani 1 1 d . . . . .
H38 H 0.5177 1.4229 0.1721 0.031 Uiso 1 1 calc R U . . .
C50 C 0.8272(3) 0.5950(3) 0.13171(16) 0.0158(9) Uani 1 1 d . . . . .
C29 C 0.4049(4) 0.4371(4) 0.36409(18) 0.0304(12) Uani 1 1 d . . . . .
C34 C 0.4363(5) 0.3252(4) 0.37863(19) 0.0406(14) Uani 1 1 d . . . . .
H34 H 0.5174 0.2885 0.3742 0.049 Uiso 1 1 calc R U . . .
C32 C 0.2265(6) 0.3185(6) 0.4053(2) 0.066(2) Uani 1 1 d . . . . .
H32 H 0.1671 0.2786 0.4186 0.079 Uiso 1 1 calc R U . . .
C30 C 0.2820(4) 0.4900(5) 0.37027(19) 0.0422(14) Uani 1 1 d . . . . .
H30 H 0.2592 0.5649 0.3607 0.051 Uiso 1 1 calc R U . . .
C10 C 0.4415(4) 0.6957(4) 0.47482(19) 0.0321(12) Uani 1 1 d . . . . .
H10 H 0.4214 0.7011 0.5163 0.038 Uiso 1 1 calc R U . . .
C23 C 1.0408(4) 0.3972(4) 0.2555(2) 0.0322(11) Uani 1 1 d . . . . .
H23 H 1.1149 0.4107 0.2630 0.039 Uiso 1 1 calc R U . . .
C59 C 1.1267(3) 0.6417(3) 0.17603(17) 0.0170(9) Uani 1 1 d . . . . .
C33 C 0.3454(7) 0.2680(5) 0.3999(2) 0.064(2) Uani 1 1 d . . . . .
H33 H 0.3674 0.1933 0.4106 0.077 Uiso 1 1 calc R U . . .
C58 C 0.9929(3) 0.6461(3) 0.17488(17) 0.0170(9) Uani 1 1 d . . . . .
C11 C 0.5689(4) 0.6182(4) 0.46917(18) 0.0315(11) Uani 1 1 d . . . . .
H11A H 0.6057 0.6080 0.5056 0.038 Uiso 1 1 calc R U . . .
H11B H 0.5594 0.5477 0.4612 0.038 Uiso 1 1 calc R U . . .
C12 C 0.7525(4) 0.6723(4) 0.43671(19) 0.0285(11) Uani 1 1 d . . . . .
H12 H 0.7714 0.6460 0.4744 0.034 Uiso 1 1 calc R U . . .
C13 C 0.8430(4) 0.7219(4) 0.39998(18) 0.0257(10) Uani 1 1 d . . . . .
C18 C 0.8183(4) 0.7821(3) 0.34613(17) 0.0185(9) Uani 1 1 d . . . . .
C17 C 0.9107(4) 0.8313(3) 0.31538(17) 0.0187(9) Uani 1 1 d . . . . .
C14 C 0.9564(4) 0.7154(4) 0.42163(19) 0.0345(12) Uani 1 1 d . . . . .
H14 H 0.9724 0.6764 0.4576 0.041 Uiso 1 1 calc R U . . .
C15 C 1.0432(4) 0.7648(4) 0.3911(2) 0.0361(12) Uani 1 1 d . . . . .
H15 H 1.1174 0.7594 0.4062 0.043 Uiso 1 1 calc R U . . .
C49 C 0.8540(3) 0.8645(3) 0.01464(17) 0.0211(10) Uani 1 1 d . . . . .
H49 H 0.8486 0.7993 0.0373 0.025 Uiso 1 1 calc R U . . .
C48 C 0.8981(4) 0.8636(4) -0.04316(18) 0.0251(10) Uani 1 1 d . . . . .
H48 H 0.9210 0.7979 -0.0590 0.030 Uiso 1 1 calc R U . . .
C47 C 0.9080(4) 0.9592(4) -0.07728(18) 0.0272(11) Uani 1 1 d . . . . .
H47 H 0.9390 0.9580 -0.1158 0.033 Uiso 1 1 calc R U . . .
C46 C 0.8718(4) 1.0569(4) -0.05389(19) 0.0305(11) Uani 1 1 d . . . . .
H46 H 0.8774 1.1218 -0.0768 0.037 Uiso 1 1 calc R U . . .
C3 C 0.4247(3) 0.8914(3) 0.19348(18) 0.0191(9) Uani 1 1 d . . . . .
C2 C 0.4376(3) 0.8542(3) 0.25290(18) 0.0171(9) Uani 1 1 d . . . . .
C7 C 0.3490(3) 0.9046(3) 0.29383(18) 0.0203(9) Uani 1 1 d . . . . .
C6 C 0.2489(4) 0.9849(3) 0.2741(2) 0.0237(10) Uani 1 1 d . . . . .
H6 H 0.1898 1.0182 0.3008 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2377(4) 1.0143(3) 0.2159(2) 0.0250(10) Uani 1 1 d . . . . .
H5 H 0.1702 1.0662 0.2038 0.030 Uiso 1 1 calc R U . . .
C4 C 0.3265(4) 0.9675(3) 0.17442(19) 0.0237(10) Uani 1 1 d . . . . .
H4 H 0.3187 0.9877 0.1350 0.028 Uiso 1 1 calc R U . . .
C1 C 0.5171(4) 0.8624(4) 0.09755(17) 0.0296(11) Uani 1 1 d . . . . .
H1A H 0.5121 0.9385 0.0855 0.044 Uiso 1 1 calc R U . . .
H1B H 0.4462 0.8419 0.0874 0.044 Uiso 1 1 calc R U . . .
H1C H 0.5890 0.8209 0.0786 0.044 Uiso 1 1 calc R U . . .
C22 C 0.9325(4) 0.4590(3) 0.27738(18) 0.0240(10) Uani 1 1 d . . . . .
H22 H 0.9338 0.5150 0.2990 0.029 Uiso 1 1 calc R U . . .
C21 C 0.8209(4) 0.4380(3) 0.26720(18) 0.0220(10) Uani 1 1 d . . . . .
C20 C 0.7063(4) 0.5056(3) 0.29290(17) 0.0192(9) Uani 1 1 d . . . . .
C27 C 0.6080(4) 0.4552(3) 0.31305(17) 0.0230(10) Uani 1 1 d . . . . .
H27 H 0.6166 0.3834 0.3060 0.028 Uiso 1 1 calc R U . . .
C28 C 0.4985(4) 0.5034(4) 0.34277(17) 0.0233(10) Uani 1 1 d . . . . .
C26 C 0.8210(4) 0.3549(4) 0.23421(19) 0.0319(11) Uani 1 1 d . . . . .
H26 H 0.7474 0.3397 0.2273 0.038 Uiso 1 1 calc R U . . .
C53 C 0.8373(4) 0.3778(4) 0.0329(2) 0.0346(12) Uani 1 1 d . . . . .
H53 H 0.8945 0.3259 0.0142 0.042 Uiso 1 1 calc R U . . .
C54 C 0.7143(4) 0.3881(4) 0.02791(18) 0.0262(10) Uani 1 1 d . . . . .
H54 H 0.6884 0.3417 0.0069 0.031 Uiso 1 1 calc R U . . .
C55 C 0.6303(4) 0.4671(4) 0.05413(18) 0.0268(11) Uani 1 1 d . . . . .
H55 H 0.5476 0.4757 0.0499 0.032 Uiso 1 1 calc R U . . .
C56 C 0.6691(4) 0.5342(4) 0.08698(18) 0.0236(10) Uani 1 1 d . . . . .
H56 H 0.6118 0.5871 0.1049 0.028 Uiso 1 1 calc R U . . .
C51 C 0.7925(3) 0.5231(3) 0.09335(17) 0.0177(9) Uani 1 1 d . . . . .
C9 C 0.4357(4) 0.8114(4) 0.44614(18) 0.0303(11) Uani 1 1 d . . . . .
H9A H 0.3596 0.8576 0.4595 0.036 Uiso 1 1 calc R U . . .
H9B H 0.5022 0.8384 0.4576 0.036 Uiso 1 1 calc R U . . .
C39 C 0.4012(4) 1.3490(3) 0.22616(18) 0.0248(10) Uani 1 1 d . . . . .
H39 H 0.3480 1.4121 0.2365 0.030 Uiso 1 1 calc R U . . .
C40 C 0.3797(4) 1.2484(3) 0.24916(18) 0.0226(10) Uani 1 1 d . . . . .
H40 H 0.3109 1.2441 0.2746 0.027 Uiso 1 1 calc R U . . .
C41 C 0.4595(3) 1.1539(3) 0.23474(17) 0.0193(9) Uani 1 1 d . . . . .
H41 H 0.4455 1.0865 0.2514 0.023 Uiso 1 1 calc R U . . .
C36 C 0.5610(3) 1.1596(3) 0.19520(17) 0.0162(9) Uani 1 1 d . . . . .
C64 C 1.2089(3) 0.6284(3) 0.12738(17) 0.0198(9) Uani 1 1 d . . . . .
H64 H 1.1823 0.6178 0.0928 0.024 Uiso 1 1 calc R U . . .
C63 C 1.3302(4) 0.6308(3) 0.12990(19) 0.0237(10) Uani 1 1 d . . . . .
H63 H 1.3841 0.6233 0.0968 0.028 Uiso 1 1 calc R U . . .
C62 C 1.3720(4) 0.6443(3) 0.18118(18) 0.0201(9) Uani 1 1 d . . . . .
H62 H 1.4535 0.6459 0.1826 0.024 Uiso 1 1 calc R U . . .
C61 C 1.2915(4) 0.6554(3) 0.23035(18) 0.0209(10) Uani 1 1 d . . . . .
H61 H 1.3192 0.6635 0.2651 0.025 Uiso 1 1 calc R U . . .
C60 C 1.1705(4) 0.6543(3) 0.22787(17) 0.0182(9) Uani 1 1 d . . . . .
H60 H 1.1170 0.6621 0.2611 0.022 Uiso 1 1 calc R U . . .
C24 C 1.0394(4) 0.3148(4) 0.2226(2) 0.0391(13) Uani 1 1 d . . . . .
H24 H 1.1125 0.2734 0.2078 0.047 Uiso 1 1 calc R U . . .
Cl4 Cl 0.54829(15) 0.78885(17) -0.03914(7) 0.0860(7) Uani 1 1 d . . . . .
Cl3 Cl 0.76444(14) 0.62970(12) -0.06832(8) 0.0675(5) Uani 1 1 d . . . . .
C66 C 0.6667(5) 0.7484(4) -0.0916(2) 0.0488(15) Uani 1 1 d . . . . .
H66A H 0.6324 0.7387 -0.1261 0.059 Uiso 1 1 calc R U . . .
H66B H 0.7123 0.8055 -0.1018 0.059 Uiso 1 1 calc R U . . .
Cl1 Cl 0.74048(16) 1.13496(13) 0.32230(7) 0.0712(5) Uani 1 1 d . . . . .
Cl2 Cl 0.6327(4) 1.0249(2) 0.42442(10) 0.0746(13) Uani 0.758(7) 1 d . . P A 1
C65 C 0.6455(5) 1.0459(4) 0.3482(2) 0.0506(15) Uani 1 1 d . . . . .
H65A H 0.6778 0.9767 0.3331 0.061 Uiso 0.758(7) 1 calc R U P A 1
H65B H 0.5651 1.0752 0.3346 0.061 Uiso 0.758(7) 1 calc R U P A 1
H65C H 0.6105 1.0339 0.3143 0.061 Uiso 0.242(7) 1 calc R U P A 2
H65D H 0.7001 0.9776 0.3602 0.061 Uiso 0.242(7) 1 calc R U P A 2
Cl1A Cl 0.5333(11) 1.0580(6) 0.3984(6) 0.104(6) Uani 0.242(7) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O11 2.277(2) . ?
Tb1 O9 2.305(3) . ?
Tb1 O10 2.308(2) . ?
Tb1 O8 2.326(3) . ?
Tb1 O2 2.328(2) . ?
Tb1 O4 2.385(2) . ?
Tb1 O5 2.674(3) . ?
Tb1 O1 2.744(3) . ?
Tb1 O6 2.766(3) . ?
Tb1 Ni1 3.3048(5) . ?
Ni1 O2 2.013(3) . ?
Ni1 N2 2.023(3) . ?
Ni1 O4 2.035(3) . ?
Ni1 O7 2.045(3) . ?
Ni1 O6 2.047(3) . ?
Ni1 N1 2.052(3) . ?
O11 C58 1.278(4) . ?
O3 C10 1.414(5) . ?
O3 H3 0.8200 . ?
O5 C17 1.386(5) . ?
O5 C19 1.425(4) . ?
O4 C18 1.325(4) . ?
O10 C50 1.280(4) . ?
O9 C43 1.255(5) . ?
O1 C3 1.384(4) . ?
O1 C1 1.427(5) . ?
O2 C2 1.316(4) . ?
O6 C20 1.272(5) . ?
O7 C28 1.284(5) . ?
O8 C35 1.267(5) . ?
N2 C12 1.280(5) . ?
N2 C11 1.462(5) . ?
N1 C8 1.273(5) . ?
N1 C9 1.473(5) . ?
C25 C24 1.375(6) . ?
C25 C26 1.387(6) . ?
C25 H25 0.9300 . ?
C43 C42 1.400(5) . ?
C43 C44 1.508(5) . ?
C44 C49 1.389(5) . ?
C44 C45 1.395(6) . ?
C35 C42 1.408(5) . ?
C35 C36 1.499(5) . ?
C45 C46 1.388(6) . ?
C45 H45 0.9300 . ?
C16 C17 1.364(5) . ?
C16 C15 1.401(6) . ?
C16 H16 0.9300 . ?
C52 C51 1.383(5) . ?
C52 C53 1.384(6) . ?
C52 H52 0.9300 . ?
C37 C36 1.384(6) . ?
C37 C38 1.388(5) . ?
C37 H37 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C57 C50 1.399(5) . ?
C57 C58 1.403(5) . ?
C57 H57 0.9300 . ?
C42 H42 0.9300 . ?
C8 C7 1.455(6) . ?
C8 H8 0.9300 . ?
C31 C32 1.378(9) . ?
C31 C30 1.399(7) . ?
C31 H31 0.9300 . ?
C38 C39 1.384(6) . ?
C38 H38 0.9300 . ?
C50 C51 1.504(5) . ?
C29 C34 1.388(7) . ?
C29 C30 1.398(7) . ?
C29 C28 1.498(6) . ?
C34 C33 1.397(7) . ?
C34 H34 0.9300 . ?
C32 C33 1.350(9) . ?
C32 H32 0.9300 . ?
C30 H30 0.9300 . ?
C10 C9 1.519(6) . ?
C10 C11 1.551(6) . ?
C10 H10 0.9800 . ?
C23 C22 1.381(6) . ?
C23 C24 1.387(6) . ?
C23 H23 0.9300 . ?
C59 C64 1.388(5) . ?
C59 C60 1.402(5) . ?
C59 C58 1.502(5) . ?
C33 H33 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.457(6) . ?
C12 H12 0.9300 . ?
C13 C18 1.402(6) . ?
C13 C14 1.410(6) . ?
C18 C17 1.413(5) . ?
C14 C15 1.365(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C49 C48 1.387(5) . ?
C49 H49 0.9300 . ?
C48 C47 1.378(6) . ?
C48 H48 0.9300 . ?
C47 C46 1.383(6) . ?
C47 H47 0.9300 . ?
C46 H46 0.9300 . ?
C3 C4 1.367(6) . ?
C3 C2 1.418(6) . ?
C2 C7 1.410(5) . ?
C7 C6 1.412(6) . ?
C6 C5 1.373(6) . ?
C6 H6 0.9300 . ?
C5 C4 1.403(5) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C22 C21 1.398(5) . ?
C22 H22 0.9300 . ?
C21 C26 1.391(5) . ?
C21 C20 1.494(5) . ?
C20 C27 1.408(5) . ?
C27 C28 1.402(6) . ?
C27 H27 0.9300 . ?
C26 H26 0.9300 . ?
C53 C54 1.382(6) . ?
C53 H53 0.9300 . ?
C54 C55 1.374(5) . ?
C54 H54 0.9300 . ?
C55 C56 1.392(5) . ?
C55 H55 0.9300 . ?
C56 C51 1.390(5) . ?
C56 H56 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C39 C40 1.378(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.385(5) . ?
C40 H40 0.9300 . ?
C41 C36 1.398(5) . ?
C41 H41 0.9300 . ?
C64 C63 1.385(5) . ?
C64 H64 0.9300 . ?
C63 C62 1.383(5) . ?
C63 H63 0.9300 . ?
C62 C61 1.385(5) . ?
C62 H62 0.9300 . ?
C61 C60 1.377(5) . ?
C61 H61 0.9300 . ?
C60 H60 0.9300 . ?
C24 H24 0.9300 . ?
Cl4 C66 1.745(5) . ?
Cl3 C66 1.714(5) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
Cl1 C65 1.736(5) . ?
Cl2 C65 1.760(5) . ?
C65 Cl1A 1.621(9) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 H65C 0.9700 . ?
C65 H65D 0.9700 . ?

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
O11 Tb1 O9 80.33(9) . . ?
O11 Tb1 O10 73.94(9) . . ?
O9 Tb1 O10 78.43(9) . . ?
O11 Tb1 O8 129.75(9) . . ?
O9 Tb1 O8 73.06(9) . . ?
O10 Tb1 O8 137.19(9) . . ?
O11 Tb1 O2 142.86(9) . . ?
O9 Tb1 O2 133.96(9) . . ?
O10 Tb1 O2 96.67(9) . . ?
O8 Tb1 O2 81.57(9) . . ?
O11 Tb1 O4 94.21(9) . . ?
O9 Tb1 O4 142.19(9) . . ?
O10 Tb1 O4 136.23(9) . . ?
O8 Tb1 O4 82.72(9) . . ?
O2 Tb1 O4 67.51(8) . . ?
O11 Tb1 O5 66.64(8) . . ?
O9 Tb1 O5 84.49(9) . . ?
O10 Tb1 O5 139.07(8) . . ?
O8 Tb1 O5 69.00(8) . . ?
O2 Tb1 O5 121.34(8) . . ?
O4 Tb1 O5 59.53(8) . . ?
O11 Tb1 O1 142.31(8) . . ?
O9 Tb1 O1 76.10(9) . . ?
O10 Tb1 O1 72.81(8) . . ?
O8 Tb1 O1 69.81(8) . . ?
O2 Tb1 O1 59.10(8) . . ?
O4 Tb1 O1 122.24(8) . . ?
O5 Tb1 O1 137.99(8) . . ?
O11 Tb1 O6 80.00(8) . . ?
O9 Tb1 O6 151.19(8) . . ?
O10 Tb1 O6 76.03(9) . . ?
O8 Tb1 O6 135.64(8) . . ?
O2 Tb1 O6 62.87(8) . . ?
O4 Tb1 O6 60.33(8) . . ?
O5 Tb1 O6 106.54(8) . . ?
O1 Tb1 O6 108.32(8) . . ?
O11 Tb1 Ni1 110.12(7) . . ?
O9 Tb1 Ni1 169.25(6) . . ?
O10 Tb1 Ni1 106.37(7) . . ?
O8 Tb1 Ni1 97.57(6) . . ?
O2 Tb1 Ni1 36.99(6) . . ?
O4 Tb1 Ni1 37.72(6) . . ?
O5 Tb1 Ni1 97.22(6) . . ?
O1 Tb1 Ni1 95.91(6) . . ?
O6 Tb1 Ni1 38.12(5) . . ?
O2 Ni1 N2 169.98(12) . . ?
O2 Ni1 O4 80.65(10) . . ?
N2 Ni1 O4 89.80(12) . . ?
O2 Ni1 O7 94.24(11) . . ?
N2 Ni1 O7 95.71(13) . . ?
O4 Ni1 O7 167.96(10) . . ?
O2 Ni1 O6 82.74(10) . . ?
N2 Ni1 O6 98.62(12) . . ?
O4 Ni1 O6 79.48(10) . . ?
O7 Ni1 O6 89.09(10) . . ?
O2 Ni1 N1 90.19(12) . . ?
N2 Ni1 N1 88.93(14) . . ?
O4 Ni1 N1 102.75(12) . . ?
O7 Ni1 N1 88.09(12) . . ?
O6 Ni1 N1 172.18(12) . . ?
O2 Ni1 Tb1 44.10(7) . . ?
N2 Ni1 Tb1 129.04(10) . . ?
O4 Ni1 Tb1 45.82(7) . . ?
O7 Ni1 Tb1 123.92(8) . . ?
O6 Ni1 Tb1 56.54(8) . . ?
N1 Ni1 Tb1 119.75(10) . . ?
C58 O11 Tb1 131.8(2) . . ?
C10 O3 H3 109.5 . . ?
C17 O5 C19 117.0(3) . . ?
C17 O5 Tb1 110.0(2) . . ?
C19 O5 Tb1 123.7(2) . . ?
C18 O4 Ni1 125.7(3) . . ?
C18 O4 Tb1 118.1(2) . . ?
Ni1 O4 Tb1 96.46(9) . . ?
C50 O10 Tb1 133.7(2) . . ?
C43 O9 Tb1 137.3(2) . . ?
C3 O1 C1 117.7(3) . . ?
C3 O1 Tb1 109.2(2) . . ?
C1 O1 Tb1 128.5(2) . . ?
C2 O2 Ni1 128.0(2) . . ?
C2 O2 Tb1 120.9(2) . . ?
Ni1 O2 Tb1 98.91(10) . . ?
C20 O6 Ni1 126.6(2) . . ?
C20 O6 Tb1 135.1(2) . . ?
Ni1 O6 Tb1 85.34(9) . . ?
C28 O7 Ni1 126.0(3) . . ?
C35 O8 Tb1 136.1(2) . . ?
C12 N2 C11 117.2(4) . . ?
C12 N2 Ni1 125.7(3) . . ?
C11 N2 Ni1 116.8(3) . . ?
C8 N1 C9 118.0(3) . . ?
C8 N1 Ni1 125.1(3) . . ?
C9 N1 Ni1 116.6(3) . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
O9 C43 C42 124.3(4) . . ?
O9 C43 C44 116.1(3) . . ?
C42 C43 C44 119.5(4) . . ?
C49 C44 C45 118.2(4) . . ?
C49 C44 C43 118.5(4) . . ?
C45 C44 C43 123.3(3) . . ?
O8 C35 C42 124.6(3) . . ?
O8 C35 C36 117.0(3) . . ?
C42 C35 C36 118.3(4) . . ?
C46 C45 C44 121.0(4) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C51 C52 C53 120.9(4) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 H52 119.6 . . ?
C36 C37 C38 120.7(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C50 C57 C58 123.7(3) . . ?
C50 C57 H57 118.2 . . ?
C58 C57 H57 118.2 . . ?
C43 C42 C35 123.7(4) . . ?
C43 C42 H42 118.1 . . ?
C35 C42 H42 118.1 . . ?
N1 C8 C7 127.7(4) . . ?
N1 C8 H8 116.1 . . ?
C7 C8 H8 116.1 . . ?
C32 C31 C30 120.7(6) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C39 C38 C37 120.1(4) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
O10 C50 C57 124.0(3) . . ?
O10 C50 C51 116.1(3) . . ?
C57 C50 C51 119.9(3) . . ?
C34 C29 C30 119.0(4) . . ?
C34 C29 C28 122.2(4) . . ?
C30 C29 C28 118.9(5) . . ?
C29 C34 C33 119.7(6) . . ?
C29 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C33 C32 C31 119.5(5) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C29 C30 C31 119.6(6) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
O3 C10 C9 110.3(4) . . ?
O3 C10 C11 112.4(4) . . ?
C9 C10 C11 115.2(4) . . ?
O3 C10 H10 106.1 . . ?
C9 C10 H10 106.1 . . ?
C11 C10 H10 106.1 . . ?
C22 C23 C24 120.1(4) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C64 C59 C60 118.3(4) . . ?
C64 C59 C58 122.7(4) . . ?
C60 C59 C58 119.0(3) . . ?
C32 C33 C34 121.5(6) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
O11 C58 C57 124.5(3) . . ?
O11 C58 C59 114.3(3) . . ?
C57 C58 C59 121.2(3) . . ?
N2 C11 C10 111.9(4) . . ?
N2 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N2 C12 C13 127.4(4) . . ?
N2 C12 H12 116.3 . . ?
C13 C12 H12 116.3 . . ?
C18 C13 C14 119.1(4) . . ?
C18 C13 C12 122.5(4) . . ?
C14 C13 C12 118.2(4) . . ?
O4 C18 C13 125.2(4) . . ?
O4 C18 C17 117.0(4) . . ?
C13 C18 C17 117.8(4) . . ?
C16 C17 O5 126.2(4) . . ?
C16 C17 C18 122.3(4) . . ?
O5 C17 C18 111.5(3) . . ?
C15 C14 C13 121.7(4) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 119.7(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C48 C49 C44 120.7(4) . . ?
C48 C49 H49 119.6 . . ?
C44 C49 H49 119.6 . . ?
C47 C48 C49 120.5(4) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C48 C47 C46 119.6(4) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C47 C46 C45 120.0(4) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C4 C3 O1 125.7(4) . . ?
C4 C3 C2 122.9(4) . . ?
O1 C3 C2 111.4(3) . . ?
O2 C2 C7 125.0(4) . . ?
O2 C2 C3 117.2(3) . . ?
C7 C2 C3 117.7(4) . . ?
C2 C7 C6 119.1(4) . . ?
C2 C7 C8 123.1(4) . . ?
C6 C7 C8 117.7(4) . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C5 C4 121.1(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C3 C4 C5 118.1(4) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C23 C22 C21 120.3(4) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C26 C21 C22 118.9(4) . . ?
C26 C21 C20 122.9(4) . . ?
C22 C21 C20 118.3(4) . . ?
O6 C20 C27 125.2(4) . . ?
O6 C20 C21 116.4(4) . . ?
C27 C20 C21 118.3(4) . . ?
C28 C27 C20 125.9(4) . . ?
C28 C27 H27 117.0 . . ?
C20 C27 H27 117.0 . . ?
O7 C28 C27 125.4(4) . . ?
O7 C28 C29 115.1(4) . . ?
C27 C28 C29 119.6(4) . . ?
C25 C26 C21 120.5(4) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C54 C53 C52 120.2(4) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C55 C54 C53 119.8(4) . . ?
C55 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C54 C55 C56 119.9(4) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C51 C56 C55 120.8(4) . . ?
C51 C56 H56 119.6 . . ?
C55 C56 H56 119.6 . . ?
C52 C51 C56 118.4(4) . . ?
C52 C51 C50 123.8(4) . . ?
C56 C51 C50 117.8(3) . . ?
N1 C9 C10 112.0(3) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C40 C39 C38 119.6(4) . . ?
C40 C39 H39 120.2 . . ?
C38 C39 H39 120.2 . . ?
C39 C40 C41 120.6(4) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C36 120.2(4) . . ?
C40 C41 H41 119.9 . . ?
C36 C41 H41 119.9 . . ?
C37 C36 C41 118.8(4) . . ?
C37 C36 C35 123.4(3) . . ?
C41 C36 C35 117.7(4) . . ?
C63 C64 C59 120.5(4) . . ?
C63 C64 H64 119.8 . . ?
C59 C64 H64 119.8 . . ?
C62 C63 C64 120.6(4) . . ?
C62 C63 H63 119.7 . . ?
C64 C63 H63 119.7 . . ?
C63 C62 C61 119.5(4) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C60 C61 C62 120.1(4) . . ?
C60 C61 H61 120.0 . . ?
C62 C61 H61 120.0 . . ?
C61 C60 C59 121.0(4) . . ?
C61 C60 H60 119.5 . . ?
C59 C60 H60 119.5 . . ?
C25 C24 C23 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
Cl3 C66 Cl4 112.4(3) . . ?
Cl3 C66 H66A 109.1 . . ?
Cl4 C66 H66A 109.1 . . ?
Cl3 C66 H66B 109.1 . . ?
Cl4 C66 H66B 109.1 . . ?
H66A C66 H66B 107.8 . . ?
Cl1A C65 Cl1 129.3(4) . . ?
Cl1 C65 Cl2 111.3(3) . . ?
Cl1 C65 H65A 109.4 . . ?
Cl2 C65 H65A 109.4 . . ?
Cl1 C65 H65B 109.4 . . ?
Cl2 C65 H65B 109.4 . . ?
H65A C65 H65B 108.0 . . ?
Cl1A C65 H65C 105.0 . . ?
Cl1 C65 H65C 105.0 . . ?
Cl1A C65 H65D 105.0 . . ?
Cl1 C65 H65D 105.0 . . ?
H65C C65 H65D 105.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O9 C43 C42 12.4(6) . . . . ?
Tb1 O9 C43 C44 -164.1(2) . . . . ?
O9 C43 C44 C49 15.6(5) . . . . ?
C42 C43 C44 C49 -161.0(4) . . . . ?
O9 C43 C44 C45 -164.1(4) . . . . ?
C42 C43 C44 C45 19.2(6) . . . . ?
Tb1 O8 C35 C42 -3.9(6) . . . . ?
Tb1 O8 C35 C36 172.0(2) . . . . ?
C49 C44 C45 C46 -0.5(6) . . . . ?
C43 C44 C45 C46 179.2(4) . . . . ?
O9 C43 C42 C35 -4.9(6) . . . . ?
C44 C43 C42 C35 171.4(3) . . . . ?
O8 C35 C42 C43 1.0(6) . . . . ?
C36 C35 C42 C43 -174.8(3) . . . . ?
C9 N1 C8 C7 178.3(4) . . . . ?
Ni1 N1 C8 C7 -8.9(6) . . . . ?
C36 C37 C38 C39 -0.7(6) . . . . ?
Tb1 O10 C50 C57 7.5(6) . . . . ?
Tb1 O10 C50 C51 -172.7(2) . . . . ?
C58 C57 C50 O10 11.7(7) . . . . ?
C58 C57 C50 C51 -168.1(4) . . . . ?
C30 C29 C34 C33 -1.0(7) . . . . ?
C28 C29 C34 C33 178.1(4) . . . . ?
C30 C31 C32 C33 0.7(8) . . . . ?
C34 C29 C30 C31 0.1(7) . . . . ?
C28 C29 C30 C31 -179.1(4) . . . . ?
C32 C31 C30 C29 0.1(7) . . . . ?
C31 C32 C33 C34 -1.7(9) . . . . ?
C29 C34 C33 C32 1.9(8) . . . . ?
Tb1 O11 C58 C57 -28.3(6) . . . . ?
Tb1 O11 C58 C59 153.1(3) . . . . ?
C50 C57 C58 O11 -1.4(7) . . . . ?
C50 C57 C58 C59 177.1(4) . . . . ?
C64 C59 C58 O11 -156.7(4) . . . . ?
C60 C59 C58 O11 21.6(5) . . . . ?
C64 C59 C58 C57 24.6(6) . . . . ?
C60 C59 C58 C57 -157.1(4) . . . . ?
C12 N2 C11 C10 124.0(4) . . . . ?
Ni1 N2 C11 C10 -50.6(4) . . . . ?
O3 C10 C11 N2 110.0(4) . . . . ?
C9 C10 C11 N2 -17.5(5) . . . . ?
C11 N2 C12 C13 -173.9(4) . . . . ?
Ni1 N2 C12 C13 0.2(7) . . . . ?
N2 C12 C13 C18 11.8(7) . . . . ?
N2 C12 C13 C14 -172.9(4) . . . . ?
Ni1 O4 C18 C13 -15.7(5) . . . . ?
Tb1 O4 C18 C13 -138.4(4) . . . . ?
Ni1 O4 C18 C17 164.3(3) . . . . ?
Tb1 O4 C18 C17 41.5(4) . . . . ?
C14 C13 C18 O4 -178.4(4) . . . . ?
C12 C13 C18 O4 -3.1(7) . . . . ?
C14 C13 C18 C17 1.6(6) . . . . ?
C12 C13 C18 C17 176.9(4) . . . . ?
C15 C16 C17 O5 179.5(4) . . . . ?
C15 C16 C17 C18 0.5(6) . . . . ?
C19 O5 C17 C16 0.0(6) . . . . ?
Tb1 O5 C17 C16 147.9(3) . . . . ?
C19 O5 C17 C18 179.2(3) . . . . ?
Tb1 O5 C17 C18 -32.9(4) . . . . ?
O4 C18 C17 C16 178.6(3) . . . . ?
C13 C18 C17 C16 -1.4(6) . . . . ?
O4 C18 C17 O5 -0.6(5) . . . . ?
C13 C18 C17 O5 179.4(3) . . . . ?
C18 C13 C14 C15 -1.0(7) . . . . ?
C12 C13 C14 C15 -176.4(4) . . . . ?
C13 C14 C15 C16 0.0(7) . . . . ?
C17 C16 C15 C14 0.3(7) . . . . ?
C45 C44 C49 C48 0.1(6) . . . . ?
C43 C44 C49 C48 -179.6(3) . . . . ?
C44 C49 C48 C47 0.7(6) . . . . ?
C49 C48 C47 C46 -1.1(6) . . . . ?
C48 C47 C46 C45 0.8(6) . . . . ?
C44 C45 C46 C47 0.0(6) . . . . ?
C1 O1 C3 C4 -6.7(6) . . . . ?
Tb1 O1 C3 C4 151.2(3) . . . . ?
C1 O1 C3 C2 173.7(3) . . . . ?
Tb1 O1 C3 C2 -28.4(4) . . . . ?
Ni1 O2 C2 C7 0.5(5) . . . . ?
Tb1 O2 C2 C7 -133.6(3) . . . . ?
Ni1 O2 C2 C3 178.2(2) . . . . ?
Tb1 O2 C2 C3 44.1(4) . . . . ?
C4 C3 C2 O2 177.3(4) . . . . ?
O1 C3 C2 O2 -3.1(5) . . . . ?
C4 C3 C2 C7 -4.8(6) . . . . ?
O1 C3 C2 C7 174.8(3) . . . . ?
O2 C2 C7 C6 -179.0(4) . . . . ?
C3 C2 C7 C6 3.3(6) . . . . ?
O2 C2 C7 C8 4.7(6) . . . . ?
C3 C2 C7 C8 -173.0(4) . . . . ?
N1 C8 C7 C2 0.0(7) . . . . ?
N1 C8 C7 C6 -176.3(4) . . . . ?
C2 C7 C6 C5 -0.3(6) . . . . ?
C8 C7 C6 C5 176.2(4) . . . . ?
C7 C6 C5 C4 -1.4(6) . . . . ?
O1 C3 C4 C5 -176.4(3) . . . . ?
C2 C3 C4 C5 3.2(6) . . . . ?
C6 C5 C4 C3 0.0(6) . . . . ?
C24 C23 C22 C21 1.0(7) . . . . ?
C23 C22 C21 C26 -0.8(7) . . . . ?
C23 C22 C21 C20 178.6(4) . . . . ?
Ni1 O6 C20 C27 9.7(6) . . . . ?
Tb1 O6 C20 C27 -117.4(4) . . . . ?
Ni1 O6 C20 C21 -166.6(3) . . . . ?
Tb1 O6 C20 C21 66.3(5) . . . . ?
C26 C21 C20 O6 -147.8(4) . . . . ?
C22 C21 C20 O6 32.8(6) . . . . ?
C26 C21 C20 C27 35.6(6) . . . . ?
C22 C21 C20 C27 -143.8(4) . . . . ?
O6 C20 C27 C28 -2.2(7) . . . . ?
C21 C20 C27 C28 174.1(4) . . . . ?
Ni1 O7 C28 C27 -11.9(6) . . . . ?
Ni1 O7 C28 C29 168.4(3) . . . . ?
C20 C27 C28 O7 3.4(7) . . . . ?
C20 C27 C28 C29 -176.9(4) . . . . ?
C34 C29 C28 O7 -152.0(4) . . . . ?
C30 C29 C28 O7 27.1(6) . . . . ?
C34 C29 C28 C27 28.3(6) . . . . ?
C30 C29 C28 C27 -152.6(4) . . . . ?
C24 C25 C26 C21 1.3(8) . . . . ?
C22 C21 C26 C25 -0.4(7) . . . . ?
C20 C21 C26 C25 -179.8(4) . . . . ?
C51 C52 C53 C54 -0.8(8) . . . . ?
C52 C53 C54 C55 2.0(7) . . . . ?
C53 C54 C55 C56 -1.9(7) . . . . ?
C54 C55 C56 C51 0.5(7) . . . . ?
C53 C52 C51 C56 -0.6(7) . . . . ?
C53 C52 C51 C50 177.3(4) . . . . ?
C55 C56 C51 C52 0.7(7) . . . . ?
C55 C56 C51 C50 -177.2(4) . . . . ?
O10 C50 C51 C52 -169.0(4) . . . . ?
C57 C50 C51 C52 10.8(6) . . . . ?
O10 C50 C51 C56 8.9(5) . . . . ?
C57 C50 C51 C56 -171.3(4) . . . . ?
C8 N1 C9 C10 124.1(4) . . . . ?
Ni1 N1 C9 C10 -49.4(4) . . . . ?
O3 C10 C9 N1 -56.1(5) . . . . ?
C11 C10 C9 N1 72.5(5) . . . . ?
C37 C38 C39 C40 0.3(6) . . . . ?
C38 C39 C40 C41 1.1(6) . . . . ?
C39 C40 C41 C36 -2.0(6) . . . . ?
C38 C37 C36 C41 -0.1(6) . . . . ?
C38 C37 C36 C35 178.9(4) . . . . ?
C40 C41 C36 C37 1.5(6) . . . . ?
C40 C41 C36 C35 -177.6(3) . . . . ?
O8 C35 C36 C37 153.7(4) . . . . ?
C42 C35 C36 C37 -30.2(5) . . . . ?
O8 C35 C36 C41 -27.3(5) . . . . ?
C42 C35 C36 C41 148.9(4) . . . . ?
C60 C59 C64 C63 -1.8(6) . . . . ?
C58 C59 C64 C63 176.4(4) . . . . ?
C59 C64 C63 C62 1.3(6) . . . . ?
C64 C63 C62 C61 0.1(6) . . . . ?
C63 C62 C61 C60 -0.8(6) . . . . ?
C62 C61 C60 C59 0.3(6) . . . . ?
C64 C59 C60 C61 1.0(6) . . . . ?
C58 C59 C60 C61 -177.3(4) . . . . ?
C26 C25 C24 C23 -1.1(8) . . . . ?
C22 C23 C24 C25 -0.1(7) . . . . ?

_refine_diff_density_max         0.747
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.105



####################################################################### 
# 
# 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_nihode_sq
_database_code_depnum_ccdc_archive 'CCDC 1555628'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 Ho2 N4 Ni2 O22'
_chemical_formula_sum            'C48 H58 Ho2 N4 Ni2 O22'
_chemical_formula_weight         1490.26
_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'
Ho Ho -0.2175 4.6783 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.906(3)
_cell_length_b                   14.263(3)
_cell_length_c                   17.352(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.13(3)
_cell_angle_gamma                90
_cell_volume                     3191.9(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6562
_cell_measurement_temperature    128.35(10)
_cell_measurement_theta_max      28.9680
_cell_measurement_theta_min      3.4740
_exptl_absorpt_coefficient_mu    3.103
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11957
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.879
_diffrn_ambient_temperature      128.35(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4971
_reflns_number_total             5629
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5619
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0729
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H11a,H11b} of C11, H5 of C5, {H9a,H9b} of C9, H14 of C14, H12 of C12, H15
  of C15, H10 of C10, H16 of C16, H8 of C8, {H22a,H22b} of C22, H6 of C6, H4 of
  C4
 At 1.5 times of:
  {H23a,H23b,H23c} of C23, {H21a,H21b,H21c} of C21, H11 of O11, {H19a,H19b,
  H19c} of C19, H3 of O3, {H1a,H1b,H1c} of C1
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C22-H11
 1.916974 with sigma of 0.02
 Ni1-H11
 2.730833 with sigma of 0.02
3. Rigid bond restraints
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C11(H11a,H11b), C9(H9a,H9b)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C8(H8), C6(H6), C4(H4), C12(H12), C5(H5)
4.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C23(H23a,H23b,H23c), C21(H21a,H21b,H21c)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.2556(2) 0.4884(2) 1.07333(16) 0.0240(7) Uani 1 1 d . U . . .
Ho1 Ho 0.50549(2) 0.63903(2) 1.00696(2) 0.01526(8) Uani 1 1 d . . . . .
Ni1 Ni 0.74540(4) 0.65930(4) 0.93543(3) 0.01830(14) Uani 1 1 d D . . . .
O5 O 0.39550(19) 0.6433(2) 0.88609(15) 0.0220(7) Uani 1 1 d . . . . .
O4 O 0.59439(18) 0.6660(2) 0.89829(14) 0.0178(6) Uani 1 1 d . . . . .
O8 O 0.3334(2) 0.6280(2) 1.05940(15) 0.0206(7) Uani 1 1 d . U . . .
O2 O 0.67682(19) 0.6605(2) 1.03926(15) 0.0205(7) Uani 1 1 d . . . . .
C17 C 0.4471(3) 0.6459(3) 0.8167(2) 0.0208(10) Uani 1 1 d . . . . .
C2 C 0.7202(3) 0.6331(3) 1.1058(2) 0.0193(10) Uani 1 1 d . . . . .
N2 N 0.7894(2) 0.6673(3) 0.82384(19) 0.0218(8) Uani 1 1 d . . . . .
C18 C 0.5550(3) 0.6569(3) 0.8278(2) 0.0161(9) Uani 1 1 d . . . . .
O1 O 0.5495(2) 0.6244(2) 1.14673(14) 0.0200(7) Uani 1 1 d . . . . .
N1 N 0.8892(2) 0.6496(3) 0.9893(2) 0.0249(9) Uani 1 1 d . . . . .
C14 C 0.5651(3) 0.6513(3) 0.6887(2) 0.0261(11) Uani 1 1 d . . . . .
H14 H 0.6044 0.6536 0.6449 0.031 Uiso 1 1 calc R U . . .
O6 O 0.4127(2) 0.50257(18) 1.02221(16) 0.0220(7) Uani 1 1 d . U . . .
O11 O 0.7450(2) 0.8069(2) 0.93926(16) 0.0267(7) Uani 1 1 d D . . . .
H11 H 0.6907(18) 0.8376(14) 0.9221(17) 0.040 Uiso 1 1 d D U . . .
C15 C 0.4587(3) 0.6410(3) 0.6801(2) 0.0292(11) Uani 1 1 d . . . . .
H15 H 0.4270 0.6360 0.6313 0.035 Uiso 1 1 calc R U . . .
C10 C 0.9714(3) 0.6218(4) 0.8628(3) 0.0384(14) Uani 1 1 d . . . . .
H10 H 1.0405 0.6241 0.8413 0.046 Uiso 1 1 calc R U . . .
C19 C 0.2831(3) 0.6403(3) 0.8792(2) 0.0282(12) Uani 1 1 d . . . . .
H19A H 0.2615 0.5812 0.8575 0.042 Uiso 1 1 calc R U . . .
H19B H 0.2585 0.6902 0.8462 0.042 Uiso 1 1 calc R U . . .
H19C H 0.2549 0.6474 0.9293 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3995(3) 0.6384(3) 0.7459(2) 0.0245(11) Uani 1 1 d . . . . .
H16 H 0.3279 0.6315 0.7411 0.029 Uiso 1 1 calc R U . . .
C24 C 0.3302(3) 0.5383(3) 1.0528(2) 0.0203(9) Uani 1 1 d . U . . .
C8 C 0.9058(3) 0.6306(3) 1.0605(2) 0.0244(11) Uani 1 1 d . . . . .
H8 H 0.9746 0.6217 1.0767 0.029 Uiso 1 1 calc R U . . .
C13 C 0.6157(3) 0.6582(3) 0.7614(2) 0.0192(10) Uani 1 1 d . . . . .
C22 C 0.7822(4) 0.8584(4) 1.0067(3) 0.0401(13) Uani 1 1 d D . . . .
H22A H 0.8222 0.8170 1.0407 0.048 Uiso 1 1 calc R U . . .
H22B H 0.7237 0.8815 1.0346 0.048 Uiso 1 1 calc R U . . .
C7 C 0.8285(3) 0.6213(3) 1.1196(2) 0.0185(9) Uani 1 1 d . . . . .
O3 O 0.9396(3) 0.5226(3) 0.8615(2) 0.0526(11) Uani 1 1 d . . . . .
H3 H 0.8884 0.5158 0.8874 0.079 Uiso 1 1 calc R U . . .
C6 C 0.8650(3) 0.5966(3) 1.1941(2) 0.0291(11) Uani 1 1 d . . . . .
H6 H 0.9359 0.5883 1.2032 0.035 Uiso 1 1 calc R U . . .
C4 C 0.6935(3) 0.5933(3) 1.2406(2) 0.0252(10) Uani 1 1 d . . . . .
H4 H 0.6488 0.5838 1.2807 0.030 Uiso 1 1 calc R U . . .
C3 C 0.6543(3) 0.6163(3) 1.1678(2) 0.0197(10) Uani 1 1 d . . . . .
C1 C 0.4781(3) 0.6149(3) 1.2093(2) 0.0270(11) Uani 1 1 d . . . . .
H1A H 0.4088 0.6281 1.1903 0.041 Uiso 1 1 calc R U . . .
H1B H 0.4971 0.6582 1.2497 0.041 Uiso 1 1 calc R U . . .
H1C H 0.4813 0.5520 1.2290 0.041 Uiso 1 1 calc R U . . .
C12 C 0.7283(3) 0.6673(3) 0.7649(2) 0.0235(10) Uani 1 1 d . . . . .
H12 H 0.7594 0.6740 0.7177 0.028 Uiso 1 1 calc R U . . .
O9 O 0.4806(2) 0.7931(2) 1.00254(14) 0.0247(7) Uani 1 1 d . . . . .
C11 C 0.9010(3) 0.6801(4) 0.8096(2) 0.0343(13) Uani 1 1 d . . . . .
H11A H 0.9186 0.7458 0.8163 0.041 Uiso 1 1 calc R U . . .
H11B H 0.9134 0.6633 0.7566 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8002(3) 0.5844(4) 1.2539(2) 0.0315(12) Uani 1 1 d . . . . .
H5 H 0.8271 0.5702 1.3030 0.038 Uiso 1 1 calc R U . . .
C9 C 0.9835(3) 0.6570(4) 0.9436(2) 0.0352(13) Uani 1 1 d . . . . .
H9A H 1.0389 0.6222 0.9699 0.042 Uiso 1 1 calc R U . . .
H9B H 1.0045 0.7222 0.9422 0.042 Uiso 1 1 calc R U . . .
C23 C 0.8484(5) 0.9392(5) 0.9835(3) 0.077(2) Uani 1 1 d . . . . .
H23A H 0.9065 0.9162 0.9562 0.115 Uiso 1 1 calc R U . . .
H23B H 0.8729 0.9724 1.0287 0.115 Uiso 1 1 calc R U . . .
H23C H 0.8082 0.9808 0.9508 0.115 Uiso 1 1 calc R U . . .
O10 O 0.5603(2) 0.8825(2) 0.91640(17) 0.0342(8) Uani 1 1 d . . . . .
C20 C 0.4847(3) 0.8619(3) 0.9558(2) 0.0250(11) Uani 1 1 d . . . . .
C21 C 0.3914(3) 0.9259(4) 0.9515(3) 0.0451(14) Uani 1 1 d . . . . .
H21A H 0.3293 0.8889 0.9479 0.068 Uiso 1 1 calc R U . . .
H21B H 0.3948 0.9652 0.9067 0.068 Uiso 1 1 calc R U . . .
H21C H 0.3908 0.9642 0.9969 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Ni1 2.112(3) 3_667 ?
O7 C24 1.260(5) . ?
Ho1 Ho1 3.9754(9) 3_667 ?
Ho1 Ni1 3.3908(9) . ?
Ho1 O5 2.489(3) . ?
Ho1 O4 2.276(2) . ?
Ho1 O8 2.436(2) . ?
Ho1 O2 2.282(3) . ?
Ho1 O1 2.479(3) . ?
Ho1 O6 2.306(3) . ?
Ho1 O6 2.343(3) 3_667 ?
Ho1 C24 2.819(4) . ?
Ho1 O9 2.222(3) . ?
Ni1 O7 2.112(3) 3_667 ?
Ni1 O4 2.032(3) . ?
Ni1 O2 2.037(3) . ?
Ni1 N2 2.041(3) . ?
Ni1 N1 2.052(3) . ?
Ni1 O11 2.106(3) . ?
O5 C17 1.397(4) . ?
O5 C19 1.452(4) . ?
O4 C18 1.313(5) . ?
O8 C24 1.284(5) . ?
O2 C2 1.324(5) . ?
C17 C18 1.408(5) . ?
C17 C16 1.358(6) . ?
C2 C7 1.419(5) . ?
C2 C3 1.417(5) . ?
N2 C12 1.268(5) . ?
N2 C11 1.481(5) . ?
C18 C13 1.417(5) . ?
O1 C3 1.392(5) . ?
O1 C1 1.456(4) . ?
N1 C8 1.275(5) . ?
N1 C9 1.481(5) . ?
C14 C15 1.384(6) . ?
C14 C13 1.402(6) . ?
O6 Ho1 2.343(3) 3_667 ?
O6 C24 1.311(4) . ?
O11 C22 1.449(5) . ?
C15 C16 1.397(5) . ?
C10 O3 1.473(6) . ?
C10 C11 1.519(6) . ?
C10 C9 1.492(6) . ?
C8 C7 1.463(5) . ?
C13 C12 1.459(5) . ?
C22 C23 1.499(7) . ?
C7 C6 1.405(6) . ?
C6 C5 1.368(5) . ?
C4 C3 1.383(5) . ?
C4 C5 1.393(5) . ?
O9 C20 1.275(5) . ?
O10 C20 1.247(5) . ?
C20 C21 1.510(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
C24 O7 Ni1 123.1(3) . 3_667 ?
Ni1 Ho1 Ho1 95.383(11) . 3_667 ?
O5 Ho1 Ho1 87.45(7) . 3_667 ?
O5 Ho1 Ni1 100.91(6) . . ?
O5 Ho1 C24 79.17(10) . . ?
O4 Ho1 Ho1 97.83(7) . 3_667 ?
O4 Ho1 Ni1 35.61(7) . . ?
O4 Ho1 O5 65.61(8) . . ?
O4 Ho1 O8 144.58(10) . . ?
O4 Ho1 O2 70.55(9) . . ?
O4 Ho1 O1 136.09(9) . . ?
O4 Ho1 O6 121.19(10) . . ?
O4 Ho1 O6 73.83(10) . 3_667 ?
O4 Ho1 C24 138.99(11) . . ?
O8 Ho1 Ho1 85.84(7) . 3_667 ?
O8 Ho1 Ni1 178.73(7) . . ?
O8 Ho1 O5 79.46(9) . . ?
O8 Ho1 O1 78.94(9) . . ?
O8 Ho1 C24 27.05(10) . . ?
O2 Ho1 Ho1 100.43(7) . 3_667 ?
O2 Ho1 Ni1 35.77(6) . . ?
O2 Ho1 O5 136.12(9) . . ?
O2 Ho1 O8 143.66(9) . . ?
O2 Ho1 O1 65.56(9) . . ?
O2 Ho1 O6 126.02(10) . . ?
O2 Ho1 O6 74.24(10) . 3_667 ?
O2 Ho1 C24 141.22(11) . . ?
O1 Ho1 Ho1 88.95(7) . 3_667 ?
O1 Ho1 Ni1 100.73(6) . . ?
O1 Ho1 O5 158.30(8) . . ?
O1 Ho1 C24 80.66(11) . . ?
O6 Ho1 Ho1 31.50(6) . 3_667 ?
O6 Ho1 Ho1 30.95(6) 3_667 3_667 ?
O6 Ho1 Ni1 126.82(6) . . ?
O6 Ho1 Ni1 64.49(6) 3_667 . ?
O6 Ho1 O5 80.51(10) . . ?
O6 Ho1 O5 94.97(10) 3_667 . ?
O6 Ho1 O8 54.41(9) . . ?
O6 Ho1 O8 116.71(9) 3_667 . ?
O6 Ho1 O1 85.27(10) . . ?
O6 Ho1 O1 92.86(10) 3_667 . ?
O6 Ho1 O6 62.45(10) . 3_667 ?
O6 Ho1 C24 89.70(11) 3_667 . ?
O6 Ho1 C24 27.36(11) . . ?
C24 Ho1 Ho1 58.79(9) . 3_667 ?
C24 Ho1 Ni1 154.17(9) . . ?
O9 Ho1 Ho1 168.48(7) . 3_667 ?
O9 Ho1 Ni1 92.05(7) . . ?
O9 Ho1 O5 82.50(10) . . ?
O9 Ho1 O4 83.16(10) . . ?
O9 Ho1 O8 86.80(9) . . ?
O9 Ho1 O2 90.75(10) . . ?
O9 Ho1 O1 98.32(9) . . ?
O9 Ho1 O6 139.81(9) . . ?
O9 Ho1 O6 155.61(9) . 3_667 ?
O9 Ho1 C24 113.40(11) . . ?
O7 Ni1 Ho1 86.47(7) 3_667 . ?
O4 Ni1 O7 91.21(11) . 3_667 ?
O4 Ni1 Ho1 40.71(7) . . ?
O4 Ni1 O2 80.61(10) . . ?
O4 Ni1 N2 89.65(12) . . ?
O4 Ni1 N1 171.26(12) . . ?
O4 Ni1 O11 87.67(11) . . ?
O2 Ni1 O7 94.05(11) . 3_667 ?
O2 Ni1 Ho1 40.90(8) . . ?
O2 Ni1 N2 169.74(12) . . ?
O2 Ni1 N1 90.73(12) . . ?
O2 Ni1 O11 87.81(11) . . ?
N2 Ni1 O7 89.35(13) . 3_667 ?
N2 Ni1 Ho1 129.94(10) . . ?
N2 Ni1 N1 99.06(13) . . ?
N2 Ni1 O11 88.57(13) . . ?
N1 Ni1 O7 88.18(13) . 3_667 ?
N1 Ni1 Ho1 130.56(9) . . ?
N1 Ni1 O11 93.24(13) . . ?
O11 Ni1 O7 177.64(12) . 3_667 ?
O11 Ni1 Ho1 94.02(7) . . ?
C17 O5 Ho1 116.8(2) . . ?
C17 O5 C19 115.9(3) . . ?
C19 O5 Ho1 127.3(2) . . ?
Ni1 O4 Ho1 103.68(11) . . ?
C18 O4 Ho1 124.4(2) . . ?
C18 O4 Ni1 128.6(2) . . ?
C24 O8 Ho1 93.3(2) . . ?
Ni1 O2 Ho1 103.33(12) . . ?
C2 O2 Ho1 123.3(2) . . ?
C2 O2 Ni1 125.8(2) . . ?
O5 C17 C18 112.7(3) . . ?
C16 C17 O5 124.3(4) . . ?
C16 C17 C18 123.0(4) . . ?
O2 C2 C7 124.3(3) . . ?
O2 C2 C3 117.8(4) . . ?
C3 C2 C7 117.9(4) . . ?
C12 N2 Ni1 125.4(3) . . ?
C12 N2 C11 116.4(3) . . ?
C11 N2 Ni1 118.1(3) . . ?
O4 C18 C17 119.0(3) . . ?
O4 C18 C13 123.4(4) . . ?
C17 C18 C13 117.6(4) . . ?
C3 O1 Ho1 116.7(2) . . ?
C3 O1 C1 115.6(3) . . ?
C1 O1 Ho1 127.5(2) . . ?
C8 N1 Ni1 124.9(3) . . ?
C8 N1 C9 115.0(3) . . ?
C9 N1 Ni1 119.9(3) . . ?
C15 C14 C13 122.0(4) . . ?
Ho1 O6 Ho1 117.55(10) . 3_667 ?
C24 O6 Ho1 98.7(2) . . ?
C24 O6 Ho1 143.4(3) . 3_667 ?
C22 O11 Ni1 122.1(3) . . ?
C14 C15 C16 119.1(4) . . ?
O3 C10 C11 110.9(4) . . ?
O3 C10 C9 110.9(4) . . ?
C9 C10 C11 115.2(4) . . ?
C17 C16 C15 119.7(4) . . ?
O7 C24 Ho1 176.1(3) . . ?
O7 C24 O8 124.1(3) . . ?
O7 C24 O6 122.4(4) . . ?
O8 C24 Ho1 59.64(19) . . ?
O8 C24 O6 113.6(3) . . ?
O6 C24 Ho1 53.95(19) . . ?
N1 C8 C7 127.2(4) . . ?
C18 C13 C12 123.2(4) . . ?
C14 C13 C18 118.6(4) . . ?
C14 C13 C12 118.2(3) . . ?
O11 C22 C23 110.4(4) . . ?
C2 C7 C8 124.4(4) . . ?
C6 C7 C2 118.6(4) . . ?
C6 C7 C8 117.0(4) . . ?
C5 C6 C7 122.4(4) . . ?
C3 C4 C5 119.9(4) . . ?
O1 C3 C2 113.0(3) . . ?
C4 C3 C2 121.6(4) . . ?
C4 C3 O1 125.4(3) . . ?
N2 C12 C13 128.5(3) . . ?
C20 O9 Ho1 140.7(3) . . ?
N2 C11 C10 113.3(3) . . ?
C6 C5 C4 119.5(4) . . ?
N1 C9 C10 114.9(4) . . ?
O9 C20 C21 116.5(4) . . ?
O10 C20 O9 125.5(4) . . ?
O10 C20 C21 117.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O5 C17 C18 -7.2(4) . . . . ?
Ho1 O5 C17 C16 172.7(3) . . . . ?
Ho1 O4 C18 C17 11.7(5) . . . . ?
Ho1 O4 C18 C13 -168.7(3) . . . . ?
Ho1 O8 C24 O7 178.7(4) . . . . ?
Ho1 O8 C24 O6 -1.5(4) . . . . ?
Ho1 O2 C2 C7 161.7(3) . . . . ?
Ho1 O2 C2 C3 -19.7(5) . . . . ?
Ho1 O1 C3 C2 9.6(4) . . . . ?
Ho1 O1 C3 C4 -169.6(4) . . . . ?
Ho1 O6 C24 O7 -6.8(7) 3_667 . . . ?
Ho1 O6 C24 O7 -178.6(3) . . . . ?
Ho1 O6 C24 Ho1 171.8(5) 3_667 . . . ?
Ho1 O6 C24 O8 1.7(4) . . . . ?
Ho1 O6 C24 O8 173.5(3) 3_667 . . . ?
Ho1 O9 C20 O10 -52.6(7) . . . . ?
Ho1 O9 C20 C21 130.5(4) . . . . ?
Ni1 O7 C24 O8 -178.3(3) 3_667 . . . ?
Ni1 O7 C24 O6 2.0(6) 3_667 . . . ?
Ni1 O4 C18 C17 167.7(3) . . . . ?
Ni1 O4 C18 C13 -12.6(6) . . . . ?
Ni1 O2 C2 C7 17.1(6) . . . . ?
Ni1 O2 C2 C3 -164.3(3) . . . . ?
Ni1 N2 C12 C13 -2.6(7) . . . . ?
Ni1 N2 C11 C10 40.9(5) . . . . ?
Ni1 N1 C8 C7 -6.6(7) . . . . ?
Ni1 N1 C9 C10 -30.7(5) . . . . ?
Ni1 O11 C22 C23 136.2(4) . . . . ?
O5 C17 C18 O4 -1.8(5) . . . . ?
O5 C17 C18 C13 178.5(4) . . . . ?
O5 C17 C16 C15 -179.5(4) . . . . ?
O4 C18 C13 C14 -177.7(4) . . . . ?
O4 C18 C13 C12 1.6(7) . . . . ?
O2 C2 C7 C8 -5.1(7) . . . . ?
O2 C2 C7 C6 176.6(4) . . . . ?
O2 C2 C3 O1 5.0(5) . . . . ?
O2 C2 C3 C4 -175.8(4) . . . . ?
C17 C18 C13 C14 1.9(6) . . . . ?
C17 C18 C13 C12 -178.8(4) . . . . ?
C2 C7 C6 C5 -0.6(7) . . . . ?
C18 C17 C16 C15 0.4(7) . . . . ?
C18 C13 C12 N2 6.6(7) . . . . ?
N1 C8 C7 C2 -0.5(7) . . . . ?
N1 C8 C7 C6 177.8(5) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C14 C13 C12 N2 -174.1(5) . . . . ?
C15 C14 C13 C18 -1.6(7) . . . . ?
C15 C14 C13 C12 179.0(4) . . . . ?
C19 O5 C17 C18 174.8(3) . . . . ?
C19 O5 C17 C16 -5.3(6) . . . . ?
C16 C17 C18 O4 178.3(4) . . . . ?
C16 C17 C18 C13 -1.4(6) . . . . ?
C8 N1 C9 C10 144.5(4) . . . . ?
C8 C7 C6 C5 -179.0(4) . . . . ?
C13 C14 C15 C16 0.6(7) . . . . ?
C7 C2 C3 O1 -176.3(3) . . . . ?
C7 C2 C3 C4 2.9(6) . . . . ?
C7 C6 C5 C4 2.3(7) . . . . ?
O3 C10 C11 N2 52.0(5) . . . . ?
O3 C10 C9 N1 -58.4(5) . . . . ?
C3 C2 C7 C8 176.3(4) . . . . ?
C3 C2 C7 C6 -2.0(6) . . . . ?
C3 C4 C5 C6 -1.4(7) . . . . ?
C1 O1 C3 C2 -175.6(4) . . . . ?
C1 O1 C3 C4 5.2(6) . . . . ?
C12 N2 C11 C10 -142.7(5) . . . . ?
C11 N2 C12 C13 -178.7(4) . . . . ?
C11 C10 C9 N1 68.6(6) . . . . ?
C5 C4 C3 C2 -1.3(7) . . . . ?
C5 C4 C3 O1 177.9(4) . . . . ?
C9 N1 C8 C7 178.4(4) . . . . ?
C9 C10 C11 N2 -75.0(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_p140118e_sq
_database_code_depnum_ccdc_archive 'CCDC 1555627'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 N4 Ni2 O22 Tb2'
_chemical_formula_sum            'C48 H58 N4 Ni2 O22 Tb2'
_chemical_formula_weight         1478.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.950(3)
_cell_length_b                   14.299(3)
_cell_length_c                   17.450(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.61(3)
_cell_angle_gamma                90
_cell_volume                     3230.0(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7789
_cell_measurement_temperature    130.45(10)
_cell_measurement_theta_max      28.7570
_cell_measurement_theta_min      3.2370
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12736
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         3.079
_diffrn_ambient_temperature      130.45(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5052
_reflns_number_total             5690
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.570
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0540P)²+0.6438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1046
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H6 of C6, {H22A,H22B} of C22, H12 of C12, H4 of C4, H5 of C5, {H9A,H9B} of
  C9, {H11A,H11B} of C11, H10 of C10, H17 of C17, H16 of C16, H15 of C15, H8 of
  C8
 At 1.5 times of:
  H3 of O3, {H1A,H1B,H1C} of C1, {H23A,H23B,H23C} of C23, {H21A,H21B,H21C} of
  C21, H11 of O11, {H19A,H19B,H19C} of C19
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C22-H11
 1.901302 with sigma of 0.02
 Ni1-H11
 2.726953 with sigma of 0.02
3. Rigid bond restraints
 C24, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C9(H9A,H9B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C8(H8), C6(H6), C12(H12), C4(H4), C5(H5)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.2556(2) 0.4869(2) 1.0742(2) 0.0214(7) Uani 1 1 d . U . . .
Tb1 Tb 0.50504(2) 0.64000(2) 1.00827(2) 0.01471(10) Uani 1 1 d . . . . .
Ni1 Ni 0.74591(4) 0.66008(4) 0.93481(3) 0.01738(15) Uani 1 1 d D . . . .
C18 C 0.4478(4) 0.6472(3) 0.8178(3) 0.0184(11) Uani 1 1 d . . . . .
O2 O 0.6780(2) 0.6605(2) 1.03958(18) 0.0182(7) Uani 1 1 d . . . . .
O5 O 0.3954(2) 0.6446(2) 0.88709(19) 0.0202(8) Uani 1 1 d . . . . .
O6 O 0.3316(2) 0.6263(2) 1.06281(19) 0.0196(7) Uani 1 1 d . U . . .
O11 O 0.7457(2) 0.8072(2) 0.93876(19) 0.0233(7) Uani 1 1 d D . . . .
H11 H 0.694(2) 0.8395(14) 0.921(2) 0.035 Uiso 1 1 d D U . . .
O1 O 0.5504(2) 0.6238(2) 1.14861(18) 0.0205(7) Uani 1 1 d . . . . .
O4 O 0.5949(2) 0.6670(2) 0.89799(17) 0.0181(7) Uani 1 1 d . . . . .
N2 N 0.7902(3) 0.6690(3) 0.8233(2) 0.0204(9) Uani 1 1 d . . . . .
C2 C 0.7213(4) 0.6329(3) 1.1063(3) 0.0192(11) Uani 1 1 d . . . . .
O8 O 0.4111(2) 0.50239(19) 1.0225(2) 0.0232(8) Uani 1 1 d . U . . .
C19 C 0.2837(4) 0.6399(4) 0.8807(3) 0.0276(13) Uani 1 1 d . . . . .
H19A H 0.2635 0.5827 0.8556 0.041 Uiso 1 1 calc R U . . .
H19B H 0.2582 0.6921 0.8512 0.041 Uiso 1 1 calc R U . . .
H19C H 0.2555 0.6417 0.9309 0.041 Uiso 1 1 calc R U . . .
C13 C 0.5563(3) 0.6584(3) 0.8278(3) 0.0173(10) Uani 1 1 d . . . . .
N1 N 0.8898(3) 0.6506(3) 0.9876(3) 0.0234(10) Uani 1 1 d . . . . .
C10 C 0.9716(4) 0.6229(4) 0.8596(3) 0.0347(13) Uani 1 1 d . . . . .
H10 H 1.0403 0.6254 0.8375 0.042 Uiso 1 1 calc R U . . .
C24 C 0.3286(3) 0.5376(3) 1.0546(3) 0.0176(8) Uani 1 1 d . U . . .
C17 C 0.4012(4) 0.6393(3) 0.7461(3) 0.0256(12) Uani 1 1 d . . . . .
H17 H 0.3300 0.6315 0.7414 0.031 Uiso 1 1 calc R U . . .
C16 C 0.4602(4) 0.6428(3) 0.6806(3) 0.0300(13) Uani 1 1 d . . . . .
H16 H 0.4287 0.6385 0.6321 0.036 Uiso 1 1 calc R U . . .
C14 C 0.6155(3) 0.6587(3) 0.7616(3) 0.0178(10) Uani 1 1 d . . . . .
C15 C 0.5666(4) 0.6529(4) 0.6886(3) 0.0290(12) Uani 1 1 d . . . . .
H15 H 0.6063 0.6559 0.6451 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9052(4) 0.6308(3) 1.0581(3) 0.0243(12) Uani 1 1 d . . . . .
H8 H 0.9737 0.6217 1.0736 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8660(4) 0.5956(4) 1.1928(3) 0.0269(11) Uani 1 1 d . . . . .
H6 H 0.9366 0.5875 1.2016 0.032 Uiso 1 1 calc R U . . .
C22 C 0.7816(4) 0.8587(3) 1.0057(3) 0.0337(13) Uani 1 1 d D . . . .
H22A H 0.8210 0.8174 1.0396 0.040 Uiso 1 1 calc R U . . .
H22B H 0.7227 0.8815 1.0334 0.040 Uiso 1 1 calc R U . . .
C3 C 0.6562(3) 0.6146(3) 1.1679(3) 0.0196(10) Uani 1 1 d . . . . .
C7 C 0.8296(3) 0.6207(3) 1.1175(3) 0.0210(10) Uani 1 1 d . . . . .
O3 O 0.9407(3) 0.5242(3) 0.8595(3) 0.0544(12) Uani 1 1 d . . . . .
H3 H 0.8907 0.5174 0.8868 0.082 Uiso 1 1 calc R U . . .
C1 C 0.4799(4) 0.6130(4) 1.2111(3) 0.0243(11) Uani 1 1 d . . . . .
H1A H 0.4102 0.6211 1.1922 0.036 Uiso 1 1 calc R U . . .
H1B H 0.4952 0.6591 1.2498 0.036 Uiso 1 1 calc R U . . .
H1C H 0.4877 0.5516 1.2329 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7281(3) 0.6686(3) 0.7638(3) 0.0227(11) Uani 1 1 d . . . . .
H12 H 0.7589 0.6754 0.7166 0.027 Uiso 1 1 calc R U . . .
C4 C 0.6943(4) 0.5925(3) 1.2407(3) 0.0245(11) Uani 1 1 d . . . . .
H4 H 0.6499 0.5840 1.2811 0.029 Uiso 1 1 calc R U . . .
C5 C 0.8016(4) 0.5832(4) 1.2519(3) 0.0299(12) Uani 1 1 d . . . . .
H5 H 0.8287 0.5683 1.3003 0.036 Uiso 1 1 calc R U . . .
C9 C 0.9839(4) 0.6586(4) 0.9414(3) 0.0367(14) Uani 1 1 d . . . . .
H9A H 1.0393 0.6241 0.9670 0.044 Uiso 1 1 calc R U . . .
H9B H 1.0044 0.7238 0.9399 0.044 Uiso 1 1 calc R U . . .
C11 C 0.9016(3) 0.6809(4) 0.8081(3) 0.0362(14) Uani 1 1 d . . . . .
H11A H 0.9197 0.7463 0.8145 0.043 Uiso 1 1 calc R U . . .
H11B H 0.9134 0.6641 0.7552 0.043 Uiso 1 1 calc R U . . .
C23 C 0.8471(5) 0.9387(5) 0.9835(4) 0.0629(19) Uani 1 1 d . . . . .
H23A H 0.8088 0.9785 0.9487 0.094 Uiso 1 1 calc R U . . .
H23B H 0.9076 0.9158 0.9591 0.094 Uiso 1 1 calc R U . . .
H23C H 0.8673 0.9737 1.0285 0.094 Uiso 1 1 calc R U . . .
O9 O 0.4819(3) 0.7959(3) 1.00333(18) 0.0283(8) Uani 1 1 d . . . . .
C20 C 0.4859(4) 0.8643(3) 0.9565(3) 0.0249(12) Uani 1 1 d . . . . .
O10 O 0.5623(3) 0.8835(2) 0.9161(2) 0.0324(9) Uani 1 1 d . . . . .
C21 C 0.3933(4) 0.9271(4) 0.9519(4) 0.0472(16) Uani 1 1 d . . . . .
H21A H 0.3316 0.8898 0.9491 0.071 Uiso 1 1 calc R U . . .
H21B H 0.3966 0.9656 0.9070 0.071 Uiso 1 1 calc R U . . .
H21C H 0.3922 0.9661 0.9967 0.071 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Ni1 2.108(3) 3_667 ?
O7 C24 1.246(5) . ?
Tb1 Tb1 4.0158(9) 3_667 ?
Tb1 Ni1 3.4176(10) . ?
Tb1 O2 2.309(3) . ?
Tb1 O5 2.514(3) . ?
Tb1 O6 2.471(3) . ?
Tb1 O1 2.513(3) . ?
Tb1 O4 2.309(3) . ?
Tb1 O8 2.330(3) . ?
Tb1 O8 2.376(3) 3_667 ?
Tb1 C24 2.850(4) . ?
Tb1 O9 2.250(4) . ?
Ni1 O7 2.108(3) 3_667 ?
Ni1 O2 2.051(3) . ?
Ni1 O11 2.105(3) . ?
Ni1 O4 2.043(3) . ?
Ni1 N2 2.048(4) . ?
Ni1 N1 2.059(4) . ?
C18 O5 1.403(6) . ?
C18 C13 1.419(6) . ?
C18 C17 1.379(7) . ?
O2 C2 1.337(5) . ?
O5 C19 1.449(5) . ?
O6 C24 1.277(5) . ?
O11 C22 1.447(6) . ?
O1 C3 1.407(5) . ?
O1 C1 1.451(5) . ?
O4 C13 1.316(5) . ?
N2 C12 1.295(6) . ?
N2 C11 1.484(5) . ?
C2 C3 1.409(7) . ?
C2 C7 1.421(7) . ?
O8 Tb1 2.376(3) 3_667 ?
O8 C24 1.320(5) . ?
C13 C14 1.405(7) . ?
N1 C8 1.273(7) . ?
N1 C9 1.484(6) . ?
C10 O3 1.467(7) . ?
C10 C9 1.521(8) . ?
C10 C11 1.507(7) . ?
C17 C16 1.393(7) . ?
C16 C15 1.389(7) . ?
C14 C15 1.408(7) . ?
C14 C12 1.464(6) . ?
C8 C7 1.452(7) . ?
C6 C7 1.429(7) . ?
C6 C5 1.357(7) . ?
C22 C23 1.482(8) . ?
C3 C4 1.387(6) . ?
C4 C5 1.404(6) . ?
O9 C20 1.277(6) . ?
C20 O10 1.262(6) . ?
C20 C21 1.498(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
C24 O7 Ni1 124.3(3) . 3_667 ?
Ni1 Tb1 Tb1 94.876(12) . 3_667 ?
O2 Tb1 Tb1 99.94(8) . 3_667 ?
O2 Tb1 Ni1 35.77(8) . . ?
O2 Tb1 O5 135.78(11) . . ?
O2 Tb1 O6 143.59(11) . . ?
O2 Tb1 O1 65.31(11) . . ?
O2 Tb1 O8 73.48(11) . 3_667 ?
O2 Tb1 O8 125.98(11) . . ?
O2 Tb1 C24 141.07(12) . . ?
O5 Tb1 Tb1 87.08(7) . 3_667 ?
O5 Tb1 Ni1 100.49(8) . . ?
O5 Tb1 C24 79.27(12) . . ?
O6 Tb1 Tb1 85.44(7) . 3_667 ?
O6 Tb1 Ni1 179.33(8) . . ?
O6 Tb1 O5 80.11(11) . . ?
O6 Tb1 O1 78.91(11) . . ?
O6 Tb1 C24 26.56(11) . . ?
O1 Tb1 Tb1 89.11(7) . 3_667 ?
O1 Tb1 Ni1 100.50(8) . . ?
O1 Tb1 O5 158.91(11) . . ?
O1 Tb1 C24 81.01(12) . . ?
O4 Tb1 Tb1 97.05(8) . 3_667 ?
O4 Tb1 Ni1 35.58(7) . . ?
O4 Tb1 O2 70.59(11) . . ?
O4 Tb1 O5 65.21(10) . . ?
O4 Tb1 O6 144.98(11) . . ?
O4 Tb1 O1 135.87(10) . . ?
O4 Tb1 O8 73.17(11) . 3_667 ?
O4 Tb1 O8 120.45(12) . . ?
O4 Tb1 C24 138.52(12) . . ?
O8 Tb1 Tb1 31.09(8) 3_667 3_667 ?
O8 Tb1 Tb1 31.77(8) . 3_667 ?
O8 Tb1 Ni1 63.86(8) 3_667 . ?
O8 Tb1 Ni1 126.56(8) . . ?
O8 Tb1 O5 80.08(11) . . ?
O8 Tb1 O5 94.76(11) 3_667 . ?
O8 Tb1 O6 53.78(10) . . ?
O8 Tb1 O6 116.42(10) 3_667 . ?
O8 Tb1 O1 85.80(11) . . ?
O8 Tb1 O1 92.61(11) 3_667 . ?
O8 Tb1 O8 62.86(13) . 3_667 ?
O8 Tb1 C24 27.22(12) . . ?
O8 Tb1 C24 89.94(12) 3_667 . ?
C24 Tb1 Tb1 58.89(9) . 3_667 ?
C24 Tb1 Ni1 153.76(9) . . ?
O9 Tb1 Tb1 168.73(8) . 3_667 ?
O9 Tb1 Ni1 91.39(9) . . ?
O9 Tb1 O2 90.61(11) . . ?
O9 Tb1 O5 82.57(11) . . ?
O9 Tb1 O6 88.40(11) . . ?
O9 Tb1 O1 98.96(11) . . ?
O9 Tb1 O4 82.67(12) . . ?
O9 Tb1 O8 140.46(11) . . ?
O9 Tb1 O8 154.32(12) . 3_667 ?
O9 Tb1 C24 114.39(13) . . ?
O7 Ni1 Tb1 86.43(9) 3_667 . ?
O2 Ni1 O7 93.77(13) . 3_667 ?
O2 Ni1 Tb1 41.17(8) . . ?
O2 Ni1 O11 88.11(12) . . ?
O2 Ni1 N1 90.37(15) . . ?
O11 Ni1 O7 177.56(14) . 3_667 ?
O11 Ni1 Tb1 93.98(8) . . ?
O4 Ni1 O7 91.04(13) . 3_667 ?
O4 Ni1 Tb1 41.11(9) . . ?
O4 Ni1 O2 81.36(12) . . ?
O4 Ni1 O11 87.70(12) . . ?
O4 Ni1 N2 89.39(14) . . ?
O4 Ni1 N1 171.67(15) . . ?
N2 Ni1 O7 89.63(15) . 3_667 ?
N2 Ni1 Tb1 130.13(11) . . ?
N2 Ni1 O2 170.19(13) . . ?
N2 Ni1 O11 88.27(14) . . ?
N2 Ni1 N1 98.93(16) . . ?
N1 Ni1 O7 88.51(14) . 3_667 ?
N1 Ni1 Tb1 130.57(12) . . ?
N1 Ni1 O11 93.05(14) . . ?
O5 C18 C13 113.4(4) . . ?
C17 C18 O5 124.7(4) . . ?
C17 C18 C13 121.8(4) . . ?
Ni1 O2 Tb1 103.06(13) . . ?
C2 O2 Tb1 123.3(3) . . ?
C2 O2 Ni1 126.5(3) . . ?
C18 O5 Tb1 116.7(3) . . ?
C18 O5 C19 116.1(4) . . ?
C19 O5 Tb1 127.0(3) . . ?
C24 O6 Tb1 93.5(3) . . ?
C22 O11 Ni1 122.3(3) . . ?
C3 O1 Tb1 116.2(3) . . ?
C3 O1 C1 116.1(3) . . ?
C1 O1 Tb1 127.4(3) . . ?
Ni1 O4 Tb1 103.31(13) . . ?
C13 O4 Tb1 124.9(3) . . ?
C13 O4 Ni1 128.6(3) . . ?
C12 N2 Ni1 125.3(3) . . ?
C12 N2 C11 116.2(4) . . ?
C11 N2 Ni1 118.5(3) . . ?
O2 C2 C3 118.3(4) . . ?
O2 C2 C7 122.9(5) . . ?
C3 C2 C7 118.8(4) . . ?
Tb1 O8 Tb1 117.14(13) . 3_667 ?
C24 O8 Tb1 143.4(3) . 3_667 ?
C24 O8 Tb1 98.9(3) . . ?
O4 C13 C18 118.3(4) . . ?
O4 C13 C14 124.2(4) . . ?
C14 C13 C18 117.4(4) . . ?
C8 N1 Ni1 124.2(3) . . ?
C8 N1 C9 115.7(4) . . ?
C9 N1 Ni1 119.9(3) . . ?
O3 C10 C9 110.1(5) . . ?
O3 C10 C11 111.7(5) . . ?
C11 C10 C9 114.9(5) . . ?
O7 C24 Tb1 175.4(3) . . ?
O7 C24 O6 124.6(4) . . ?
O7 C24 O8 121.6(4) . . ?
O6 C24 Tb1 59.9(2) . . ?
O6 C24 O8 113.8(4) . . ?
O8 C24 Tb1 53.9(2) . . ?
C18 C17 C16 120.4(4) . . ?
C15 C16 C17 119.1(5) . . ?
C13 C14 C15 120.1(4) . . ?
C13 C14 C12 123.0(4) . . ?
C15 C14 C12 116.9(4) . . ?
C16 C15 C14 121.2(5) . . ?
N1 C8 C7 128.4(4) . . ?
C5 C6 C7 122.5(4) . . ?
O11 C22 C23 110.8(5) . . ?
O1 C3 C2 113.5(4) . . ?
C4 C3 O1 124.0(4) . . ?
C4 C3 C2 122.5(4) . . ?
C2 C7 C8 124.9(4) . . ?
C2 C7 C6 117.1(4) . . ?
C6 C7 C8 118.0(4) . . ?
N2 C12 C14 128.1(4) . . ?
C3 C4 C5 118.3(4) . . ?
C6 C5 C4 120.7(4) . . ?
N1 C9 C10 114.8(4) . . ?
N2 C11 C10 113.7(4) . . ?
C20 O9 Tb1 140.9(3) . . ?
O9 C20 C21 116.6(5) . . ?
O10 C20 O9 124.8(4) . . ?
O10 C20 C21 118.6(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O2 C2 C3 -18.0(5) . . . . ?
Tb1 O2 C2 C7 161.5(3) . . . . ?
Tb1 O6 C24 O7 178.9(4) . . . . ?
Tb1 O6 C24 O8 -1.4(4) . . . . ?
Tb1 O1 C3 C2 10.9(5) . . . . ?
Tb1 O1 C3 C4 -171.0(4) . . . . ?
Tb1 O4 C13 C18 11.1(6) . . . . ?
Tb1 O4 C13 C14 -168.2(3) . . . . ?
Tb1 O8 C24 O7 -178.8(4) . . . . ?
Tb1 O8 C24 O7 -8.5(8) 3_667 . . . ?
Tb1 O8 C24 Tb1 170.4(6) 3_667 . . . ?
Tb1 O8 C24 O6 1.5(4) . . . . ?
Tb1 O8 C24 O6 171.8(3) 3_667 . . . ?
Tb1 O9 C20 O10 -53.0(7) . . . . ?
Tb1 O9 C20 C21 128.9(5) . . . . ?
Ni1 O7 C24 O6 -177.0(3) 3_667 . . . ?
Ni1 O7 C24 O8 3.3(6) 3_667 . . . ?
Ni1 O2 C2 C3 -163.4(3) . . . . ?
Ni1 O2 C2 C7 16.1(6) . . . . ?
Ni1 O11 C22 C23 136.3(4) . . . . ?
Ni1 O4 C13 C18 167.6(3) . . . . ?
Ni1 O4 C13 C14 -11.7(7) . . . . ?
Ni1 N2 C12 C14 -2.3(7) . . . . ?
Ni1 N2 C11 C10 40.4(6) . . . . ?
Ni1 N1 C8 C7 -7.1(7) . . . . ?
Ni1 N1 C9 C10 -30.8(6) . . . . ?
C18 C13 C14 C15 3.3(7) . . . . ?
C18 C13 C14 C12 -179.3(4) . . . . ?
C18 C17 C16 C15 1.1(7) . . . . ?
O2 C2 C3 O1 3.1(6) . . . . ?
O2 C2 C3 C4 -175.1(4) . . . . ?
O2 C2 C7 C8 -3.8(7) . . . . ?
O2 C2 C7 C6 176.9(4) . . . . ?
O5 C18 C13 O4 -1.4(6) . . . . ?
O5 C18 C13 C14 178.0(4) . . . . ?
O5 C18 C17 C16 179.9(4) . . . . ?
O1 C3 C4 C5 178.5(4) . . . . ?
O4 C13 C14 C15 -177.4(4) . . . . ?
O4 C13 C14 C12 0.1(7) . . . . ?
C2 C3 C4 C5 -3.5(7) . . . . ?
C13 C18 O5 Tb1 -7.3(5) . . . . ?
C13 C18 O5 C19 175.8(4) . . . . ?
C13 C18 C17 C16 -0.5(7) . . . . ?
C13 C14 C15 C16 -2.8(7) . . . . ?
C13 C14 C12 N2 7.5(8) . . . . ?
N1 C8 C7 C2 -0.9(8) . . . . ?
N1 C8 C7 C6 178.4(5) . . . . ?
C17 C18 O5 Tb1 172.3(4) . . . . ?
C17 C18 O5 C19 -4.6(6) . . . . ?
C17 C18 C13 O4 179.0(4) . . . . ?
C17 C18 C13 C14 -1.7(7) . . . . ?
C17 C16 C15 C14 0.6(7) . . . . ?
C15 C14 C12 N2 -175.0(5) . . . . ?
C8 N1 C9 C10 143.9(5) . . . . ?
C3 C2 C7 C8 175.7(4) . . . . ?
C3 C2 C7 C6 -3.6(7) . . . . ?
C3 C4 C5 C6 0.0(8) . . . . ?
C7 C2 C3 O1 -176.5(4) . . . . ?
C7 C2 C3 C4 5.4(7) . . . . ?
C7 C6 C5 C4 1.5(8) . . . . ?
O3 C10 C9 N1 -58.5(6) . . . . ?
O3 C10 C11 N2 51.9(7) . . . . ?
C1 O1 C3 C2 -175.3(4) . . . . ?
C1 O1 C3 C4 2.8(6) . . . . ?
C12 N2 C11 C10 -142.0(5) . . . . ?
C12 C14 C15 C16 179.6(4) . . . . ?
C5 C6 C7 C2 0.3(7) . . . . ?
C5 C6 C7 C8 -179.1(5) . . . . ?
C9 N1 C8 C7 178.4(5) . . . . ?
C9 C10 C11 N2 -74.4(6) . . . . ?
C11 N2 C12 C14 -179.6(5) . . . . ?
C11 C10 C9 N1 68.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_nidyde_sq
_audit_block_doi                 10.5517/ccdc.csd.cc1p6rf2
_database_code_depnum_ccdc_archive 'CCDC 1555624'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 Dy2 N4 Ni2 O22'
_chemical_formula_sum            'C48 H58 Dy2 N4 Ni2 O22'
_chemical_formula_weight         1485.36
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.869(3)
_cell_length_b                   14.249(3)
_cell_length_c                   17.379(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.38(3)
_cell_angle_gamma                90
_cell_volume                     3184.1(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    128.60(10)
_cell_measurement_theta_max      28.8790
_cell_measurement_theta_min      3.4770
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12505
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         2.885
_diffrn_ambient_temperature      128.60(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5033
_reflns_number_total             5601
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         0.674
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+2.6725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0690
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H11a,H11b} of C11, H8 of C8, H15 of C15, H16 of C16, {H9a,H9b} of C9,
  {H20a,H20b} of C20, H14 of C14, H12 of C12, H6 of C6, H5 of C5, H10 of C10,
  H4 of C4
 At 1.5 times of:
  H11 of O11, {H21a,H21b,H21c} of C21, {H23a,H23b,H23c} of C23, {H19a,H19b,
  H19c} of C19, H3 of O3, {H1a,H1b,H1c} of C1
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C20-H11
 1.900874 with sigma of 0.02
 Ni1-H11
 2.715827 with sigma of 0.02
3. Rigid bond restraints
 C3, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O7, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C3, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C11(H11a,H11b), C9(H9a,H9b)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C12(H12), C14(H14), C15(H15), C8(H8), C16(H16)
4.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c)
4.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.74431(19) 0.51251(18) 0.42734(15) 0.0206(6) Uani 1 1 d . U . . .
O6 O 0.58751(19) 0.49758(17) 0.47742(15) 0.0209(6) Uani 1 1 d . U . . .
Dy1 Dy 0.49460(2) 0.36021(2) 0.49292(2) 0.01428(7) Uani 1 1 d . . . . .
Ni1 Ni 0.25419(4) 0.33998(3) 0.56414(3) 0.01679(12) Uani 1 1 d D . . . .
O4 O 0.32179(18) 0.33942(18) 0.45982(14) 0.0181(6) Uani 1 1 d . . . . .
O2 O 0.40546(18) 0.33292(18) 0.60185(14) 0.0173(6) Uani 1 1 d . . . . .
O1 O 0.60479(19) 0.35639(19) 0.61460(14) 0.0204(6) Uani 1 1 d . . . . .
O5 O 0.44961(19) 0.37524(19) 0.35255(14) 0.0187(6) Uani 1 1 d . . . . .
C0AA C 0.5530(3) 0.3537(3) 0.6835(2) 0.0172(8) Uani 1 1 d . . . . .
O11 O 0.2544(2) 0.19273(19) 0.56007(15) 0.0228(6) Uani 1 1 d D . . . .
H11 H 0.3074(19) 0.1616(14) 0.5785(17) 0.034 Uiso 1 1 d D U . . .
N1 N 0.2102(2) 0.3314(2) 0.67546(18) 0.0205(7) Uani 1 1 d . . . . .
C18 C 0.2785(3) 0.3665(3) 0.3934(2) 0.0176(8) Uani 1 1 d . . . . .
C4 C 0.6010(3) 0.3624(3) 0.7554(2) 0.0234(9) Uani 1 1 d . . . . .
H4 H 0.6727 0.3703 0.7606 0.028 Uiso 1 1 calc R U . . .
C10 C 0.0291(3) 0.3789(3) 0.6367(3) 0.0333(11) Uani 1 1 d . . . . .
H10 H -0.0401 0.3769 0.6580 0.040 Uiso 1 1 calc R U . . .
C2 C 0.4445(3) 0.3427(2) 0.6727(2) 0.0143(8) Uani 1 1 d . . . . .
C7 C 0.3843(3) 0.3420(3) 0.7387(2) 0.0175(8) Uani 1 1 d . . . . .
N2 N 0.1105(2) 0.3507(2) 0.51052(19) 0.0222(8) Uani 1 1 d . . . . .
C5 C 0.5410(3) 0.3594(3) 0.8203(2) 0.0267(10) Uani 1 1 d . . . . .
H5 H 0.5726 0.3643 0.8693 0.032 Uiso 1 1 calc R U . . .
C1 C 0.7169(3) 0.3599(3) 0.6215(2) 0.0247(10) Uani 1 1 d . . . . .
H1A H 0.7448 0.3563 0.5712 0.037 Uiso 1 1 calc R U . . .
H1B H 0.7421 0.3080 0.6521 0.037 Uiso 1 1 calc R U . . .
H1C H 0.7383 0.4177 0.6457 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4345(3) 0.3490(3) 0.8115(2) 0.0250(10) Uani 1 1 d . . . . .
H6 H 0.3951 0.3466 0.8551 0.030 Uiso 1 1 calc R U . . .
C12 C 0.0938(3) 0.3688(3) 0.4388(2) 0.0229(9) Uani 1 1 d . . . . .
H12 H 0.0247 0.3764 0.4223 0.027 Uiso 1 1 calc R U . . .
C14 C 0.1332(3) 0.4042(3) 0.3052(2) 0.0271(10) Uani 1 1 d . . . . .
H14 H 0.0622 0.4132 0.2961 0.033 Uiso 1 1 calc R U . . .
C20 C 0.2170(3) 0.1408(3) 0.4929(3) 0.0340(11) Uani 1 1 d D . . . .
H20A H 0.2757 0.1179 0.4650 0.041 Uiso 1 1 calc R U . . .
H20B H 0.1764 0.1819 0.4589 0.041 Uiso 1 1 calc R U . . .
C17 C 0.3444(3) 0.3839(3) 0.3317(2) 0.0184(8) Uani 1 1 d . . . . .
O9 O 0.5191(2) 0.2056(2) 0.49775(14) 0.0233(6) Uani 1 1 d . . . . .
C13 C 0.1708(3) 0.3789(3) 0.3802(2) 0.0187(8) Uani 1 1 d . . . . .
O3 O 0.0604(3) 0.4770(2) 0.6379(2) 0.0500(9) Uani 1 1 d . . . . .
H3 H 0.1192 0.4818 0.6220 0.075 Uiso 1 1 calc R U . . .
C19 C 0.5201(3) 0.3858(3) 0.2903(2) 0.0235(9) Uani 1 1 d . . . . .
H19A H 0.5167 0.4491 0.2714 0.035 Uiso 1 1 calc R U . . .
H19B H 0.5005 0.3432 0.2494 0.035 Uiso 1 1 calc R U . . .
H19C H 0.5898 0.3722 0.3089 0.035 Uiso 1 1 calc R U . . .
C15 C 0.1986(3) 0.4160(3) 0.2458(2) 0.0299(10) Uani 1 1 d . . . . .
H15 H 0.1716 0.4303 0.1967 0.036 Uiso 1 1 calc R U . . .
C8 C 0.2721(3) 0.3319(3) 0.7351(2) 0.0210(9) Uani 1 1 d . . . . .
H8 H 0.2411 0.3248 0.7821 0.025 Uiso 1 1 calc R U . . .
C16 C 0.3057(3) 0.4064(3) 0.2589(2) 0.0244(9) Uani 1 1 d . . . . .
H16 H 0.3506 0.4151 0.2190 0.029 Uiso 1 1 calc R U . . .
C11 C 0.0160(3) 0.3429(4) 0.5554(3) 0.0356(12) Uani 1 1 d . . . . .
H11A H -0.0049 0.2776 0.5569 0.043 Uiso 1 1 calc R U . . .
H11B H -0.0397 0.3777 0.5290 0.043 Uiso 1 1 calc R U . . .
C9 C 0.0991(3) 0.3189(4) 0.6901(2) 0.0328(11) Uani 1 1 d . . . . .
H9A H 0.0871 0.3356 0.7431 0.039 Uiso 1 1 calc R U . . .
H9B H 0.0807 0.2534 0.6831 0.039 Uiso 1 1 calc R U . . .
C21 C 0.1517(5) 0.0601(4) 0.5159(3) 0.0640(17) Uani 1 1 d . . . . .
H21A H 0.1916 0.0199 0.5502 0.096 Uiso 1 1 calc R U . . .
H21B H 0.1292 0.0254 0.4709 0.096 Uiso 1 1 calc R U . . .
H21C H 0.0920 0.0830 0.5415 0.096 Uiso 1 1 calc R U . . .
O10 O 0.4389(2) 0.1161(2) 0.58380(17) 0.0314(7) Uani 1 1 d . . . . .
C3 C 0.6705(3) 0.4624(3) 0.4469(2) 0.0178(7) Uani 1 1 d . U . . .
C22 C 0.5146(3) 0.1361(3) 0.5451(2) 0.0226(9) Uani 1 1 d . . . . .
C23 C 0.6091(3) 0.0740(3) 0.5497(3) 0.0413(12) Uani 1 1 d . . . . .
H23A H 0.6138 0.0398 0.5024 0.062 Uiso 1 1 calc R U . . .
H23B H 0.6037 0.0308 0.5917 0.062 Uiso 1 1 calc R U . . .
H23C H 0.6703 0.1119 0.5579 0.062 Uiso 1 1 calc R U . . .
O8 O 0.66775(19) 0.37193(19) 0.44072(15) 0.0210(6) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Ni1 2.107(3) 3_666 ?
O7 C3 1.246(4) . ?
O6 Dy1 2.352(2) 3_666 ?
O6 Dy1 2.315(2) . ?
O6 C3 1.311(4) . ?
Dy1 O6 2.352(2) 3_666 ?
Dy1 Dy1 3.9934(9) 3_666 ?
Dy1 Ni1 3.3919(10) . ?
Dy1 O4 2.293(2) . ?
Dy1 O2 2.287(3) . ?
Dy1 O1 2.497(2) . ?
Dy1 O5 2.493(2) . ?
Dy1 O9 2.226(3) . ?
Dy1 C3 2.835(4) . ?
Dy1 O8 2.446(3) . ?
Ni1 O7 2.107(3) 3_666 ?
Ni1 O4 2.043(3) . ?
Ni1 O2 2.031(2) . ?
Ni1 O11 2.099(3) . ?
Ni1 N1 2.042(3) . ?
Ni1 N2 2.042(3) . ?
O4 C18 1.318(4) . ?
O2 C2 1.318(4) . ?
O1 C0AA 1.395(4) . ?
O1 C1 1.443(4) . ?
O5 C17 1.393(4) . ?
O5 C19 1.448(4) . ?
C0AA C4 1.376(5) . ?
C0AA C2 1.409(5) . ?
O11 C20 1.448(5) . ?
N1 C8 1.280(5) . ?
N1 C9 1.473(5) . ?
C18 C17 1.416(5) . ?
C18 C13 1.407(5) . ?
C4 C5 1.394(6) . ?
C10 O3 1.456(5) . ?
C10 C11 1.506(6) . ?
C10 C9 1.527(6) . ?
C2 C7 1.411(5) . ?
C7 C6 1.400(5) . ?
C7 C8 1.450(5) . ?
N2 C12 1.282(5) . ?
N2 C11 1.476(5) . ?
C5 C6 1.381(6) . ?
C12 C13 1.457(5) . ?
C14 C13 1.418(5) . ?
C14 C15 1.369(6) . ?
C20 C21 1.489(6) . ?
C17 C16 1.378(5) . ?
O9 C22 1.291(5) . ?
C15 C16 1.395(6) . ?
O10 C22 1.240(5) . ?
C3 O8 1.295(5) . ?
C22 C23 1.503(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
C3 O7 Ni1 123.8(2) . 3_666 ?
Dy1 O6 Dy1 117.64(11) . 3_666 ?
C3 O6 Dy1 99.1(2) . . ?
C3 O6 Dy1 143.0(2) . 3_666 ?
O6 Dy1 O6 62.36(11) . 3_666 ?
O6 Dy1 Dy1 31.46(6) . 3_666 ?
O6 Dy1 Dy1 30.90(6) 3_666 3_666 ?
O6 Dy1 Ni1 126.70(6) . . ?
O6 Dy1 Ni1 64.43(6) 3_666 . ?
O6 Dy1 O1 80.74(9) . . ?
O6 Dy1 O1 94.45(9) 3_666 . ?
O6 Dy1 O5 85.04(9) . . ?
O6 Dy1 O5 93.00(9) 3_666 . ?
O6 Dy1 C3 89.45(10) 3_666 . ?
O6 Dy1 C3 27.18(10) . . ?
O6 Dy1 O8 116.54(9) 3_666 . ?
O6 Dy1 O8 54.29(9) . . ?
Ni1 Dy1 Dy1 95.295(10) . 3_666 ?
O4 Dy1 O6 125.46(9) . . ?
O4 Dy1 O6 74.13(9) . 3_666 ?
O4 Dy1 Dy1 100.09(6) . 3_666 ?
O4 Dy1 Ni1 35.98(6) . . ?
O4 Dy1 O1 136.08(9) . . ?
O4 Dy1 O5 65.30(9) . . ?
O4 Dy1 C3 140.65(9) . . ?
O4 Dy1 O8 143.58(9) . . ?
O2 Dy1 O6 73.73(9) . 3_666 ?
O2 Dy1 O6 121.28(9) . . ?
O2 Dy1 Dy1 97.82(7) . 3_666 ?
O2 Dy1 Ni1 35.62(6) . . ?
O2 Dy1 O4 70.80(9) . . ?
O2 Dy1 O1 65.30(8) . . ?
O2 Dy1 O5 136.09(8) . . ?
O2 Dy1 C3 138.98(10) . . ?
O2 Dy1 O8 144.53(9) . . ?
O1 Dy1 Dy1 87.28(6) . 3_666 ?
O1 Dy1 Ni1 100.59(6) . . ?
O1 Dy1 C3 79.50(9) . . ?
O5 Dy1 Dy1 88.89(6) . 3_666 ?
O5 Dy1 Ni1 100.72(6) . . ?
O5 Dy1 O1 158.61(9) . . ?
O5 Dy1 C3 80.55(9) . . ?
O9 Dy1 O6 155.28(9) . 3_666 ?
O9 Dy1 O6 140.14(9) . . ?
O9 Dy1 Dy1 168.56(7) . 3_666 ?
O9 Dy1 Ni1 91.85(7) . . ?
O9 Dy1 O4 90.93(9) . . ?
O9 Dy1 O2 82.87(9) . . ?
O9 Dy1 O1 82.63(9) . . ?
O9 Dy1 O5 98.55(9) . . ?
O9 Dy1 C3 113.91(10) . . ?
O9 Dy1 O8 87.22(9) . . ?
C3 Dy1 Dy1 58.57(8) . 3_666 ?
C3 Dy1 Ni1 153.87(8) . . ?
O8 Dy1 Dy1 85.69(6) . 3_666 ?
O8 Dy1 Ni1 178.98(6) . . ?
O8 Dy1 O1 79.72(9) . . ?
O8 Dy1 O5 79.01(9) . . ?
O8 Dy1 C3 27.12(10) . . ?
O7 Ni1 Dy1 86.27(7) 3_666 . ?
O4 Ni1 O7 93.63(10) . 3_666 ?
O4 Ni1 Dy1 41.25(7) . . ?
O4 Ni1 O11 88.00(10) . . ?
O2 Ni1 O7 91.19(10) . 3_666 ?
O2 Ni1 Dy1 41.00(7) . . ?
O2 Ni1 O4 81.28(10) . . ?
O2 Ni1 O11 87.63(10) . . ?
O2 Ni1 N1 89.48(12) . . ?
O2 Ni1 N2 171.53(12) . . ?
O11 Ni1 O7 177.83(11) . 3_666 ?
O11 Ni1 Dy1 94.02(7) . . ?
N1 Ni1 O7 89.73(12) . 3_666 ?
N1 Ni1 Dy1 130.07(9) . . ?
N1 Ni1 O4 170.22(11) . . ?
N1 Ni1 O11 88.44(12) . . ?
N1 Ni1 N2 98.94(13) . . ?
N2 Ni1 O7 87.89(12) . 3_666 ?
N2 Ni1 Dy1 130.53(10) . . ?
N2 Ni1 O4 90.37(12) . . ?
N2 Ni1 O11 93.54(12) . . ?
Ni1 O4 Dy1 102.78(10) . . ?
C18 O4 Dy1 123.5(2) . . ?
C18 O4 Ni1 126.5(2) . . ?
Ni1 O2 Dy1 103.38(10) . . ?
C2 O2 Dy1 124.7(2) . . ?
C2 O2 Ni1 128.3(2) . . ?
C0AA O1 Dy1 116.9(2) . . ?
C0AA O1 C1 116.2(3) . . ?
C1 O1 Dy1 126.9(2) . . ?
C17 O5 Dy1 116.5(2) . . ?
C17 O5 C19 115.4(3) . . ?
C19 O5 Dy1 127.8(2) . . ?
O1 C0AA C2 113.2(3) . . ?
C4 C0AA O1 124.4(3) . . ?
C4 C0AA C2 122.4(4) . . ?
C20 O11 Ni1 122.5(2) . . ?
C8 N1 Ni1 125.4(3) . . ?
C8 N1 C9 115.9(3) . . ?
C9 N1 Ni1 118.7(2) . . ?
O4 C18 C17 118.0(3) . . ?
O4 C18 C13 123.9(4) . . ?
C13 C18 C17 118.1(3) . . ?
C0AA C4 C5 119.3(4) . . ?
O3 C10 C11 111.1(4) . . ?
O3 C10 C9 111.9(4) . . ?
C11 C10 C9 114.9(4) . . ?
O2 C2 C0AA 118.3(3) . . ?
O2 C2 C7 123.8(3) . . ?
C0AA C2 C7 117.9(3) . . ?
C2 C7 C8 123.1(3) . . ?
C6 C7 C2 119.0(3) . . ?
C6 C7 C8 117.9(4) . . ?
C12 N2 Ni1 124.8(3) . . ?
C12 N2 C11 114.9(3) . . ?
C11 N2 Ni1 120.3(3) . . ?
C6 C5 C4 119.6(4) . . ?
C5 C6 C7 121.8(4) . . ?
N2 C12 C13 127.5(3) . . ?
C15 C14 C13 121.9(4) . . ?
O11 C20 C21 110.5(4) . . ?
O5 C17 C18 113.2(3) . . ?
C16 C17 O5 124.7(4) . . ?
C16 C17 C18 122.1(3) . . ?
C22 O9 Dy1 140.6(2) . . ?
C18 C13 C12 124.6(3) . . ?
C18 C13 C14 118.6(4) . . ?
C14 C13 C12 116.9(3) . . ?
C14 C15 C16 119.9(4) . . ?
N1 C8 C7 128.4(4) . . ?
C17 C16 C15 119.3(4) . . ?
N2 C11 C10 114.0(3) . . ?
N1 C9 C10 112.3(3) . . ?
O7 C3 O6 122.3(4) . . ?
O7 C3 Dy1 176.0(3) . . ?
O7 C3 O8 124.5(4) . . ?
O6 C3 Dy1 53.76(18) . . ?
O8 C3 O6 113.2(3) . . ?
O8 C3 Dy1 59.48(19) . . ?
O9 C22 C23 115.3(4) . . ?
O10 C22 O9 125.4(4) . . ?
O10 C22 C23 119.3(4) . . ?
C3 O8 Dy1 93.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 C3 O8 Dy1 -179.2(3) . . . . ?
O6 C3 O8 Dy1 1.7(3) . . . . ?
Dy1 O6 C3 O7 6.5(6) 3_666 . . . ?
Dy1 O6 C3 O7 179.1(3) . . . . ?
Dy1 O6 C3 Dy1 -172.6(4) 3_666 . . . ?
Dy1 O6 C3 O8 -1.8(3) . . . . ?
Dy1 O6 C3 O8 -174.4(2) 3_666 . . . ?
Dy1 O4 C18 C17 18.8(5) . . . . ?
Dy1 O4 C18 C13 -161.3(3) . . . . ?
Dy1 O2 C2 C0AA -12.4(5) . . . . ?
Dy1 O2 C2 C7 168.2(3) . . . . ?
Dy1 O1 C0AA C4 -172.0(3) . . . . ?
Dy1 O1 C0AA C2 6.9(4) . . . . ?
Dy1 O5 C17 C18 -10.3(4) . . . . ?
Dy1 O5 C17 C16 170.2(3) . . . . ?
Dy1 O9 C22 O10 52.7(6) . . . . ?
Dy1 O9 C22 C23 -129.8(4) . . . . ?
Ni1 O7 C3 O6 -2.3(5) 3_666 . . . ?
Ni1 O7 C3 O8 178.7(3) 3_666 . . . ?
Ni1 O4 C18 C17 164.0(3) . . . . ?
Ni1 O4 C18 C13 -16.1(5) . . . . ?
Ni1 O2 C2 C0AA -167.5(3) . . . . ?
Ni1 O2 C2 C7 13.1(5) . . . . ?
Ni1 O11 C20 C21 -136.5(4) . . . . ?
Ni1 N1 C8 C7 2.6(6) . . . . ?
Ni1 N1 C9 C10 -41.1(5) . . . . ?
Ni1 N2 C12 C13 4.7(6) . . . . ?
Ni1 N2 C11 C10 31.5(5) . . . . ?
O4 C18 C17 O5 -4.0(5) . . . . ?
O4 C18 C17 C16 175.6(3) . . . . ?
O4 C18 C13 C12 3.7(6) . . . . ?
O4 C18 C13 C14 -177.2(4) . . . . ?
O2 C2 C7 C6 177.3(3) . . . . ?
O2 C2 C7 C8 -1.1(6) . . . . ?
O1 C0AA C4 C5 179.5(4) . . . . ?
O1 C0AA C2 O2 2.5(5) . . . . ?
O1 C0AA C2 C7 -178.1(3) . . . . ?
O5 C17 C16 C15 -178.0(4) . . . . ?
C0AA C4 C5 C6 -0.9(6) . . . . ?
C0AA C2 C7 C6 -2.1(5) . . . . ?
C0AA C2 C7 C8 179.6(4) . . . . ?
C18 C17 C16 C15 2.6(6) . . . . ?
C4 C0AA C2 O2 -178.6(3) . . . . ?
C4 C0AA C2 C7 0.8(6) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C2 C0AA C4 C5 0.7(6) . . . . ?
C2 C7 C6 C5 1.9(6) . . . . ?
C2 C7 C8 N1 -7.4(7) . . . . ?
N2 C12 C13 C18 2.5(7) . . . . ?
N2 C12 C13 C14 -176.6(4) . . . . ?
C1 O1 C0AA C4 5.9(5) . . . . ?
C1 O1 C0AA C2 -175.2(3) . . . . ?
C6 C7 C8 N1 174.2(4) . . . . ?
C12 N2 C11 C10 -145.2(4) . . . . ?
C14 C15 C16 C17 0.8(7) . . . . ?
C17 C18 C13 C12 -176.5(4) . . . . ?
C17 C18 C13 C14 2.6(6) . . . . ?
C13 C18 C17 O5 176.2(3) . . . . ?
C13 C18 C17 C16 -4.3(6) . . . . ?
C13 C14 C15 C16 -2.4(7) . . . . ?
O3 C10 C11 N2 58.6(5) . . . . ?
O3 C10 C9 N1 -52.4(5) . . . . ?
C19 O5 C17 C18 175.8(3) . . . . ?
C19 O5 C17 C16 -3.7(5) . . . . ?
C15 C14 C13 C18 0.6(6) . . . . ?
C15 C14 C13 C12 179.8(4) . . . . ?
C8 N1 C9 C10 141.9(4) . . . . ?
C8 C7 C6 C5 -179.6(4) . . . . ?
C11 C10 C9 N1 75.6(5) . . . . ?
C11 N2 C12 C13 -178.9(4) . . . . ?
C9 N1 C8 C7 179.5(4) . . . . ?
C9 C10 C11 N2 -69.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_gd
_audit_block_doi                 10.5517/ccdc.csd.cc1p7lbv
_database_code_depnum_ccdc_archive 'CCDC 1556427'

_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H24 F15 Gd N2 Ni O12'
_chemical_formula_sum            'C31 H24 F15 Gd N2 Ni O12'
_chemical_formula_weight         1117.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.293(4)
_cell_length_b                   12.677(2)
_cell_length_c                   16.658(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.715(5)
_cell_angle_gamma                90
_cell_volume                     3828.0(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11940
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2188
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32172
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.032
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0435
	          2theta: -15.1203
scan:
	Number of images: 300
	           Slice: -105.0000 - 45.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0435
	          2theta: -15.1203
scan:
	Number of images: 200
	           Slice: -105.0000 - -5.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0435
	          2theta: -15.1203
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.015929
_diffrn_orient_matrix_UB_12      -0.036807
_diffrn_orient_matrix_UB_13      0.045401
_diffrn_orient_matrix_UB_21      0.064995
_diffrn_orient_matrix_UB_22      -0.020724
_diffrn_orient_matrix_UB_23      -0.039606
_diffrn_orient_matrix_UB_31      0.029387
_diffrn_orient_matrix_UB_32      0.036473
_diffrn_orient_matrix_UB_33      0.029141
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6116
_reflns_number_total             6693
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         2.336
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0738
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+50.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2135
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H12 of C12, H15 of C15, H16 of C16, H10 of C10, H6 of C6, {H11A,
  H11B} of C11, H14 of C14, {H9A,H9B} of C9, H5 of C5, H8 of C8, H24 of C24, H4
  of C4
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, {H12A,H12B} of O12, H3 of O3, {H1A,H1B,H1C} of C1
2.a Rotating group:
 O12(H12A,H12B)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B)
2.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C24(H24), C4(H4), C29(H29), C12(H12), C15(H15), C16(H16),
 C6(H6), C14(H14)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.26917(3) 0.00201(4) 0.13364(3) 0.0352(2) Uani 1 1 d . . . . .
Ni1 Ni 0.11178(7) 0.00890(9) 0.22581(7) 0.0322(3) Uani 1 1 d . . . . .
F10 F 0.5279(5) -0.1154(11) 0.1122(8) 0.120(4) Uani 1 1 d . . . . .
F6 F 0.2864(5) 0.2472(5) -0.1550(4) 0.068(2) Uani 1 1 d . . . . .
F4 F 0.1821(5) 0.2091(8) -0.1192(5) 0.094(3) Uani 1 1 d . . . . .
F8 F 0.4490(3) 0.3564(6) 0.0720(4) 0.0626(19) Uani 1 1 d . . . . .
F3 F 0.2226(5) 0.3771(7) 0.1658(6) 0.092(3) Uani 1 1 d . . . . .
F7 F 0.3972(4) 0.3476(7) 0.1793(6) 0.088(3) Uani 1 1 d . . . . .
F1 F 0.1346(6) 0.3533(8) 0.0746(5) 0.098(3) Uani 1 1 d . . . . .
F9 F 0.4861(4) 0.2478(6) 0.1626(5) 0.066(2) Uani 1 1 d . . . . .
F13 F 0.2282(4) -0.3578(6) 0.2462(5) 0.066(2) Uani 1 1 d . . . . .
F5 F 0.2460(6) 0.0869(6) -0.1599(4) 0.094(3) Uani 1 1 d . . . . .
F2 F 0.1142(6) 0.3716(8) 0.1963(7) 0.102(3) Uani 1 1 d . . . . .
F14 F 0.3351(5) -0.3532(9) 0.3097(5) 0.097(3) Uani 1 1 d . . . . .
F15 F 0.3173(6) -0.4375(6) 0.2020(7) 0.104(3) Uani 1 1 d . . . . .
F11 F 0.4701(5) -0.1668(9) 0.0013(5) 0.097(3) Uani 1 1 d . . . . .
F12 F 0.5091(6) -0.2782(8) 0.0917(7) 0.109(4) Uani 1 1 d . . . . .
O2 O 0.2213(4) 0.0158(4) 0.2571(4) 0.0298(13) Uani 1 1 d . . . . .
O5 O 0.2159(4) -0.1336(5) 0.0224(4) 0.0389(15) Uani 1 1 d . . . . .
O7 O 0.2128(4) 0.1721(6) 0.1348(5) 0.0496(18) Uani 1 1 d . . . . .
O11 O 0.2690(4) -0.1795(5) 0.1888(4) 0.0360(14) Uani 1 1 d . . . . .
O8 O 0.3602(4) 0.1363(5) 0.1337(4) 0.0411(16) Uani 1 1 d . . . . .
O12 O 0.1222(4) -0.1564(5) 0.2560(4) 0.0379(15) Uani 1 1 d . . . . .
H12A H 0.1589 -0.1858 0.2349 0.057 Uiso 1 1 d R U . . .
H12B H 0.0816 -0.1907 0.2371 0.057 Uiso 1 1 d R U . . .
O4 O 0.1423(3) -0.0291(5) 0.1169(4) 0.0304(14) Uani 1 1 d . . . . .
O9 O 0.2602(4) 0.0731(5) 0.0004(4) 0.0355(14) Uani 1 1 d . . . . .
O6 O 0.1129(4) 0.1703(5) 0.2004(4) 0.0358(14) Uani 1 1 d . . . . .
O3 O -0.0025(5) 0.2116(7) 0.2854(6) 0.070(3) Uani 1 1 d . . . . .
H3 H 0.0357 0.2059 0.2651 0.105 Uiso 1 1 calc R U . . .
O1 O 0.3614(4) -0.0062(5) 0.2670(4) 0.0398(16) Uani 1 1 d . . . . .
O10 O 0.3738(4) -0.0854(6) 0.0986(4) 0.0461(17) Uani 1 1 d . . . . .
C1 C 0.4408(6) 0.0072(10) 0.2712(8) 0.052(3) Uani 1 1 d . . . . .
H1A H 0.4650 -0.0582 0.2870 0.078 Uiso 1 1 calc R U . . .
H1B H 0.4571 0.0606 0.3104 0.078 Uiso 1 1 calc R U . . .
H1C H 0.4526 0.0280 0.2191 0.078 Uiso 1 1 calc R U . . .
C5 C 0.3388(7) -0.0371(10) 0.4810(6) 0.056(3) Uani 1 1 d . . . . .
H5 H 0.3657 -0.0523 0.5311 0.067 Uiso 1 1 calc R U . . .
N1 N 0.0938(5) 0.0313(7) 0.3418(5) 0.0407(19) Uani 1 1 d . . . . .
C17 C 0.1415(6) -0.1562(7) 0.0149(5) 0.035(2) Uani 1 1 d . . . . .
C21 C 0.1563(6) 0.3258(9) 0.1537(7) 0.051(3) Uani 1 1 d . . . . .
C2 C 0.2564(6) 0.0014(7) 0.3307(6) 0.036(2) Uani 1 1 d . . . . .
C3 C 0.3334(6) -0.0128(7) 0.3384(6) 0.037(2) Uani 1 1 d . . . . .
C23 C 0.2860(5) 0.1546(7) -0.0287(6) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.1440(7) 0.0195(8) 0.4018(6) 0.044(2) Uani 1 1 d . . . . .
H8 H 0.1286 0.0246 0.4527 0.053 Uiso 1 1 calc R U . . .
N2 N 0.0037(5) 0.0023(7) 0.1784(5) 0.042(2) Uani 1 1 d . . . . .
C28 C 0.3153(6) -0.2524(8) 0.1902(6) 0.040(2) Uani 1 1 d . . . . .
C24 C 0.3368(5) 0.2241(7) 0.0074(6) 0.035(2) Uani 1 1 d . . . . .
H24 H 0.3495 0.2827 -0.0212 0.042 Uiso 1 1 calc R U . . .
C18 C 0.1033(5) -0.0961(7) 0.0682(5) 0.0311(19) Uani 1 1 d . . . . .
C22 C 0.2505(8) 0.1748(9) -0.1166(7) 0.055(3) Uani 1 1 d . . . . .
C4 C 0.3743(6) -0.0326(8) 0.4138(6) 0.044(2) Uani 1 1 d . . . . .
H4 H 0.4251 -0.0426 0.4183 0.053 Uiso 1 1 calc R U . . .
C27 C 0.2975(8) -0.3530(9) 0.2348(8) 0.062(3) Uani 1 1 d . . . . .
C20 C 0.1611(6) 0.2107(8) 0.1645(6) 0.038(2) Uani 1 1 d . . . . .
C7 C 0.2214(6) -0.0009(8) 0.4018(6) 0.041(2) Uani 1 1 d . . . . .
C29 C 0.3816(7) -0.2537(9) 0.1577(7) 0.051(3) Uani 1 1 d . . . . .
H29 H 0.4112 -0.3135 0.1652 0.062 Uiso 1 1 calc R U . . .
C25 C 0.3704(5) 0.2084(8) 0.0878(6) 0.033(2) Uani 1 1 d . . . . .
C26 C 0.4253(6) 0.2918(9) 0.1269(7) 0.044(2) Uani 1 1 d . . . . .
C12 C -0.0202(6) -0.0541(8) 0.1148(6) 0.039(2) Uani 1 1 d . . . . .
H12 H -0.0709 -0.0591 0.1002 0.047 Uiso 1 1 calc R U . . .
C31 C 0.4795(8) -0.1811(13) 0.0791(9) 0.069(4) Uani 1 1 d . . . . .
C13 C 0.0269(5) -0.1098(7) 0.0647(6) 0.035(2) Uani 1 1 d . . . . .
C15 C 0.0289(7) -0.2408(9) -0.0405(7) 0.052(3) Uani 1 1 d . . . . .
H15 H 0.0043 -0.2897 -0.0760 0.063 Uiso 1 1 calc R U . . .
C16 C 0.1042(6) -0.2285(8) -0.0387(6) 0.045(2) Uani 1 1 d . . . . .
H16 H 0.1296 -0.2680 -0.0730 0.054 Uiso 1 1 calc R U . . .
C10 C -0.0318(7) 0.1118(10) 0.2958(7) 0.053(3) Uani 1 1 d . . . . .
H10 H -0.0775 0.1237 0.3192 0.064 Uiso 1 1 calc R U . . .
C6 C 0.2650(6) -0.0200(9) 0.4761(7) 0.047(3) Uani 1 1 d . . . . .
H6 H 0.2429 -0.0209 0.5233 0.056 Uiso 1 1 calc R U . . .
C19 C 0.2524(6) -0.1644(10) -0.0450(6) 0.049(3) Uani 1 1 d . . . . .
H19A H 0.2232 -0.1432 -0.0946 0.074 Uiso 1 1 calc R U . . .
H19B H 0.2585 -0.2396 -0.0447 0.074 Uiso 1 1 calc R U . . .
H19C H 0.2999 -0.1310 -0.0408 0.074 Uiso 1 1 calc R U . . .
C9 C 0.0182(6) 0.0465(10) 0.3588(6) 0.048(3) Uani 1 1 d . . . . .
H9A H 0.0199 0.0808 0.4111 0.057 Uiso 1 1 calc R U . . .
H9B H -0.0042 -0.0223 0.3631 0.057 Uiso 1 1 calc R U . . .
C30 C 0.4050(6) -0.1712(10) 0.1157(6) 0.048(3) Uani 1 1 d . . . . .
C11 C -0.0548(6) 0.0558(10) 0.2151(7) 0.051(3) Uani 1 1 d . . . . .
H11A H -0.0922 0.0040 0.2231 0.062 Uiso 1 1 calc R U . . .
H11B H -0.0777 0.1074 0.1767 0.062 Uiso 1 1 calc R U . . .
C14 C -0.0102(7) -0.1833(10) 0.0085(7) 0.054(3) Uani 1 1 d . . . . .
H14 H -0.0610 -0.1920 0.0051 0.065 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Ni1 3.4411(14) . ?
Gd1 O2 2.348(6) . ?
Gd1 O5 2.618(6) . ?
Gd1 O7 2.392(8) . ?
Gd1 O11 2.477(6) . ?
Gd1 O8 2.382(7) . ?
Gd1 O4 2.333(6) . ?
Gd1 O9 2.381(6) . ?
Gd1 O1 2.606(7) . ?
Gd1 O10 2.352(7) . ?
Ni1 O2 2.003(6) . ?
Ni1 O12 2.157(7) . ?
Ni1 O4 2.026(6) . ?
Ni1 O6 2.090(6) . ?
Ni1 N1 2.023(9) . ?
Ni1 N2 2.029(9) . ?
F10 C31 1.284(19) . ?
F6 C22 1.340(13) . ?
F4 C22 1.319(16) . ?
F8 C26 1.341(13) . ?
F3 C21 1.369(15) . ?
F7 C26 1.283(13) . ?
F1 C21 1.368(13) . ?
F9 C26 1.313(12) . ?
F13 C27 1.307(15) . ?
F5 C22 1.324(14) . ?
F2 C21 1.257(15) . ?
F14 C27 1.341(16) . ?
F15 C27 1.277(14) . ?
F11 C31 1.297(16) . ?
F12 C31 1.350(17) . ?
O2 C2 1.319(11) . ?
O5 C17 1.381(12) . ?
O5 C19 1.435(11) . ?
O7 C20 1.226(13) . ?
O11 C28 1.251(12) . ?
O8 C25 1.221(11) . ?
O12 H12A 0.8824 . ?
O12 H12B 0.8817 . ?
O4 C18 1.317(10) . ?
O9 C23 1.260(11) . ?
O6 C20 1.241(12) . ?
O3 H3 0.8200 . ?
O3 C10 1.395(15) . ?
O1 C1 1.454(12) . ?
O1 C3 1.359(13) . ?
O10 C30 1.243(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C4 1.369(17) . ?
C5 C6 1.359(17) . ?
N1 C8 1.273(14) . ?
N1 C9 1.461(14) . ?
C17 C18 1.422(13) . ?
C17 C16 1.393(13) . ?
C21 C20 1.472(15) . ?
C2 C3 1.408(15) . ?
C2 C7 1.419(16) . ?
C3 C4 1.396(14) . ?
C23 C24 1.361(13) . ?
C23 C22 1.541(15) . ?
C8 H8 0.9300 . ?
C8 C7 1.439(16) . ?
N2 C12 1.304(13) . ?
N2 C11 1.469(14) . ?
C28 C27 1.533(15) . ?
C28 C29 1.394(15) . ?
C24 H24 0.9300 . ?
C24 C25 1.411(13) . ?
C18 C13 1.402(13) . ?
C4 H4 0.9300 . ?
C7 C6 1.402(15) . ?
C29 H29 0.9300 . ?
C29 C30 1.358(17) . ?
C25 C26 1.541(13) . ?
C12 H12 0.9300 . ?
C12 C13 1.459(15) . ?
C31 C30 1.571(15) . ?
C13 C14 1.427(14) . ?
C15 H15 0.9300 . ?
C15 C16 1.381(17) . ?
C15 C14 1.366(17) . ?
C16 H16 0.9300 . ?
C10 H10 0.9800 . ?
C10 C9 1.539(15) . ?
C10 C11 1.527(16) . ?
C6 H6 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C14 H14 0.9300 . ?

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 Gd1 Ni1 34.34(15) . . ?
O2 Gd1 O5 121.5(2) . . ?
O2 Gd1 O7 73.4(2) . . ?
O2 Gd1 O11 74.1(2) . . ?
O2 Gd1 O8 106.8(2) . . ?
O2 Gd1 O9 143.3(2) . . ?
O2 Gd1 O1 62.0(2) . . ?
O2 Gd1 O10 131.6(2) . . ?
O5 Gd1 Ni1 94.50(15) . . ?
O7 Gd1 Ni1 65.55(18) . . ?
O7 Gd1 O5 118.5(2) . . ?
O7 Gd1 O11 144.3(2) . . ?
O7 Gd1 O1 105.1(2) . . ?
O11 Gd1 Ni1 79.38(15) . . ?
O11 Gd1 O5 68.5(2) . . ?
O11 Gd1 O1 71.3(2) . . ?
O8 Gd1 Ni1 127.50(18) . . ?
O8 Gd1 O5 131.5(2) . . ?
O8 Gd1 O7 70.0(2) . . ?
O8 Gd1 O11 134.4(2) . . ?
O8 Gd1 O9 71.9(2) . . ?
O8 Gd1 O1 69.9(2) . . ?
O4 Gd1 Ni1 34.84(15) . . ?
O4 Gd1 O2 68.6(2) . . ?
O4 Gd1 O5 62.3(2) . . ?
O4 Gd1 O7 74.4(2) . . ?
O4 Gd1 O11 80.6(2) . . ?
O4 Gd1 O8 143.6(2) . . ?
O4 Gd1 O9 90.6(2) . . ?
O4 Gd1 O1 127.9(2) . . ?
O4 Gd1 O10 136.1(2) . . ?
O9 Gd1 Ni1 116.72(16) . . ?
O9 Gd1 O5 67.4(2) . . ?
O9 Gd1 O7 72.0(2) . . ?
O9 Gd1 O11 133.9(2) . . ?
O9 Gd1 O1 140.0(2) . . ?
O1 Gd1 Ni1 96.06(16) . . ?
O1 Gd1 O5 135.6(2) . . ?
O10 Gd1 Ni1 151.65(18) . . ?
O10 Gd1 O5 75.7(2) . . ?
O10 Gd1 O7 142.5(3) . . ?
O10 Gd1 O11 72.3(2) . . ?
O10 Gd1 O8 75.2(3) . . ?
O10 Gd1 O9 84.5(2) . . ?
O10 Gd1 O1 74.8(2) . . ?
O2 Ni1 Gd1 41.39(18) . . ?
O2 Ni1 O12 85.9(2) . . ?
O2 Ni1 O4 81.8(3) . . ?
O2 Ni1 O6 88.5(2) . . ?
O2 Ni1 N1 91.8(3) . . ?
O2 Ni1 N2 172.3(3) . . ?
O12 Ni1 Gd1 91.52(19) . . ?
O4 Ni1 Gd1 41.12(17) . . ?
O4 Ni1 O12 87.2(2) . . ?
O4 Ni1 O6 92.3(2) . . ?
O4 Ni1 N2 90.8(3) . . ?
O6 Ni1 Gd1 84.44(19) . . ?
O6 Ni1 O12 174.4(3) . . ?
N1 Ni1 Gd1 133.1(3) . . ?
N1 Ni1 O12 86.2(3) . . ?
N1 Ni1 O4 171.1(3) . . ?
N1 Ni1 O6 93.6(3) . . ?
N1 Ni1 N2 95.9(4) . . ?
N2 Ni1 Gd1 130.9(3) . . ?
N2 Ni1 O12 95.8(3) . . ?
N2 Ni1 O6 89.8(3) . . ?
Ni1 O2 Gd1 104.3(2) . . ?
C2 O2 Gd1 127.7(6) . . ?
C2 O2 Ni1 125.6(6) . . ?
C17 O5 Gd1 118.0(5) . . ?
C17 O5 C19 115.4(7) . . ?
C19 O5 Gd1 124.4(6) . . ?
C20 O7 Gd1 136.0(6) . . ?
C28 O11 Gd1 131.2(6) . . ?
C25 O8 Gd1 134.4(6) . . ?
Ni1 O12 H12A 111.5 . . ?
Ni1 O12 H12B 110.7 . . ?
H12A O12 H12B 107.4 . . ?
Ni1 O4 Gd1 104.0(2) . . ?
C18 O4 Gd1 129.1(6) . . ?
C18 O4 Ni1 120.9(6) . . ?
C23 O9 Gd1 133.4(6) . . ?
C20 O6 Ni1 121.9(6) . . ?
C10 O3 H3 109.5 . . ?
C1 O1 Gd1 124.4(6) . . ?
C3 O1 Gd1 118.1(6) . . ?
C3 O1 C1 117.2(8) . . ?
C30 O10 Gd1 136.0(7) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C6 C5 C4 121.4(10) . . ?
C8 N1 Ni1 122.7(7) . . ?
C8 N1 C9 117.7(9) . . ?
C9 N1 Ni1 118.9(7) . . ?
O5 C17 C18 113.1(8) . . ?
O5 C17 C16 125.9(9) . . ?
C16 C17 C18 120.9(9) . . ?
F3 C21 C20 114.5(9) . . ?
F1 C21 F3 99.1(11) . . ?
F1 C21 C20 112.1(9) . . ?
F2 C21 F3 107.2(10) . . ?
F2 C21 F1 107.8(10) . . ?
F2 C21 C20 114.9(12) . . ?
O2 C2 C3 117.3(9) . . ?
O2 C2 C7 124.1(10) . . ?
C7 C2 C3 118.7(9) . . ?
O1 C3 C2 113.8(9) . . ?
O1 C3 C4 125.3(10) . . ?
C4 C3 C2 120.9(10) . . ?
O9 C23 C24 129.0(9) . . ?
O9 C23 C22 111.7(8) . . ?
C24 C23 C22 119.2(9) . . ?
N1 C8 H8 115.6 . . ?
N1 C8 C7 128.8(10) . . ?
C7 C8 H8 115.6 . . ?
C12 N2 Ni1 122.8(8) . . ?
C12 N2 C11 114.1(9) . . ?
C11 N2 Ni1 123.1(7) . . ?
O11 C28 C27 115.9(9) . . ?
O11 C28 C29 128.5(9) . . ?
C29 C28 C27 115.5(10) . . ?
C23 C24 H24 119.6 . . ?
C23 C24 C25 120.9(9) . . ?
C25 C24 H24 119.6 . . ?
O4 C18 C17 117.4(8) . . ?
O4 C18 C13 124.1(9) . . ?
C13 C18 C17 118.5(8) . . ?
F6 C22 C23 113.3(9) . . ?
F4 C22 F6 106.3(10) . . ?
F4 C22 C23 111.3(10) . . ?
F5 C22 F6 108.4(10) . . ?
F5 C22 F4 105.7(11) . . ?
F5 C22 C23 111.4(9) . . ?
C5 C4 C3 119.1(10) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
F13 C27 F14 104.6(10) . . ?
F13 C27 C28 112.4(10) . . ?
F14 C27 C28 109.7(11) . . ?
F15 C27 F13 111.1(12) . . ?
F15 C27 F14 104.9(12) . . ?
F15 C27 C28 113.5(10) . . ?
O7 C20 O6 131.9(10) . . ?
O7 C20 C21 112.5(10) . . ?
O6 C20 C21 115.6(10) . . ?
C2 C7 C8 123.4(10) . . ?
C6 C7 C2 118.3(10) . . ?
C6 C7 C8 118.2(10) . . ?
C28 C29 H29 118.6 . . ?
C30 C29 C28 122.8(10) . . ?
C30 C29 H29 118.6 . . ?
O8 C25 C24 128.0(9) . . ?
O8 C25 C26 113.3(8) . . ?
C24 C25 C26 118.7(8) . . ?
F8 C26 C25 112.5(9) . . ?
F7 C26 F8 108.8(10) . . ?
F7 C26 F9 108.5(10) . . ?
F7 C26 C25 111.5(9) . . ?
F9 C26 F8 103.7(9) . . ?
F9 C26 C25 111.4(9) . . ?
N2 C12 H12 117.6 . . ?
N2 C12 C13 124.8(9) . . ?
C13 C12 H12 117.6 . . ?
F10 C31 F11 109.2(14) . . ?
F10 C31 F12 106.6(13) . . ?
F10 C31 C30 111.5(12) . . ?
F11 C31 F12 106.2(12) . . ?
F11 C31 C30 111.8(11) . . ?
F12 C31 C30 111.3(12) . . ?
C18 C13 C12 125.3(8) . . ?
C18 C13 C14 119.4(10) . . ?
C14 C13 C12 115.3(9) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C14 C15 C16 121.8(10) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 C17 119.3(10) . . ?
C15 C16 H16 120.4 . . ?
O3 C10 H10 105.8 . . ?
O3 C10 C9 111.7(10) . . ?
O3 C10 C11 112.2(10) . . ?
C9 C10 H10 105.8 . . ?
C11 C10 H10 105.8 . . ?
C11 C10 C9 114.8(10) . . ?
C5 C6 C7 121.6(11) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C9 C10 115.4(9) . . ?
N1 C9 H9A 108.4 . . ?
N1 C9 H9B 108.4 . . ?
C10 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
O10 C30 C29 128.7(10) . . ?
O10 C30 C31 112.1(10) . . ?
C29 C30 C31 119.2(11) . . ?
N2 C11 C10 116.7(9) . . ?
N2 C11 H11A 108.1 . . ?
N2 C11 H11B 108.1 . . ?
C10 C11 H11A 108.1 . . ?
C10 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(11) . . ?
C15 C14 H14 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O2 C2 C3 7.6(11) . . . . ?
Gd1 O2 C2 C7 -172.3(6) . . . . ?
Gd1 O5 C17 C18 3.0(9) . . . . ?
Gd1 O5 C17 C16 -177.7(8) . . . . ?
Gd1 O7 C20 O6 -8.2(17) . . . . ?
Gd1 O7 C20 C21 172.9(6) . . . . ?
Gd1 O11 C28 C27 176.5(7) . . . . ?
Gd1 O11 C28 C29 -2.2(16) . . . . ?
Gd1 O8 C25 C24 -14.0(15) . . . . ?
Gd1 O8 C25 C26 163.9(7) . . . . ?
Gd1 O4 C18 C17 -3.0(11) . . . . ?
Gd1 O4 C18 C13 178.4(6) . . . . ?
Gd1 O9 C23 C24 9.2(15) . . . . ?
Gd1 O9 C23 C22 -168.5(7) . . . . ?
Gd1 O1 C3 C2 -8.9(10) . . . . ?
Gd1 O1 C3 C4 170.5(8) . . . . ?
Gd1 O10 C30 C29 8.2(19) . . . . ?
Gd1 O10 C30 C31 -174.2(8) . . . . ?
Ni1 O2 C2 C3 166.9(6) . . . . ?
Ni1 O2 C2 C7 -12.9(12) . . . . ?
Ni1 O4 C18 C17 -151.2(6) . . . . ?
Ni1 O4 C18 C13 30.2(11) . . . . ?
Ni1 O6 C20 O7 3.3(14) . . . . ?
Ni1 O6 C20 C21 -177.8(6) . . . . ?
Ni1 N1 C8 C7 6.4(16) . . . . ?
Ni1 N1 C9 C10 -37.6(13) . . . . ?
Ni1 N2 C12 C13 -6.8(13) . . . . ?
Ni1 N2 C11 C10 -4.3(14) . . . . ?
F10 C31 C30 O10 66.9(15) . . . . ?
F10 C31 C30 C29 -115.2(15) . . . . ?
F3 C21 C20 O7 -41.8(13) . . . . ?
F3 C21 C20 O6 139.1(10) . . . . ?
F1 C21 C20 O7 70.1(12) . . . . ?
F1 C21 C20 O6 -109.1(11) . . . . ?
F2 C21 C20 O7 -166.5(10) . . . . ?
F2 C21 C20 O6 14.4(13) . . . . ?
F11 C31 C30 O10 -55.6(17) . . . . ?
F11 C31 C30 C29 122.3(14) . . . . ?
F12 C31 C30 O10 -174.2(12) . . . . ?
F12 C31 C30 C29 3.7(18) . . . . ?
O2 C2 C3 O1 1.9(12) . . . . ?
O2 C2 C3 C4 -177.5(8) . . . . ?
O2 C2 C7 C8 -4.3(14) . . . . ?
O2 C2 C7 C6 178.2(9) . . . . ?
O5 C17 C18 O4 -0.5(11) . . . . ?
O5 C17 C18 C13 178.2(7) . . . . ?
O5 C17 C16 C15 -178.5(9) . . . . ?
O11 C28 C27 F13 16.9(15) . . . . ?
O11 C28 C27 F14 -99.0(12) . . . . ?
O11 C28 C27 F15 144.0(12) . . . . ?
O11 C28 C29 C30 -2.0(18) . . . . ?
O8 C25 C26 F8 165.5(9) . . . . ?
O8 C25 C26 F7 -71.8(12) . . . . ?
O8 C25 C26 F9 49.6(12) . . . . ?
O4 C18 C13 C12 -1.1(14) . . . . ?
O4 C18 C13 C14 178.8(9) . . . . ?
O9 C23 C24 C25 2.2(16) . . . . ?
O9 C23 C22 F6 -167.3(9) . . . . ?
O9 C23 C22 F4 73.0(11) . . . . ?
O9 C23 C22 F5 -44.7(14) . . . . ?
O3 C10 C9 N1 -57.3(13) . . . . ?
O3 C10 C11 N2 81.9(12) . . . . ?
O1 C3 C4 C5 -180.0(10) . . . . ?
C1 O1 C3 C2 164.6(9) . . . . ?
C1 O1 C3 C4 -16.0(14) . . . . ?
N1 C8 C7 C2 7.9(17) . . . . ?
N1 C8 C7 C6 -174.6(11) . . . . ?
C17 C18 C13 C12 -179.7(8) . . . . ?
C17 C18 C13 C14 0.2(13) . . . . ?
C2 C3 C4 C5 -0.6(15) . . . . ?
C2 C7 C6 C5 -0.7(16) . . . . ?
C3 C2 C7 C8 175.8(9) . . . . ?
C3 C2 C7 C6 -1.7(13) . . . . ?
C23 C24 C25 O8 0.1(16) . . . . ?
C23 C24 C25 C26 -177.8(9) . . . . ?
C8 N1 C9 C10 151.2(10) . . . . ?
C8 C7 C6 C5 -178.3(11) . . . . ?
N2 C12 C13 C18 -12.3(15) . . . . ?
N2 C12 C13 C14 167.9(10) . . . . ?
C28 C29 C30 O10 -1(2) . . . . ?
C28 C29 C30 C31 -178.2(11) . . . . ?
C24 C23 C22 F6 14.7(15) . . . . ?
C24 C23 C22 F4 -105.0(11) . . . . ?
C24 C23 C22 F5 137.3(11) . . . . ?
C24 C25 C26 F8 -16.3(13) . . . . ?
C24 C25 C26 F7 106.3(11) . . . . ?
C24 C25 C26 F9 -132.3(10) . . . . ?
C18 C17 C16 C15 0.7(15) . . . . ?
C18 C13 C14 C15 1.1(16) . . . . ?
C22 C23 C24 C25 179.8(9) . . . . ?
C4 C5 C6 C7 2.5(18) . . . . ?
C27 C28 C29 C30 179.3(11) . . . . ?
C7 C2 C3 O1 -178.2(8) . . . . ?
C7 C2 C3 C4 2.3(13) . . . . ?
C29 C28 C27 F13 -164.2(10) . . . . ?
C29 C28 C27 F14 79.8(13) . . . . ?
C29 C28 C27 F15 -37.1(17) . . . . ?
C12 N2 C11 C10 172.5(10) . . . . ?
C12 C13 C14 C15 -179.0(10) . . . . ?
C16 C17 C18 O4 -179.7(8) . . . . ?
C16 C17 C18 C13 -1.0(13) . . . . ?
C16 C15 C14 C13 -1.5(18) . . . . ?
C6 C5 C4 C3 -1.8(18) . . . . ?
C19 O5 C17 C18 -160.8(8) . . . . ?
C19 O5 C17 C16 18.4(13) . . . . ?
C9 N1 C8 C7 177.2(10) . . . . ?
C9 C10 C11 N2 -47.0(15) . . . . ?
C11 N2 C12 C13 176.3(9) . . . . ?
C11 C10 C9 N1 71.9(14) . . . . ?
C14 C15 C16 C17 0.6(17) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_m20160305a_sq
_database_code_depnum_ccdc_archive 'CCDC 1484047'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H60 Cl4 Gd N2 Ni O11'
_chemical_formula_sum            'C66 H60 Cl4 Gd N2 Ni O11'
_chemical_formula_weight         1414.90
_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'
Gd Gd -0.1653 3.9035 '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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2556(16)
_cell_length_b                   12.667(2)
_cell_length_c                   23.339(4)
_cell_angle_alpha                82.268(15)
_cell_angle_beta                 83.837(11)
_cell_angle_gamma                77.065(11)
_cell_volume                     3203.3(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10905
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1436
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41041
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         3.039
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.8843
	          2theta: -15.1083
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.8843
	          2theta: -15.1083
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.8843
	          2theta: -15.1083
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.036249
_diffrn_orient_matrix_UB_12      0.069716
_diffrn_orient_matrix_UB_13      0.046785
_diffrn_orient_matrix_UB_21      -0.079732
_diffrn_orient_matrix_UB_22      0.016777
_diffrn_orient_matrix_UB_23      0.002904
_diffrn_orient_matrix_UB_31      0.000520
_diffrn_orient_matrix_UB_32      -0.027392
_diffrn_orient_matrix_UB_33      0.033633
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13455
_reflns_number_total             14485
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         2.798
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         14485
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+6.8699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0844
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  {H10A,H10B} of C10, {H66A,H66B} of C66, H31 of C31, H47 of C47, H41 of C41,
  H40 of C40, {H22A,H22B} of C22, H25 of C25, H3A of C3, H35 of C35, H64 of C64,
   H9 of C9, {H37A,H37B} of C37, {H12A,H12B} of C12, H46 of C46, H29 of C29,
  H57 of C57, H11 of C11, {H52A,H52B} of C52, H43 of C43, H62 of C62, H63 of
  C63, H42 of C42, H58 of C58, H56 of C56, H59 of C59, H49 of C49, H61 of C61,
  H44 of C44, H33 of C33, H28 of C28, H50 of C50, H13 of C13, H17 of C17, H65
  of C65, H32 of C32, H15 of C15, H5 of C5, H4 of C4, H16 of C16, H55 of C55,
  H27 of C27, H48 of C48, H26 of C26, H34 of C34, {H67A,H67B} of C67
 At 1.5 times of:
  H3 of O3, {H1A,H1B,H1C} of C1, {H20A,H20B,H20C} of C20
2.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C12(H12A,H12B), C37(H37A,H37B), C22(H22A,H22B), C66(H66A,
 H66B), C10(H10A,H10B), C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C62(H62), C63(H63), C42(H42), C58(H58), C56(H56), C59(H59),
 C49(H49), C61(H61), C44(H44), C33(H33), C28(H28), C50(H50), C13(H13), C17(H17),
  C65(H65), C32(H32), C15(H15), C5(H5), C4(H4), C16(H16), C55(H55), C57(H57),
 C29(H29), C46(H46), C9(H9), C64(H64), C35(H35), C3(H3A), C25(H25), C40(H40),
 C41(H41), C47(H47), C31(H31), C27(H27), C48(H48), C26(H26), C34(H34)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.77345(2) 0.21308(2) 0.27972(2) 0.01371(4) Uani 1 1 d . . . . .
Ni1 Ni 0.91667(3) 0.29066(3) 0.15488(2) 0.01678(8) Uani 1 1 d . . . . .
Cl3 Cl 0.73620(11) 0.37100(9) 0.56752(6) 0.0608(3) Uani 1 1 d . . . . .
Cl4 Cl 0.95280(12) 0.21001(14) 0.53886(5) 0.0794(5) Uani 1 1 d . . . . .
Cl2 Cl 0.75441(13) -0.13456(10) 0.17696(6) 0.0650(3) Uani 1 1 d . . . . .
O2 O 0.78565(17) 0.20158(16) 0.17725(8) 0.0175(4) Uani 1 1 d . . . . .
Cl1 Cl 0.86843(19) -0.02458(13) 0.07574(6) 0.0862(5) Uani 1 1 d . . . . .
O9 O 0.57391(17) 0.30515(16) 0.28505(8) 0.0178(4) Uani 1 1 d . . . . .
O11 O 0.85403(17) 0.02505(16) 0.28326(8) 0.0176(4) Uani 1 1 d . . . . .
O5 O 0.97620(18) 0.15735(17) 0.34055(8) 0.0209(4) Uani 1 1 d . . . . .
O4 O 0.96785(17) 0.22237(16) 0.23364(8) 0.0172(4) Uani 1 1 d . . . . .
O8 O 0.76005(17) 0.34963(16) 0.33906(8) 0.0179(4) Uani 1 1 d . . . . .
O10 O 0.70472(18) 0.13217(16) 0.36846(8) 0.0196(4) Uani 1 1 d . . . . .
O7 O 0.79120(18) 0.39506(16) 0.20280(8) 0.0193(4) Uani 1 1 d . . . . .
O1 O 0.62529(18) 0.11270(16) 0.23613(8) 0.0188(4) Uani 1 1 d . . . . .
O6 O 1.03026(19) 0.39808(18) 0.14617(9) 0.0229(4) Uani 1 1 d . . . . .
O3 O 1.1516(2) 0.3491(2) 0.04338(10) 0.0350(6) Uani 1 1 d . . . . .
H3 H 1.1324 0.3644 0.0766 0.052 Uiso 1 1 calc R U . . .
N2 N 0.8493(2) 0.3391(2) 0.07648(10) 0.0232(5) Uani 1 1 d . . . . .
C60 C 0.7072(3) 0.4775(2) 0.40699(12) 0.0189(5) Uani 1 1 d . . . . .
C52 C 0.5484(3) 0.4031(2) 0.36658(12) 0.0197(6) Uani 1 1 d . . . . .
H52A H 0.5222 0.3691 0.4041 0.024 Uiso 1 1 calc R U . . .
H52B H 0.5040 0.4785 0.3637 0.024 Uiso 1 1 calc R U . . .
C18 C 0.5891(3) 0.1680(2) 0.18379(12) 0.0198(6) Uani 1 1 d . . . . .
C45 C 0.9376(2) -0.1615(2) 0.30473(12) 0.0177(5) Uani 1 1 d . . . . .
C24 C 0.6774(3) 0.5606(2) 0.23253(13) 0.0214(6) Uani 1 1 d . . . . .
N1 N 1.0556(2) 0.1824(2) 0.11657(10) 0.0228(5) Uani 1 1 d . . . . .
C43 C 0.6273(3) -0.0575(3) 0.55445(13) 0.0298(7) Uani 1 1 d . . . . .
H43 H 0.6207 -0.1221 0.5775 0.036 Uiso 1 1 calc R U . . .
C7 C 1.0626(2) 0.1444(2) 0.24605(12) 0.0175(5) Uani 1 1 d . . . . .
C54 C 0.3715(2) 0.3592(2) 0.32397(12) 0.0176(5) Uani 1 1 d . . . . .
C19 C 0.6811(2) 0.2176(2) 0.15303(12) 0.0186(5) Uani 1 1 d . . . . .
C62 C 0.8693(3) 0.5347(3) 0.44649(13) 0.0261(6) Uani 1 1 d . . . . .
H62 H 0.9522 0.5268 0.4505 0.031 Uiso 1 1 calc R U . . .
C51 C 0.5054(2) 0.3541(2) 0.32497(12) 0.0176(5) Uani 1 1 d . . . . .
C63 C 0.7846(3) 0.6142(3) 0.47290(13) 0.0264(6) Uani 1 1 d . . . . .
H63 H 0.8106 0.6605 0.4943 0.032 Uiso 1 1 calc R U . . .
C39 C 0.6819(2) 0.0368(2) 0.46140(12) 0.0188(5) Uani 1 1 d . . . . .
C42 C 0.5929(3) 0.0407(3) 0.57762(13) 0.0277(7) Uani 1 1 d . . . . .
H42 H 0.5630 0.0420 0.6163 0.033 Uiso 1 1 calc R U . . .
C58 C 0.2063(3) 0.3438(2) 0.26951(13) 0.0212(6) Uani 1 1 d . . . . .
H58 H 0.1783 0.3353 0.2347 0.025 Uiso 1 1 calc R U . . .
C56 C 0.1676(3) 0.3686(3) 0.37051(13) 0.0243(6) Uani 1 1 d . . . . .
H56 H 0.1140 0.3759 0.4037 0.029 Uiso 1 1 calc R U . . .
C59 C 0.3282(3) 0.3455(2) 0.27205(12) 0.0191(5) Uani 1 1 d . . . . .
H59 H 0.3818 0.3376 0.2389 0.023 Uiso 1 1 calc R U . . .
C49 C 1.1199(3) -0.2509(3) 0.25092(13) 0.0234(6) Uani 1 1 d . . . . .
H49 H 1.1883 -0.2462 0.2253 0.028 Uiso 1 1 calc R U . . .
C61 C 0.8304(3) 0.4667(3) 0.41400(13) 0.0227(6) Uani 1 1 d . . . . .
H61 H 0.8878 0.4131 0.3966 0.027 Uiso 1 1 calc R U . . .
C44 C 0.6719(3) -0.0595(3) 0.49654(13) 0.0239(6) Uani 1 1 d . . . . .
H44 H 0.6952 -0.1258 0.4811 0.029 Uiso 1 1 calc R U . . .
C53 C 0.6720(3) 0.4051(2) 0.36860(11) 0.0171(5) Uani 1 1 d . . . . .
C33 C 1.2693(5) 0.6860(4) 0.09428(17) 0.0557(13) Uani 1 1 d . . . . .
H33 H 1.3278 0.7267 0.0806 0.067 Uiso 1 1 calc R U . . .
C28 C 0.4562(3) 0.6018(3) 0.24352(15) 0.0304(7) Uani 1 1 d . . . . .
H28 H 0.3821 0.5887 0.2353 0.036 Uiso 1 1 calc R U . . .
C50 C 1.0395(3) -0.1565(2) 0.26543(12) 0.0194(5) Uani 1 1 d . . . . .
H50 H 1.0536 -0.0890 0.2488 0.023 Uiso 1 1 calc R U . . .
C13 C 0.7465(3) 0.3284(3) 0.06227(13) 0.0278(7) Uani 1 1 d . . . . .
H13 H 0.7273 0.3551 0.0245 0.033 Uiso 1 1 calc R U . . .
C17 C 0.4779(3) 0.1768(3) 0.16247(14) 0.0267(6) Uani 1 1 d . . . . .
H17 H 0.4187 0.1435 0.1837 0.032 Uiso 1 1 calc R U . . .
C1 C 0.9830(3) 0.1368(3) 0.40196(13) 0.0289(7) Uani 1 1 d . . . . .
H1A H 0.9120 0.1795 0.4209 0.043 Uiso 1 1 calc R U . . .
H1B H 1.0552 0.1562 0.4120 0.043 Uiso 1 1 calc R U . . .
H1C H 0.9863 0.0608 0.4142 0.043 Uiso 1 1 calc R U . . .
C65 C 0.6231(3) 0.5567(3) 0.43449(15) 0.0288(7) Uani 1 1 d . . . . .
H65 H 0.5401 0.5644 0.4309 0.035 Uiso 1 1 calc R U . . .
C32 C 1.1488(5) 0.7363(4) 0.09945(17) 0.0519(12) Uani 1 1 d . . . . .
H32 H 1.1256 0.8109 0.0885 0.062 Uiso 1 1 calc R U . . .
C6 C 1.1509(3) 0.0945(2) 0.20518(13) 0.0201(6) Uani 1 1 d . . . . .
C15 C 0.5424(3) 0.2859(3) 0.07738(14) 0.0340(8) Uani 1 1 d . . . . .
H15 H 0.5262 0.3249 0.0413 0.041 Uiso 1 1 calc R U . . .
C20 C 0.5403(3) 0.0582(3) 0.27093(14) 0.0256(6) Uani 1 1 d . . . . .
H20A H 0.5772 0.0195 0.3050 0.038 Uiso 1 1 calc R U . . .
H20B H 0.5177 0.0077 0.2492 0.038 Uiso 1 1 calc R U . . .
H20C H 0.4687 0.1108 0.2821 0.038 Uiso 1 1 calc R U . . .
C5 C 1.2506(3) 0.0132(3) 0.22518(15) 0.0250(6) Uani 1 1 d . . . . .
H5 H 1.3093 -0.0205 0.1984 0.030 Uiso 1 1 calc R U . . .
C30 C 1.0935(3) 0.5649(3) 0.13613(13) 0.0286(7) Uani 1 1 d . . . . .
C4 C 1.2620(3) -0.0166(3) 0.28320(15) 0.0257(6) Uani 1 1 d . . . . .
H4 H 1.3295 -0.0687 0.2954 0.031 Uiso 1 1 calc R U . . .
C36 C 0.7281(2) 0.0395(2) 0.39846(12) 0.0170(5) Uani 1 1 d . . . . .
C16 C 0.4546(3) 0.2367(3) 0.10831(15) 0.0334(8) Uani 1 1 d . . . . .
H16 H 0.3797 0.2430 0.0933 0.040 Uiso 1 1 calc R U . . .
C55 C 0.2894(3) 0.3715(3) 0.37292(12) 0.0221(6) Uani 1 1 d . . . . .
H55 H 0.3165 0.3817 0.4076 0.026 Uiso 1 1 calc R U . . .
C23 C 1.0004(3) 0.4969(3) 0.15746(12) 0.0214(6) Uani 1 1 d . . . . .
C21 C 0.7923(3) 0.4942(2) 0.20694(12) 0.0189(5) Uani 1 1 d . . . . .
C11 C 1.0590(3) 0.3054(3) 0.02457(13) 0.0317(7) Uani 1 1 d . . . . .
H11 H 1.0788 0.3006 -0.0171 0.038 Uiso 1 1 calc R U . . .
C57 C 0.1254(3) 0.3549(2) 0.31899(13) 0.0218(6) Uani 1 1 d . . . . .
H57 H 0.0437 0.3530 0.3174 0.026 Uiso 1 1 calc R U . . .
C29 C 0.5661(3) 0.5389(2) 0.22199(13) 0.0235(6) Uani 1 1 d . . . . .
H29 H 0.5651 0.4823 0.2006 0.028 Uiso 1 1 calc R U . . .
C46 C 0.9168(3) -0.2635(2) 0.32837(13) 0.0212(6) Uani 1 1 d . . . . .
H46 H 0.8495 -0.2685 0.3546 0.025 Uiso 1 1 calc R U . . .
C12 C 0.9314(3) 0.3828(3) 0.03067(13) 0.0305(7) Uani 1 1 d . . . . .
H12A H 0.9413 0.4529 0.0394 0.037 Uiso 1 1 calc R U . . .
H12B H 0.8946 0.3942 -0.0060 0.037 Uiso 1 1 calc R U . . .
C38 C 0.8571(2) -0.0571(2) 0.32074(12) 0.0166(5) Uani 1 1 d . . . . .
C37 C 0.7961(3) -0.0554(2) 0.37691(12) 0.0196(6) Uani 1 1 d . . . . .
H37A H 0.7414 -0.1054 0.3798 0.024 Uiso 1 1 calc R U . . .
H37B H 0.8578 -0.0872 0.4039 0.024 Uiso 1 1 calc R U . . .
C14 C 0.6562(3) 0.2788(3) 0.09904(13) 0.0251(6) Uani 1 1 d . . . . .
C9 C 1.1419(3) 0.1164(2) 0.14272(13) 0.0231(6) Uani 1 1 d . . . . .
H9 H 1.2052 0.0787 0.1195 0.028 Uiso 1 1 calc R U . . .
C8 C 1.0745(3) 0.1079(2) 0.30602(12) 0.0195(6) Uani 1 1 d . . . . .
C64 C 0.6616(3) 0.6246(3) 0.46735(15) 0.0319(7) Uani 1 1 d . . . . .
H64 H 0.6044 0.6772 0.4856 0.038 Uiso 1 1 calc R U . . .
C35 C 1.2165(3) 0.5140(4) 0.12979(14) 0.0373(8) Uani 1 1 d . . . . .
H35 H 1.2399 0.4391 0.1393 0.045 Uiso 1 1 calc R U . . .
C3 C 1.1733(3) 0.0305(3) 0.32445(14) 0.0244(6) Uani 1 1 d . . . . .
H3A H 1.1812 0.0096 0.3638 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6776(3) 0.6437(3) 0.26569(15) 0.0294(7) Uani 1 1 d . . . . .
H25 H 0.7514 0.6592 0.2727 0.035 Uiso 1 1 calc R U . . .
C22 C 0.8902(3) 0.5449(3) 0.18646(13) 0.0242(6) Uani 1 1 d . . . . .
H22A H 0.8558 0.6089 0.1609 0.029 Uiso 1 1 calc R U . . .
H22B H 0.9128 0.5717 0.2199 0.029 Uiso 1 1 calc R U . . .
C40 C 0.6461(3) 0.1352(3) 0.48554(13) 0.0229(6) Uani 1 1 d . . . . .
H40 H 0.6513 0.2002 0.4626 0.028 Uiso 1 1 calc R U . . .
C41 C 0.6027(3) 0.1370(3) 0.54351(13) 0.0261(6) Uani 1 1 d . . . . .
H41 H 0.5803 0.2028 0.5594 0.031 Uiso 1 1 calc R U . . .
C47 C 0.9968(3) -0.3578(3) 0.31270(14) 0.0254(6) Uani 1 1 d . . . . .
H47 H 0.9817 -0.4256 0.3281 0.030 Uiso 1 1 calc R U . . .
C31 C 1.0605(4) 0.6771(3) 0.12088(15) 0.0374(8) Uani 1 1 d . . . . .
H31 H 0.9788 0.7125 0.1251 0.045 Uiso 1 1 calc R U . . .
C66 C 0.8552(5) -0.0496(4) 0.15180(18) 0.0494(10) Uani 1 1 d . . . . .
H66A H 0.9351 -0.0828 0.1652 0.059 Uiso 1 1 calc R U . . .
H66B H 0.8269 0.0193 0.1679 0.059 Uiso 1 1 calc R U . . .
C10 C 1.0640(3) 0.1892(3) 0.05292(13) 0.0289(7) Uani 1 1 d . . . . .
H10A H 0.9972 0.1624 0.0411 0.035 Uiso 1 1 calc R U . . .
H10B H 1.1401 0.1428 0.0396 0.035 Uiso 1 1 calc R U . . .
C27 C 0.4575(3) 0.6835(3) 0.27716(17) 0.0374(8) Uani 1 1 d . . . . .
H27 H 0.3843 0.7245 0.2920 0.045 Uiso 1 1 calc R U . . .
C48 C 1.0989(3) -0.3518(2) 0.27435(13) 0.0245(6) Uani 1 1 d . . . . .
H48 H 1.1526 -0.4152 0.2645 0.029 Uiso 1 1 calc R U . . .
C26 C 0.5673(4) 0.7043(3) 0.28869(17) 0.0376(8) Uani 1 1 d . . . . .
H26 H 0.5680 0.7585 0.3117 0.045 Uiso 1 1 calc R U . . .
C34 C 1.3053(4) 0.5744(5) 0.10923(16) 0.0531(13) Uani 1 1 d . . . . .
H34 H 1.3875 0.5402 0.1056 0.064 Uiso 1 1 calc R U . . .
C67 C 0.8339(4) 0.2504(3) 0.59157(17) 0.0429(9) Uani 1 1 d . . . . .
H67A H 0.7878 0.1934 0.6015 0.052 Uiso 1 1 calc R U . . .
H67B H 0.8684 0.2601 0.6264 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Ni1 3.3141(6) . ?
Gd1 O2 2.4028(19) . ?
Gd1 O9 2.2861(19) . ?
Gd1 O11 2.345(2) . ?
Gd1 O5 2.725(2) . ?
Gd1 O4 2.3525(19) . ?
Gd1 O8 2.3271(19) . ?
Gd1 O10 2.3190(19) . ?
Gd1 O7 2.755(2) . ?
Gd1 O1 2.664(2) . ?
Ni1 O2 2.035(2) . ?
Ni1 O4 2.009(2) . ?
Ni1 O7 2.053(2) . ?
Ni1 O6 2.044(2) . ?
Ni1 N2 2.022(2) . ?
Ni1 N1 2.048(3) . ?
Cl3 C67 1.734(4) . ?
Cl4 C67 1.754(4) . ?
Cl2 C66 1.739(5) . ?
O2 C19 1.323(3) . ?
Cl1 C66 1.757(4) . ?
O9 C51 1.278(3) . ?
O11 C38 1.263(3) . ?
O5 C1 1.429(3) . ?
O5 C8 1.378(3) . ?
O4 C7 1.309(3) . ?
O8 C53 1.274(3) . ?
O10 C36 1.272(3) . ?
O7 C21 1.275(4) . ?
O1 C18 1.378(3) . ?
O1 C20 1.424(3) . ?
O6 C23 1.277(4) . ?
O3 H3 0.8200 . ?
O3 C11 1.417(4) . ?
N2 C13 1.278(4) . ?
N2 C12 1.470(4) . ?
C60 C61 1.388(4) . ?
C60 C53 1.503(4) . ?
C60 C65 1.390(4) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C51 1.400(4) . ?
C52 C53 1.404(4) . ?
C18 C19 1.412(4) . ?
C18 C17 1.372(4) . ?
C45 C50 1.397(4) . ?
C45 C46 1.394(4) . ?
C45 C38 1.495(4) . ?
C24 C21 1.491(4) . ?
C24 C29 1.394(4) . ?
C24 C25 1.388(4) . ?
N1 C9 1.281(4) . ?
N1 C10 1.471(4) . ?
C43 H43 0.9300 . ?
C43 C42 1.382(5) . ?
C43 C44 1.392(4) . ?
C7 C6 1.405(4) . ?
C7 C8 1.424(4) . ?
C54 C51 1.497(4) . ?
C54 C59 1.398(4) . ?
C54 C55 1.393(4) . ?
C19 C14 1.408(4) . ?
C62 H62 0.9300 . ?
C62 C63 1.384(4) . ?
C62 C61 1.387(4) . ?
C63 H63 0.9300 . ?
C63 C64 1.380(5) . ?
C39 C44 1.395(4) . ?
C39 C36 1.503(4) . ?
C39 C40 1.396(4) . ?
C42 H42 0.9300 . ?
C42 C41 1.383(5) . ?
C58 H58 0.9300 . ?
C58 C59 1.385(4) . ?
C58 C57 1.394(4) . ?
C56 H56 0.9300 . ?
C56 C55 1.387(4) . ?
C56 C57 1.384(4) . ?
C59 H59 0.9300 . ?
C49 H49 0.9300 . ?
C49 C50 1.386(4) . ?
C49 C48 1.382(4) . ?
C61 H61 0.9300 . ?
C44 H44 0.9300 . ?
C33 H33 0.9300 . ?
C33 C32 1.363(7) . ?
C33 C34 1.387(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.396(4) . ?
C28 C27 1.384(5) . ?
C50 H50 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.455(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.402(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C65 H65 0.9300 . ?
C65 C64 1.390(4) . ?
C32 H32 0.9300 . ?
C32 C31 1.388(5) . ?
C6 C5 1.416(4) . ?
C6 C9 1.457(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.374(5) . ?
C15 C14 1.407(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C5 H5 0.9300 . ?
C5 C4 1.368(5) . ?
C30 C23 1.505(4) . ?
C30 C35 1.391(5) . ?
C30 C31 1.392(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.401(5) . ?
C36 C37 1.397(4) . ?
C16 H16 0.9300 . ?
C55 H55 0.9300 . ?
C23 C22 1.400(4) . ?
C21 C22 1.405(4) . ?
C11 H11 0.9800 . ?
C11 C12 1.551(5) . ?
C11 C10 1.522(5) . ?
C57 H57 0.9300 . ?
C29 H29 0.9300 . ?
C46 H46 0.9300 . ?
C46 C47 1.391(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C38 C37 1.413(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C9 H9 0.9300 . ?
C8 C3 1.373(4) . ?
C64 H64 0.9300 . ?
C35 H35 0.9300 . ?
C35 C34 1.398(5) . ?
C3 H3A 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.400(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C40 H40 0.9300 . ?
C40 C41 1.390(4) . ?
C41 H41 0.9300 . ?
C47 H47 0.9300 . ?
C47 C48 1.388(4) . ?
C31 H31 0.9300 . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C26 1.380(6) . ?
C48 H48 0.9300 . ?
C26 H26 0.9300 . ?
C34 H34 0.9300 . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?

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 Gd1 Ni1 37.62(5) . . ?
O2 Gd1 O5 121.70(6) . . ?
O2 Gd1 O7 60.45(6) . . ?
O2 Gd1 O1 59.52(6) . . ?
O9 Gd1 Ni1 110.28(5) . . ?
O9 Gd1 O2 94.86(7) . . ?
O9 Gd1 O11 129.43(7) . . ?
O9 Gd1 O5 142.20(6) . . ?
O9 Gd1 O4 142.68(7) . . ?
O9 Gd1 O8 73.29(7) . . ?
O9 Gd1 O10 80.10(7) . . ?
O9 Gd1 O7 79.92(7) . . ?
O9 Gd1 O1 66.97(7) . . ?
O11 Gd1 Ni1 98.17(5) . . ?
O11 Gd1 O2 82.82(7) . . ?
O11 Gd1 O5 69.82(7) . . ?
O11 Gd1 O4 82.36(7) . . ?
O11 Gd1 O7 136.26(6) . . ?
O11 Gd1 O1 68.78(6) . . ?
O5 Gd1 Ni1 95.77(4) . . ?
O5 Gd1 O7 108.42(6) . . ?
O4 Gd1 Ni1 36.82(5) . . ?
O4 Gd1 O2 67.17(7) . . ?
O4 Gd1 O5 59.10(6) . . ?
O4 Gd1 O7 62.76(6) . . ?
O4 Gd1 O1 121.24(6) . . ?
O8 Gd1 Ni1 106.54(5) . . ?
O8 Gd1 O2 136.43(7) . . ?
O8 Gd1 O11 137.17(7) . . ?
O8 Gd1 O5 73.29(7) . . ?
O8 Gd1 O4 96.91(7) . . ?
O8 Gd1 O7 76.10(6) . . ?
O8 Gd1 O1 138.81(6) . . ?
O10 Gd1 Ni1 169.32(5) . . ?
O10 Gd1 O2 142.11(7) . . ?
O10 Gd1 O11 72.51(7) . . ?
O10 Gd1 O5 76.33(7) . . ?
O10 Gd1 O4 134.24(7) . . ?
O10 Gd1 O8 78.35(7) . . ?
O10 Gd1 O7 151.15(6) . . ?
O10 Gd1 O1 84.53(7) . . ?
O7 Gd1 Ni1 38.17(4) . . ?
O1 Gd1 Ni1 97.09(4) . . ?
O1 Gd1 O5 137.93(6) . . ?
O1 Gd1 O7 106.33(6) . . ?
O2 Ni1 Gd1 46.11(5) . . ?
O2 Ni1 O7 79.50(8) . . ?
O2 Ni1 O6 168.06(8) . . ?
O2 Ni1 N1 102.45(9) . . ?
O4 Ni1 Gd1 44.58(5) . . ?
O4 Ni1 O2 81.17(8) . . ?
O4 Ni1 O7 82.63(8) . . ?
O4 Ni1 O6 94.00(8) . . ?
O4 Ni1 N2 170.31(10) . . ?
O4 Ni1 N1 90.25(9) . . ?
O7 Ni1 Gd1 56.02(6) . . ?
O6 Ni1 Gd1 123.80(6) . . ?
O6 Ni1 O7 89.08(8) . . ?
O6 Ni1 N1 88.42(9) . . ?
N2 Ni1 Gd1 128.87(7) . . ?
N2 Ni1 O2 89.62(9) . . ?
N2 Ni1 O7 98.71(9) . . ?
N2 Ni1 O6 95.61(10) . . ?
N2 Ni1 N1 88.81(10) . . ?
N1 Ni1 Gd1 120.09(7) . . ?
N1 Ni1 O7 172.27(9) . . ?
Ni1 O2 Gd1 96.27(7) . . ?
C19 O2 Gd1 117.02(16) . . ?
C19 O2 Ni1 125.52(18) . . ?
C51 O9 Gd1 132.62(17) . . ?
C38 O11 Gd1 136.44(18) . . ?
C1 O5 Gd1 128.51(18) . . ?
C8 O5 Gd1 109.52(15) . . ?
C8 O5 C1 117.6(2) . . ?
Ni1 O4 Gd1 98.61(8) . . ?
C7 O4 Gd1 120.05(17) . . ?
C7 O4 Ni1 127.95(18) . . ?
C53 O8 Gd1 133.65(18) . . ?
C36 O10 Gd1 137.34(18) . . ?
Ni1 O7 Gd1 85.82(7) . . ?
C21 O7 Gd1 135.64(17) . . ?
C21 O7 Ni1 126.30(18) . . ?
C18 O1 Gd1 110.14(16) . . ?
C18 O1 C20 117.1(2) . . ?
C20 O1 Gd1 123.43(17) . . ?
C23 O6 Ni1 126.00(19) . . ?
C11 O3 H3 109.5 . . ?
C13 N2 Ni1 126.2(2) . . ?
C13 N2 C12 117.5(3) . . ?
C12 N2 Ni1 116.1(2) . . ?
C61 C60 C53 118.2(2) . . ?
C61 C60 C65 118.3(3) . . ?
C65 C60 C53 123.5(3) . . ?
H52A C52 H52B 106.5 . . ?
C51 C52 H52A 106.5 . . ?
C51 C52 H52B 106.5 . . ?
C51 C52 C53 123.5(3) . . ?
C53 C52 H52A 106.5 . . ?
C53 C52 H52B 106.5 . . ?
O1 C18 C19 111.9(2) . . ?
C17 C18 O1 126.0(3) . . ?
C17 C18 C19 122.1(3) . . ?
C50 C45 C46 118.7(3) . . ?
C50 C45 C38 118.5(3) . . ?
C46 C45 C38 122.7(3) . . ?
C29 C24 C21 118.4(3) . . ?
C25 C24 C21 122.3(3) . . ?
C25 C24 C29 119.3(3) . . ?
C9 N1 Ni1 125.6(2) . . ?
C9 N1 C10 117.2(3) . . ?
C10 N1 Ni1 117.0(2) . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 119.9(3) . . ?
C44 C43 H43 120.0 . . ?
O4 C7 C6 125.2(3) . . ?
O4 C7 C8 116.2(2) . . ?
C6 C7 C8 118.5(3) . . ?
C59 C54 C51 118.2(2) . . ?
C55 C54 C51 123.0(3) . . ?
C55 C54 C59 118.7(3) . . ?
O2 C19 C18 116.8(2) . . ?
O2 C19 C14 124.9(3) . . ?
C14 C19 C18 118.3(3) . . ?
C63 C62 H62 120.0 . . ?
C63 C62 C61 120.0(3) . . ?
C61 C62 H62 120.0 . . ?
O9 C51 C52 124.1(3) . . ?
O9 C51 C54 115.3(2) . . ?
C52 C51 C54 120.6(2) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 C62 119.7(3) . . ?
C64 C63 H63 120.1 . . ?
C44 C39 C36 122.9(3) . . ?
C40 C39 C44 118.6(3) . . ?
C40 C39 C36 118.5(3) . . ?
C43 C42 H42 119.9 . . ?
C43 C42 C41 120.3(3) . . ?
C41 C42 H42 119.9 . . ?
C59 C58 H58 119.9 . . ?
C59 C58 C57 120.2(3) . . ?
C57 C58 H58 119.9 . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C57 C56 C55 120.3(3) . . ?
C54 C59 H59 119.7 . . ?
C58 C59 C54 120.6(3) . . ?
C58 C59 H59 119.7 . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.3(3) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 C60 121.1(3) . . ?
C62 C61 H61 119.5 . . ?
C43 C44 C39 120.7(3) . . ?
C43 C44 H44 119.7 . . ?
C39 C44 H44 119.7 . . ?
O8 C53 C60 115.8(2) . . ?
O8 C53 C52 124.4(3) . . ?
C52 C53 C60 119.8(2) . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.5(4) . . ?
C34 C33 H33 119.7 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.1(3) . . ?
C45 C50 H50 119.6 . . ?
C49 C50 C45 120.8(3) . . ?
C49 C50 H50 119.6 . . ?
N2 C13 H13 116.6 . . ?
N2 C13 C14 126.7(3) . . ?
C14 C13 H13 116.6 . . ?
C18 C17 H17 120.4 . . ?
C18 C17 C16 119.1(3) . . ?
C16 C17 H17 120.4 . . ?
O5 C1 H1A 109.5 . . ?
O5 C1 H1B 109.5 . . ?
O5 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C60 C65 H65 119.6 . . ?
C60 C65 C64 120.9(3) . . ?
C64 C65 H65 119.6 . . ?
C33 C32 H32 119.8 . . ?
C33 C32 C31 120.5(4) . . ?
C31 C32 H32 119.8 . . ?
C7 C6 C5 118.9(3) . . ?
C7 C6 C9 123.6(3) . . ?
C5 C6 C9 117.4(3) . . ?
C16 C15 H15 119.3 . . ?
C16 C15 C14 121.5(3) . . ?
C14 C15 H15 119.3 . . ?
O1 C20 H20A 109.5 . . ?
O1 C20 H20B 109.5 . . ?
O1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C6 C5 H5 119.5 . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C35 C30 C23 119.1(3) . . ?
C35 C30 C31 118.6(3) . . ?
C31 C30 C23 122.2(3) . . ?
C5 C4 H4 119.6 . . ?
C5 C4 C3 120.8(3) . . ?
C3 C4 H4 119.6 . . ?
O10 C36 C39 115.8(2) . . ?
O10 C36 C37 124.2(3) . . ?
C37 C36 C39 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 C17 120.0(3) . . ?
C15 C16 H16 120.0 . . ?
C54 C55 H55 119.6 . . ?
C56 C55 C54 120.7(3) . . ?
C56 C55 H55 119.6 . . ?
O6 C23 C30 115.2(3) . . ?
O6 C23 C22 125.5(3) . . ?
C22 C23 C30 119.2(3) . . ?
O7 C21 C24 116.1(2) . . ?
O7 C21 C22 124.9(3) . . ?
C22 C21 C24 119.0(3) . . ?
O3 C11 H11 106.3 . . ?
O3 C11 C12 112.0(3) . . ?
O3 C11 C10 110.7(3) . . ?
C12 C11 H11 106.3 . . ?
C10 C11 H11 106.3 . . ?
C10 C11 C12 114.7(3) . . ?
C58 C57 H57 120.2 . . ?
C56 C57 C58 119.5(3) . . ?
C56 C57 H57 120.2 . . ?
C24 C29 C28 120.2(3) . . ?
C24 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 120.0(3) . . ?
C47 C46 H46 120.0 . . ?
N2 C12 C11 112.2(3) . . ?
N2 C12 H12A 109.2 . . ?
N2 C12 H12B 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O11 C38 C45 116.4(2) . . ?
O11 C38 C37 124.9(3) . . ?
C37 C38 C45 118.6(2) . . ?
C36 C37 C38 123.5(3) . . ?
C36 C37 H37A 106.4 . . ?
C36 C37 H37B 106.4 . . ?
C38 C37 H37A 106.4 . . ?
C38 C37 H37B 106.4 . . ?
H37A C37 H37B 106.5 . . ?
C19 C14 C13 122.9(3) . . ?
C15 C14 C19 118.9(3) . . ?
C15 C14 C13 118.0(3) . . ?
N1 C9 C6 126.6(3) . . ?
N1 C9 H9 116.7 . . ?
C6 C9 H9 116.7 . . ?
O5 C8 C7 112.1(2) . . ?
C3 C8 O5 126.4(3) . . ?
C3 C8 C7 121.5(3) . . ?
C63 C64 C65 120.1(3) . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
C30 C35 H35 119.6 . . ?
C30 C35 C34 120.7(4) . . ?
C34 C35 H35 119.6 . . ?
C4 C3 H3A 120.4 . . ?
C8 C3 C4 119.2(3) . . ?
C8 C3 H3A 120.4 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.3(3) . . ?
C26 C25 H25 119.9 . . ?
C23 C22 C21 126.3(3) . . ?
C23 C22 H22A 105.7 . . ?
C23 C22 H22B 105.7 . . ?
C21 C22 H22A 105.7 . . ?
C21 C22 H22B 105.7 . . ?
H22A C22 H22B 106.2 . . ?
C39 C40 H40 119.7 . . ?
C41 C40 C39 120.7(3) . . ?
C41 C40 H40 119.7 . . ?
C42 C41 C40 119.9(3) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C46 C47 H47 119.6 . . ?
C48 C47 C46 120.8(3) . . ?
C48 C47 H47 119.6 . . ?
C32 C31 C30 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
Cl2 C66 Cl1 112.3(2) . . ?
Cl2 C66 H66A 109.1 . . ?
Cl2 C66 H66B 109.1 . . ?
Cl1 C66 H66A 109.1 . . ?
Cl1 C66 H66B 109.1 . . ?
H66A C66 H66B 107.9 . . ?
N1 C10 C11 111.9(3) . . ?
N1 C10 H10A 109.2 . . ?
N1 C10 H10B 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C28 C27 H27 119.9 . . ?
C26 C27 C28 120.1(3) . . ?
C26 C27 H27 119.9 . . ?
C49 C48 C47 119.4(3) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.3 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.0(3) . . ?
C27 C26 H26 120.0 . . ?
C33 C34 C35 119.2(4) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
Cl3 C67 Cl4 111.8(2) . . ?
Cl3 C67 H67A 109.3 . . ?
Cl3 C67 H67B 109.3 . . ?
Cl4 C67 H67A 109.3 . . ?
Cl4 C67 H67B 109.3 . . ?
H67A C67 H67B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O6 0.82 1.92 2.706(3) 159.0 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O2 C19 C18 -42.7(3) . . . . ?
Gd1 O2 C19 C14 138.3(3) . . . . ?
Gd1 O9 C51 C52 28.9(4) . . . . ?
Gd1 O9 C51 C54 -152.80(19) . . . . ?
Gd1 O11 C38 C45 -171.01(17) . . . . ?
Gd1 O11 C38 C37 5.2(4) . . . . ?
Gd1 O5 C8 C7 28.2(3) . . . . ?
Gd1 O5 C8 C3 -150.5(3) . . . . ?
Gd1 O4 C7 C6 134.0(2) . . . . ?
Gd1 O4 C7 C8 -45.3(3) . . . . ?
Gd1 O8 C53 C60 173.05(17) . . . . ?
Gd1 O8 C53 C52 -7.7(4) . . . . ?
Gd1 O10 C36 C39 163.40(19) . . . . ?
Gd1 O10 C36 C37 -14.1(4) . . . . ?
Gd1 O7 C21 C24 -65.5(3) . . . . ?
Gd1 O7 C21 C22 118.1(3) . . . . ?
Gd1 O1 C18 C19 32.7(3) . . . . ?
Gd1 O1 C18 C17 -146.8(3) . . . . ?
Ni1 O2 C19 C18 -163.65(19) . . . . ?
Ni1 O2 C19 C14 17.3(4) . . . . ?
Ni1 O4 C7 C6 1.9(4) . . . . ?
Ni1 O4 C7 C8 -177.38(18) . . . . ?
Ni1 O7 C21 C24 166.01(18) . . . . ?
Ni1 O7 C21 C22 -10.3(4) . . . . ?
Ni1 O6 C23 C30 -168.13(18) . . . . ?
Ni1 O6 C23 C22 10.8(4) . . . . ?
Ni1 N2 C13 C14 -0.4(5) . . . . ?
Ni1 N2 C12 C11 51.3(3) . . . . ?
Ni1 N1 C9 C6 8.5(4) . . . . ?
Ni1 N1 C10 C11 49.6(3) . . . . ?
O2 C19 C14 C13 2.5(5) . . . . ?
O2 C19 C14 C15 177.6(3) . . . . ?
O11 C38 C37 C36 -2.4(5) . . . . ?
O5 C8 C3 C4 176.1(3) . . . . ?
O4 C7 C6 C5 178.1(3) . . . . ?
O4 C7 C6 C9 -6.0(4) . . . . ?
O4 C7 C8 O5 4.6(3) . . . . ?
O4 C7 C8 C3 -176.6(3) . . . . ?
O10 C36 C37 C38 6.5(5) . . . . ?
O7 C21 C22 C23 1.3(5) . . . . ?
O1 C18 C19 O2 2.0(4) . . . . ?
O1 C18 C19 C14 -178.9(3) . . . . ?
O1 C18 C17 C16 179.7(3) . . . . ?
O6 C23 C22 C21 -1.6(5) . . . . ?
O3 C11 C12 N2 -110.5(3) . . . . ?
O3 C11 C10 N1 55.8(3) . . . . ?
N2 C13 C14 C19 -12.0(6) . . . . ?
N2 C13 C14 C15 172.9(3) . . . . ?
C60 C65 C64 C63 0.2(5) . . . . ?
C18 C19 C14 C13 -176.5(3) . . . . ?
C18 C19 C14 C15 -1.4(5) . . . . ?
C18 C17 C16 C15 -0.3(5) . . . . ?
C45 C46 C47 C48 1.1(5) . . . . ?
C45 C38 C37 C36 173.7(3) . . . . ?
C24 C21 C22 C23 -174.9(3) . . . . ?
C24 C25 C26 C27 -1.7(5) . . . . ?
C43 C42 C41 C40 0.7(5) . . . . ?
C7 C6 C5 C4 -0.3(4) . . . . ?
C7 C6 C9 N1 0.3(5) . . . . ?
C7 C8 C3 C4 -2.5(4) . . . . ?
C19 C18 C17 C16 0.3(5) . . . . ?
C62 C63 C64 C65 -1.1(5) . . . . ?
C51 C52 C53 O8 -11.0(5) . . . . ?
C51 C52 C53 C60 168.2(3) . . . . ?
C51 C54 C59 C58 176.6(3) . . . . ?
C51 C54 C55 C56 -175.8(3) . . . . ?
C63 C62 C61 C60 0.5(5) . . . . ?
C39 C36 C37 C38 -170.9(3) . . . . ?
C39 C40 C41 C42 -1.1(5) . . . . ?
C42 C43 C44 C39 -0.2(5) . . . . ?
C59 C54 C51 O9 -20.9(4) . . . . ?
C59 C54 C51 C52 157.5(3) . . . . ?
C59 C54 C55 C56 1.0(4) . . . . ?
C59 C58 C57 C56 0.6(4) . . . . ?
C61 C60 C53 O8 -9.3(4) . . . . ?
C61 C60 C53 C52 171.4(3) . . . . ?
C61 C60 C65 C64 1.1(5) . . . . ?
C61 C62 C63 C64 0.8(5) . . . . ?
C44 C43 C42 C41 -0.1(5) . . . . ?
C44 C39 C36 O10 163.3(3) . . . . ?
C44 C39 C36 C37 -19.0(4) . . . . ?
C44 C39 C40 C41 0.8(4) . . . . ?
C53 C60 C61 C62 176.7(3) . . . . ?
C53 C60 C65 C64 -177.0(3) . . . . ?
C53 C52 C51 O9 0.8(5) . . . . ?
C53 C52 C51 C54 -177.4(3) . . . . ?
C33 C32 C31 C30 -1.5(6) . . . . ?
C28 C27 C26 C25 0.9(6) . . . . ?
C50 C45 C46 C47 0.0(4) . . . . ?
C50 C45 C38 O11 27.7(4) . . . . ?
C50 C45 C38 C37 -148.8(3) . . . . ?
C50 C49 C48 C47 -0.3(5) . . . . ?
C13 N2 C12 C11 -124.1(3) . . . . ?
C17 C18 C19 O2 -178.5(3) . . . . ?
C17 C18 C19 C14 0.6(4) . . . . ?
C1 O5 C8 C7 -173.4(2) . . . . ?
C1 O5 C8 C3 8.0(4) . . . . ?
C65 C60 C61 C62 -1.4(5) . . . . ?
C65 C60 C53 O8 168.8(3) . . . . ?
C65 C60 C53 C52 -10.5(4) . . . . ?
C32 C33 C34 C35 -0.1(6) . . . . ?
C6 C7 C8 O5 -174.8(2) . . . . ?
C6 C7 C8 C3 4.0(4) . . . . ?
C6 C5 C4 C3 1.8(5) . . . . ?
C20 O1 C18 C19 -179.5(2) . . . . ?
C20 O1 C18 C17 1.1(4) . . . . ?
C5 C6 C9 N1 176.2(3) . . . . ?
C5 C4 C3 C8 -0.4(5) . . . . ?
C30 C23 C22 C21 177.3(3) . . . . ?
C30 C35 C34 C33 -1.0(5) . . . . ?
C36 C39 C44 C43 -179.3(3) . . . . ?
C36 C39 C40 C41 180.0(3) . . . . ?
C16 C15 C14 C19 1.4(5) . . . . ?
C16 C15 C14 C13 176.8(3) . . . . ?
C55 C54 C51 O9 155.9(3) . . . . ?
C55 C54 C51 C52 -25.8(4) . . . . ?
C55 C54 C59 C58 -0.3(4) . . . . ?
C55 C56 C57 C58 0.1(5) . . . . ?
C23 C30 C35 C34 179.0(3) . . . . ?
C23 C30 C31 C32 -177.7(3) . . . . ?
C21 C24 C29 C28 -177.8(3) . . . . ?
C21 C24 C25 C26 179.8(3) . . . . ?
C57 C58 C59 C54 -0.5(4) . . . . ?
C57 C56 C55 C54 -0.9(5) . . . . ?
C29 C24 C21 O7 -33.6(4) . . . . ?
C29 C24 C21 C22 142.9(3) . . . . ?
C29 C24 C25 C26 0.6(5) . . . . ?
C29 C28 C27 C26 1.1(5) . . . . ?
C46 C45 C50 C49 -1.2(4) . . . . ?
C46 C45 C38 O11 -153.8(3) . . . . ?
C46 C45 C38 C37 29.7(4) . . . . ?
C46 C47 C48 C49 -1.0(5) . . . . ?
C12 N2 C13 C14 174.5(3) . . . . ?
C12 C11 C10 N1 -72.1(4) . . . . ?
C38 C45 C50 C49 177.3(3) . . . . ?
C38 C45 C46 C47 -178.5(3) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C9 N1 C10 C11 -124.2(3) . . . . ?
C9 C6 C5 C4 -176.3(3) . . . . ?
C8 C7 C6 C5 -2.5(4) . . . . ?
C8 C7 C6 C9 173.3(3) . . . . ?
C35 C30 C23 O6 -27.4(4) . . . . ?
C35 C30 C23 C22 153.6(3) . . . . ?
C35 C30 C31 C32 0.4(5) . . . . ?
C25 C24 C21 O7 147.2(3) . . . . ?
C25 C24 C21 C22 -36.3(4) . . . . ?
C25 C24 C29 C28 1.4(5) . . . . ?
C40 C39 C44 C43 -0.1(4) . . . . ?
C40 C39 C36 O10 -15.8(4) . . . . ?
C40 C39 C36 C37 161.8(3) . . . . ?
C31 C30 C23 O6 150.7(3) . . . . ?
C31 C30 C23 C22 -28.3(4) . . . . ?
C31 C30 C35 C34 0.8(5) . . . . ?
C10 N1 C9 C6 -178.4(3) . . . . ?
C10 C11 C12 N2 16.8(4) . . . . ?
C27 C28 C29 C24 -2.3(5) . . . . ?
C48 C49 C50 C45 1.4(4) . . . . ?
C34 C33 C32 C31 1.3(6) . . . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_eu
_audit_block_doi                 10.5517/ccdc.csd.cc1p7ldx
_database_code_depnum_ccdc_archive 'CCDC 1556429'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H24 Eu F15 N2 Ni O12'
_chemical_formula_sum            'C31 H24 Eu F15 N2 Ni O12'
_chemical_formula_weight         1112.19
_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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.242(2)
_cell_length_b                   12.6901(14)
_cell_length_c                   16.6310(19)
_cell_angle_alpha                90
_cell_angle_beta                 97.744(2)
_cell_angle_gamma                90
_cell_volume                     3814.8(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12184
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   0.681
_exptl_transmission_factor_min   0.658
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32455
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         3.034
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6145
_reflns_number_total             6759
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.0021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²+33.7660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2775
_refine_ls_wR_factor_ref         0.2836
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, H24 of C24, H5 of C5, H29 of C29, H10 of C10, {H11A,H11B} of C11,
  H6 of C6, {H9A,H9B} of C9, H14 of C14, H15 of C15, H12 of C12, H16 of C16, H8
  of C8
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H19A,H19B,H19C} of C19, {H12A,H12B} of O12, H3 of O3
2. Rigid bond restraints
 F1, C21
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3.a Rotating group:
 O12(H12A,H12B)
3.b Ternary CH refined with riding coordinates:
 C10(H10)
3.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B)
3.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C12(H12), C16(H16), C8(H8), C4(H4), C24(H24), C5(H5),
 C29(H29), C6(H6)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C)
3.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.26883(3) 0.50218(4) 0.13371(3) 0.0349(3) Uani 1 1 d . . . . .
Ni1 Ni 0.11112(7) 0.50709(9) 0.22684(8) 0.0310(4) Uani 1 1 d . . . . .
F2 F 0.1339(6) 0.8535(9) 0.0742(6) 0.107(4) Uani 1 1 d . . . . .
F1 F 0.1128(6) 0.8706(8) 0.1967(7) 0.108(3) Uani 1 1 d . U . . .
F15 F 0.3177(6) 0.0616(6) 0.1998(6) 0.094(3) Uani 1 1 d . . . . .
F3 F 0.2223(6) 0.8757(7) 0.1670(7) 0.106(3) Uani 1 1 d . . . . .
F6 F 0.2866(4) 0.7486(5) -0.1558(4) 0.0619(19) Uani 1 1 d . . . . .
F14 F 0.2288(4) 0.1402(5) 0.2455(5) 0.065(2) Uani 1 1 d . . . . .
F4 F 0.1808(4) 0.7099(8) -0.1180(5) 0.086(3) Uani 1 1 d . . . . .
F8 F 0.3967(5) 0.8468(8) 0.1798(6) 0.089(3) Uani 1 1 d . . . . .
F7 F 0.4487(3) 0.8574(6) 0.0721(4) 0.062(2) Uani 1 1 d . . . . .
F13 F 0.3354(5) 0.1478(8) 0.3100(5) 0.087(3) Uani 1 1 d . . . . .
F9 F 0.4861(3) 0.7490(5) 0.1623(5) 0.063(2) Uani 1 1 d . . . . .
F5 F 0.2439(6) 0.5897(6) -0.1601(4) 0.089(3) Uani 1 1 d . . . . .
F11 F 0.5103(6) 0.2208(8) 0.0919(7) 0.108(4) Uani 1 1 d . . . . .
F12 F 0.4715(5) 0.3337(9) 0.0013(5) 0.095(3) Uani 1 1 d . . . . .
F10 F 0.5290(5) 0.3853(11) 0.1125(7) 0.114(4) Uani 1 1 d . . . . .
O8 O 0.2602(4) 0.5735(5) -0.0002(4) 0.0351(15) Uani 1 1 d . . . . .
O4 O 0.2207(4) 0.5145(4) 0.2586(4) 0.0277(14) Uani 1 1 d . . . . .
O1 O 0.2157(4) 0.3662(5) 0.0223(4) 0.0350(14) Uani 1 1 d . . . . .
O2 O 0.1417(3) 0.4710(4) 0.1176(4) 0.0266(13) Uani 1 1 d . . . . .
O5 O 0.3614(4) 0.4918(5) 0.2676(5) 0.0371(16) Uani 1 1 d . . . . .
O6 O 0.2120(4) 0.6734(6) 0.1367(5) 0.0468(18) Uani 1 1 d . . . . .
O11 O 0.2701(4) 0.3192(5) 0.1886(4) 0.0352(14) Uani 1 1 d . . . . .
O12 O 0.1212(4) 0.3404(5) 0.2568(4) 0.0367(15) Uani 1 1 d . . . . .
H12A H 0.1620 0.3156 0.2442 0.055 Uiso 1 1 d R U . . .
H12B H 0.0850 0.3065 0.2300 0.055 Uiso 1 1 d R U . . .
O9 O 0.3603(4) 0.6371(5) 0.1328(4) 0.0393(16) Uani 1 1 d . . . . .
O7 O 0.1123(4) 0.6677(5) 0.2022(4) 0.0335(14) Uani 1 1 d . . . . .
O3 O -0.0024(5) 0.7105(8) 0.2870(7) 0.074(3) Uani 1 1 d . . . . .
H3 H 0.0379 0.7049 0.2709 0.111 Uiso 1 1 calc R U . . .
O10 O 0.3748(4) 0.4128(6) 0.0982(4) 0.0450(17) Uani 1 1 d . . . . .
N2 N 0.0925(5) 0.5294(7) 0.3427(5) 0.0385(19) Uani 1 1 d . . . . .
N1 N 0.0030(5) 0.5014(6) 0.1798(6) 0.041(2) Uani 1 1 d . . . . .
C14 C 0.2635(7) 0.4770(8) 0.4774(7) 0.043(2) Uani 1 1 d . . . . .
H14 H 0.2409 0.4740 0.5242 0.052 Uiso 1 1 calc R U . . .
C20 C 0.1605(6) 0.7109(8) 0.1663(6) 0.039(2) Uani 1 1 d . . . . .
C21 C 0.1535(7) 0.8238(8) 0.1564(7) 0.052(3) Uani 1 1 d . U . . .
C15 C 0.3394(6) 0.4618(9) 0.4833(6) 0.046(3) Uani 1 1 d . . . . .
H15 H 0.3668 0.4481 0.5335 0.055 Uiso 1 1 calc R U . . .
C12 C 0.1437(7) 0.5172(7) 0.4033(6) 0.038(2) Uani 1 1 d . . . . .
H12 H 0.1283 0.5227 0.4542 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1406(5) 0.3435(7) 0.0140(5) 0.033(2) Uani 1 1 d . . . . .
C18 C 0.2558(6) 0.4987(6) 0.3313(7) 0.034(2) Uani 1 1 d . . . . .
C23 C 0.2860(5) 0.6552(7) -0.0294(6) 0.0317(19) Uani 1 1 d . . . . .
C2 C 0.1020(5) 0.4041(6) 0.0678(5) 0.0285(18) Uani 1 1 d . . . . .
C30 C 0.3157(6) 0.2467(8) 0.1902(5) 0.039(2) Uani 1 1 d . . . . .
C16 C 0.3746(6) 0.4670(8) 0.4137(6) 0.043(2) Uani 1 1 d . . . . .
H16 H 0.4256 0.4580 0.4177 0.052 Uiso 1 1 calc R U . . .
C25 C 0.3699(5) 0.7110(7) 0.0871(6) 0.0309(19) Uani 1 1 d . . . . .
C8 C -0.0210(5) 0.4452(7) 0.1159(5) 0.033(2) Uani 1 1 d . . . . .
H8 H -0.0720 0.4393 0.1020 0.039 Uiso 1 1 calc R U . . .
C31 C 0.2997(6) 0.1458(8) 0.2356(7) 0.046(3) Uani 1 1 d . . . . .
C22 C 0.2495(8) 0.6759(9) -0.1177(7) 0.054(3) Uani 1 1 d . . . . .
C4 C 0.1038(6) 0.2723(7) -0.0401(6) 0.039(2) Uani 1 1 d . . . . .
H4 H 0.1291 0.2328 -0.0746 0.047 Uiso 1 1 calc R U . . .
C24 C 0.3362(5) 0.7246(8) 0.0076(6) 0.035(2) Uani 1 1 d . . . . .
H24 H 0.3486 0.7833 -0.0213 0.042 Uiso 1 1 calc R U . . .
C5 C 0.0273(7) 0.2613(9) -0.0414(7) 0.052(3) Uani 1 1 d . . . . .
H5 H 0.0021 0.2134 -0.0775 0.062 Uiso 1 1 calc R U . . .
C26 C 0.4259(5) 0.7935(8) 0.1265(7) 0.040(2) Uani 1 1 d . . . . .
C13 C 0.2205(7) 0.4967(7) 0.4037(7) 0.040(3) Uani 1 1 d . . . . .
C7 C 0.0263(5) 0.3906(6) 0.0641(6) 0.033(2) Uani 1 1 d . . . . .
C29 C 0.3835(6) 0.2468(10) 0.1591(7) 0.049(3) Uani 1 1 d . . . . .
H29 H 0.4146 0.1887 0.1686 0.059 Uiso 1 1 calc R U . . .
C27 C 0.4819(7) 0.3226(12) 0.0798(8) 0.060(3) Uani 1 1 d . . . . .
C1 C 0.2513(6) 0.3344(9) -0.0452(6) 0.044(2) Uani 1 1 d . . . . .
H1A H 0.2973 0.3713 -0.0439 0.067 Uiso 1 1 calc R U . . .
H1B H 0.2199 0.3505 -0.0947 0.067 Uiso 1 1 calc R U . . .
H1C H 0.2604 0.2599 -0.0423 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3330(6) 0.4857(7) 0.3383(7) 0.036(2) Uani 1 1 d . . . . .
C19 C 0.4403(6) 0.5087(9) 0.2716(8) 0.051(3) Uani 1 1 d . . . . .
H19A H 0.4659 0.4433 0.2837 0.076 Uiso 1 1 calc R U . . .
H19B H 0.4562 0.5591 0.3134 0.076 Uiso 1 1 calc R U . . .
H19C H 0.4511 0.5350 0.2204 0.076 Uiso 1 1 calc R U . . .
C10 C -0.0326(6) 0.6082(9) 0.2967(7) 0.050(3) Uani 1 1 d . . . . .
H10 H -0.0787 0.6203 0.3196 0.060 Uiso 1 1 calc R U . . .
C11 C 0.0171(6) 0.5445(10) 0.3613(6) 0.045(2) Uani 1 1 d . . . . .
H11A H 0.0193 0.5803 0.4130 0.054 Uiso 1 1 calc R U . . .
H11B H -0.0052 0.4759 0.3668 0.054 Uiso 1 1 calc R U . . .
C6 C -0.0116(7) 0.3175(10) 0.0078(6) 0.049(3) Uani 1 1 d . . . . .
H6 H -0.0625 0.3086 0.0049 0.059 Uiso 1 1 calc R U . . .
C28 C 0.4054(6) 0.3292(11) 0.1154(7) 0.049(3) Uani 1 1 d . . . . .
C9 C -0.0554(5) 0.5554(11) 0.2166(7) 0.052(3) Uani 1 1 d . . . . .
H9A H -0.0935 0.5043 0.2235 0.062 Uiso 1 1 calc R U . . .
H9B H -0.0774 0.6081 0.1786 0.062 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Ni1 3.4469(14) . ?
Eu1 O8 2.390(6) . ?
Eu1 O4 2.367(7) . ?
Eu1 O1 2.620(6) . ?
Eu1 O2 2.332(6) . ?
Eu1 O5 2.610(7) . ?
Eu1 O6 2.411(8) . ?
Eu1 O11 2.494(6) . ?
Eu1 O9 2.392(7) . ?
Eu1 O10 2.383(7) . ?
Ni1 O4 1.999(7) . ?
Ni1 O2 2.023(6) . ?
Ni1 O12 2.175(7) . ?
Ni1 O7 2.079(6) . ?
Ni1 N2 2.021(9) . ?
Ni1 N1 2.022(10) . ?
F2 C21 1.417(14) . ?
F1 C21 1.221(16) . ?
F15 C31 1.287(13) . ?
F3 C21 1.406(15) . ?
F6 C22 1.351(13) . ?
F14 C31 1.328(13) . ?
F4 C22 1.325(15) . ?
F8 C26 1.285(13) . ?
F7 C26 1.323(12) . ?
F13 C31 1.318(14) . ?
F9 C26 1.305(11) . ?
F5 C22 1.298(14) . ?
F11 C27 1.396(16) . ?
F12 C27 1.302(15) . ?
F10 C27 1.241(17) . ?
O8 C23 1.263(11) . ?
O4 C18 1.305(12) . ?
O1 C3 1.390(11) . ?
O1 C1 1.428(11) . ?
O2 C2 1.331(10) . ?
O5 C17 1.349(14) . ?
O5 C19 1.449(13) . ?
O6 C20 1.215(13) . ?
O11 C30 1.239(12) . ?
O12 H12A 0.8604 . ?
O12 H12B 0.8606 . ?
O9 C25 1.235(11) . ?
O7 C20 1.253(12) . ?
O3 H3 0.8200 . ?
O3 C10 1.427(16) . ?
O10 C28 1.216(14) . ?
N2 C12 1.288(14) . ?
N2 C11 1.463(13) . ?
N1 C8 1.306(13) . ?
N1 C9 1.467(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.387(17) . ?
C14 C13 1.385(16) . ?
C20 C21 1.446(14) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(17) . ?
C12 H12 0.9300 . ?
C12 C13 1.423(18) . ?
C3 C2 1.435(13) . ?
C3 C4 1.383(13) . ?
C18 C13 1.442(19) . ?
C18 C17 1.407(16) . ?
C23 C22 1.551(15) . ?
C23 C24 1.357(13) . ?
C2 C7 1.384(13) . ?
C30 C31 1.534(14) . ?
C30 C29 1.404(15) . ?
C16 H16 0.9300 . ?
C16 C17 1.396(14) . ?
C25 C24 1.392(13) . ?
C25 C26 1.545(12) . ?
C8 H8 0.9300 . ?
C8 C7 1.473(14) . ?
C4 H4 0.9300 . ?
C4 C5 1.400(17) . ?
C24 H24 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.356(18) . ?
C7 C6 1.430(13) . ?
C29 H29 0.9300 . ?
C29 C28 1.363(17) . ?
C27 C28 1.588(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C11 1.539(15) . ?
C10 C9 1.499(16) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C6 H6 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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
O8 Eu1 Ni1 117.26(16) . . ?
O8 Eu1 O1 67.6(2) . . ?
O8 Eu1 O5 140.2(2) . . ?
O8 Eu1 O6 72.7(2) . . ?
O8 Eu1 O11 133.6(2) . . ?
O8 Eu1 O9 71.4(2) . . ?
O4 Eu1 Ni1 34.25(16) . . ?
O4 Eu1 O8 143.8(2) . . ?
O4 Eu1 O1 121.2(2) . . ?
O4 Eu1 O5 61.9(2) . . ?
O4 Eu1 O6 73.2(2) . . ?
O4 Eu1 O11 74.1(2) . . ?
O4 Eu1 O9 107.5(2) . . ?
O4 Eu1 O10 131.2(2) . . ?
O1 Eu1 Ni1 94.49(14) . . ?
O2 Eu1 Ni1 34.64(15) . . ?
O2 Eu1 O8 91.0(2) . . ?
O2 Eu1 O4 68.3(2) . . ?
O2 Eu1 O1 62.6(2) . . ?
O2 Eu1 O5 127.4(2) . . ?
O2 Eu1 O6 74.4(2) . . ?
O2 Eu1 O11 81.0(2) . . ?
O2 Eu1 O9 143.5(2) . . ?
O2 Eu1 O10 135.9(2) . . ?
O5 Eu1 Ni1 95.76(17) . . ?
O5 Eu1 O1 134.8(2) . . ?
O6 Eu1 Ni1 65.62(18) . . ?
O6 Eu1 O1 119.3(2) . . ?
O6 Eu1 O5 105.0(2) . . ?
O6 Eu1 O11 144.5(2) . . ?
O11 Eu1 Ni1 79.58(15) . . ?
O11 Eu1 O1 68.3(2) . . ?
O11 Eu1 O5 70.6(2) . . ?
O9 Eu1 Ni1 127.96(18) . . ?
O9 Eu1 O1 131.2(2) . . ?
O9 Eu1 O5 70.7(2) . . ?
O9 Eu1 O6 70.0(2) . . ?
O9 Eu1 O11 134.2(2) . . ?
O10 Eu1 Ni1 150.93(17) . . ?
O10 Eu1 O8 84.4(2) . . ?
O10 Eu1 O1 75.3(2) . . ?
O10 Eu1 O5 74.6(2) . . ?
O10 Eu1 O6 143.1(2) . . ?
O10 Eu1 O11 71.4(2) . . ?
O10 Eu1 O9 75.5(2) . . ?
O4 Ni1 Eu1 41.80(19) . . ?
O4 Ni1 O2 82.0(3) . . ?
O4 Ni1 O12 86.3(2) . . ?
O4 Ni1 O7 88.2(2) . . ?
O4 Ni1 N2 91.8(3) . . ?
O4 Ni1 N1 172.6(3) . . ?
O2 Ni1 Eu1 40.93(17) . . ?
O2 Ni1 O12 87.7(2) . . ?
O2 Ni1 O7 91.9(2) . . ?
O12 Ni1 Eu1 92.05(18) . . ?
O7 Ni1 Eu1 84.12(19) . . ?
O7 Ni1 O12 174.5(2) . . ?
N2 Ni1 Eu1 133.5(2) . . ?
N2 Ni1 O2 171.8(3) . . ?
N2 Ni1 O12 86.4(3) . . ?
N2 Ni1 O7 93.3(3) . . ?
N2 Ni1 N1 95.4(4) . . ?
N1 Ni1 Eu1 130.9(3) . . ?
N1 Ni1 O2 91.0(3) . . ?
N1 Ni1 O12 95.8(3) . . ?
N1 Ni1 O7 89.7(3) . . ?
C23 O8 Eu1 133.5(6) . . ?
Ni1 O4 Eu1 103.9(3) . . ?
C18 O4 Eu1 127.5(7) . . ?
C18 O4 Ni1 125.9(7) . . ?
C3 O1 Eu1 118.2(5) . . ?
C3 O1 C1 114.2(7) . . ?
C1 O1 Eu1 125.3(6) . . ?
Ni1 O2 Eu1 104.4(2) . . ?
C2 O2 Eu1 129.0(6) . . ?
C2 O2 Ni1 120.7(5) . . ?
C17 O5 Eu1 117.8(6) . . ?
C17 O5 C19 117.7(9) . . ?
C19 O5 Eu1 123.8(7) . . ?
C20 O6 Eu1 136.0(6) . . ?
C30 O11 Eu1 132.2(6) . . ?
Ni1 O12 H12A 110.4 . . ?
Ni1 O12 H12B 109.4 . . ?
H12A O12 H12B 108.7 . . ?
C25 O9 Eu1 134.8(6) . . ?
C20 O7 Ni1 123.3(7) . . ?
C10 O3 H3 109.5 . . ?
C28 O10 Eu1 136.0(7) . . ?
C12 N2 Ni1 122.2(8) . . ?
C12 N2 C11 117.0(9) . . ?
C11 N2 Ni1 120.2(6) . . ?
C8 N1 Ni1 122.5(7) . . ?
C8 N1 C9 114.3(9) . . ?
C9 N1 Ni1 123.2(7) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 121.9(11) . . ?
O6 C20 O7 130.7(10) . . ?
O6 C20 C21 113.7(10) . . ?
O7 C20 C21 115.6(11) . . ?
F2 C21 C20 112.4(9) . . ?
F1 C21 F2 107.9(10) . . ?
F1 C21 F3 107.5(10) . . ?
F1 C21 C20 118.1(13) . . ?
F3 C21 F2 95.9(11) . . ?
F3 C21 C20 112.7(9) . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0(9) . . ?
C16 C15 H15 120.0 . . ?
N2 C12 H12 115.3 . . ?
N2 C12 C13 129.4(10) . . ?
C13 C12 H12 115.3 . . ?
O1 C3 C2 112.8(7) . . ?
C4 C3 O1 125.9(9) . . ?
C4 C3 C2 121.4(9) . . ?
O4 C18 C13 123.9(11) . . ?
O4 C18 C17 117.2(10) . . ?
C17 C18 C13 118.9(11) . . ?
O8 C23 C22 111.6(8) . . ?
O8 C23 C24 128.5(9) . . ?
C24 C23 C22 119.8(8) . . ?
O2 C2 C3 117.3(8) . . ?
O2 C2 C7 124.2(8) . . ?
C7 C2 C3 118.4(8) . . ?
O11 C30 C31 117.3(9) . . ?
O11 C30 C29 127.9(10) . . ?
C29 C30 C31 114.7(9) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 C15 119.7(10) . . ?
C17 C16 H16 120.1 . . ?
O9 C25 C24 126.8(8) . . ?
O9 C25 C26 113.2(8) . . ?
C24 C25 C26 120.0(8) . . ?
N1 C8 H8 117.5 . . ?
N1 C8 C7 125.0(8) . . ?
C7 C8 H8 117.5 . . ?
F15 C31 F14 109.0(10) . . ?
F15 C31 F13 109.0(10) . . ?
F15 C31 C30 112.8(9) . . ?
F14 C31 C30 111.0(8) . . ?
F13 C31 F14 104.6(9) . . ?
F13 C31 C30 110.1(9) . . ?
F6 C22 C23 112.3(9) . . ?
F4 C22 F6 108.0(10) . . ?
F4 C22 C23 110.1(9) . . ?
F5 C22 F6 109.2(10) . . ?
F5 C22 F4 105.5(11) . . ?
F5 C22 C23 111.3(9) . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 118.1(10) . . ?
C5 C4 H4 121.0 . . ?
C23 C24 C25 122.3(8) . . ?
C23 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C4 C5 H5 118.7 . . ?
C6 C5 C4 122.7(10) . . ?
C6 C5 H5 118.7 . . ?
F8 C26 F7 110.3(9) . . ?
F8 C26 F9 108.3(10) . . ?
F8 C26 C25 109.7(8) . . ?
F7 C26 C25 112.1(8) . . ?
F9 C26 F7 104.7(8) . . ?
F9 C26 C25 111.6(8) . . ?
C14 C13 C12 118.5(11) . . ?
C14 C13 C18 118.6(12) . . ?
C12 C13 C18 122.9(11) . . ?
C2 C7 C8 125.2(8) . . ?
C2 C7 C6 120.1(9) . . ?
C6 C7 C8 114.7(9) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 C30 122.3(11) . . ?
C28 C29 H29 118.9 . . ?
F11 C27 C28 108.8(10) . . ?
F12 C27 F11 104.2(12) . . ?
F12 C27 C28 110.6(11) . . ?
F10 C27 F11 108.0(12) . . ?
F10 C27 F12 111.6(13) . . ?
F10 C27 C28 113.2(11) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O5 C17 C18 114.7(9) . . ?
O5 C17 C16 124.6(10) . . ?
C16 C17 C18 120.8(10) . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C10 H10 105.4 . . ?
O3 C10 C11 110.9(10) . . ?
O3 C10 C9 111.8(10) . . ?
C11 C10 H10 105.4 . . ?
C9 C10 H10 105.4 . . ?
C9 C10 C11 116.8(10) . . ?
N2 C11 C10 113.8(9) . . ?
N2 C11 H11A 108.8 . . ?
N2 C11 H11B 108.8 . . ?
C10 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C5 C6 C7 119.4(10) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
O10 C28 C29 129.5(10) . . ?
O10 C28 C27 110.9(10) . . ?
C29 C28 C27 119.6(11) . . ?
N1 C9 C10 116.7(9) . . ?
N1 C9 H9A 108.1 . . ?
N1 C9 H9B 108.1 . . ?
C10 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O8 C23 C22 -167.7(7) . . . . ?
Eu1 O8 C23 C24 9.0(15) . . . . ?
Eu1 O4 C18 C13 -173.0(6) . . . . ?
Eu1 O4 C18 C17 8.6(10) . . . . ?
Eu1 O1 C3 C2 2.5(9) . . . . ?
Eu1 O1 C3 C4 -178.4(7) . . . . ?
Eu1 O2 C2 C3 -2.0(10) . . . . ?
Eu1 O2 C2 C7 178.9(6) . . . . ?
Eu1 O5 C17 C18 -7.4(10) . . . . ?
Eu1 O5 C17 C16 171.9(8) . . . . ?
Eu1 O6 C20 O7 -7.4(16) . . . . ?
Eu1 O6 C20 C21 174.1(6) . . . . ?
Eu1 O11 C30 C31 175.5(6) . . . . ?
Eu1 O11 C30 C29 -0.5(15) . . . . ?
Eu1 O9 C25 C24 -16.5(15) . . . . ?
Eu1 O9 C25 C26 163.8(7) . . . . ?
Eu1 O10 C28 C29 7(2) . . . . ?
Eu1 O10 C28 C27 -172.1(8) . . . . ?
Ni1 O4 C18 C13 -14.6(11) . . . . ?
Ni1 O4 C18 C17 167.0(6) . . . . ?
Ni1 O2 C2 C3 -150.6(6) . . . . ?
Ni1 O2 C2 C7 30.4(10) . . . . ?
Ni1 O7 C20 O6 3.1(13) . . . . ?
Ni1 O7 C20 C21 -178.4(6) . . . . ?
Ni1 N2 C12 C13 6.0(15) . . . . ?
Ni1 N2 C11 C10 -36.4(12) . . . . ?
Ni1 N1 C8 C7 -8.1(13) . . . . ?
Ni1 N1 C9 C10 -5.6(14) . . . . ?
F11 C27 C28 O10 -172.5(11) . . . . ?
F11 C27 C28 C29 8.1(17) . . . . ?
F12 C27 C28 O10 -58.6(16) . . . . ?
F12 C27 C28 C29 121.9(13) . . . . ?
F10 C27 C28 O10 67.5(15) . . . . ?
F10 C27 C28 C29 -112.0(15) . . . . ?
O8 C23 C22 F6 -166.8(9) . . . . ?
O8 C23 C22 F4 72.8(11) . . . . ?
O8 C23 C22 F5 -43.9(13) . . . . ?
O8 C23 C24 C25 2.5(16) . . . . ?
O4 C18 C13 C14 178.7(8) . . . . ?
O4 C18 C13 C12 -3.4(13) . . . . ?
O4 C18 C17 O5 0.3(11) . . . . ?
O4 C18 C17 C16 -179.1(8) . . . . ?
O1 C3 C2 O2 -0.6(10) . . . . ?
O1 C3 C2 C7 178.5(7) . . . . ?
O1 C3 C4 C5 -178.5(9) . . . . ?
O2 C2 C7 C8 -2.0(13) . . . . ?
O2 C2 C7 C6 179.2(9) . . . . ?
O6 C20 C21 F2 66.9(12) . . . . ?
O6 C20 C21 F1 -166.5(10) . . . . ?
O6 C20 C21 F3 -40.1(13) . . . . ?
O11 C30 C31 F15 141.5(11) . . . . ?
O11 C30 C31 F14 18.9(13) . . . . ?
O11 C30 C31 F13 -96.4(11) . . . . ?
O11 C30 C29 C28 -5.5(17) . . . . ?
O9 C25 C24 C23 1.1(16) . . . . ?
O9 C25 C26 F8 -72.3(11) . . . . ?
O9 C25 C26 F7 164.8(8) . . . . ?
O9 C25 C26 F9 47.7(12) . . . . ?
O7 C20 C21 F2 -111.8(12) . . . . ?
O7 C20 C21 F1 14.8(13) . . . . ?
O7 C20 C21 F3 141.2(10) . . . . ?
O3 C10 C11 N2 -59.3(12) . . . . ?
O3 C10 C9 N1 82.9(12) . . . . ?
N2 C12 C13 C14 -174.1(10) . . . . ?
N2 C12 C13 C18 8.0(16) . . . . ?
N1 C8 C7 C2 -10.7(14) . . . . ?
N1 C8 C7 C6 168.1(9) . . . . ?
C14 C15 C16 C17 -1.2(17) . . . . ?
C15 C14 C13 C12 -176.6(10) . . . . ?
C15 C14 C13 C18 1.4(15) . . . . ?
C15 C16 C17 O5 -179.7(9) . . . . ?
C15 C16 C17 C18 -0.4(15) . . . . ?
C12 N2 C11 C10 152.5(10) . . . . ?
C3 C2 C7 C8 179.0(8) . . . . ?
C3 C2 C7 C6 0.1(13) . . . . ?
C3 C4 C5 C6 0.2(16) . . . . ?
C2 C3 C4 C5 0.5(14) . . . . ?
C2 C7 C6 C5 0.5(16) . . . . ?
C30 C29 C28 O10 2(2) . . . . ?
C30 C29 C28 C27 -178.2(11) . . . . ?
C8 N1 C9 C10 171.5(10) . . . . ?
C8 C7 C6 C5 -178.5(10) . . . . ?
C31 C30 C29 C28 178.3(10) . . . . ?
C22 C23 C24 C25 178.9(9) . . . . ?
C4 C3 C2 O2 -179.7(8) . . . . ?
C4 C3 C2 C7 -0.6(12) . . . . ?
C4 C5 C6 C7 -0.6(18) . . . . ?
C24 C23 C22 F6 16.3(15) . . . . ?
C24 C23 C22 F4 -104.2(11) . . . . ?
C24 C23 C22 F5 139.1(11) . . . . ?
C24 C25 C26 F8 107.9(11) . . . . ?
C24 C25 C26 F7 -14.9(13) . . . . ?
C24 C25 C26 F9 -132.0(10) . . . . ?
C26 C25 C24 C23 -179.1(9) . . . . ?
C13 C14 C15 C16 0.6(17) . . . . ?
C13 C18 C17 O5 -178.2(7) . . . . ?
C13 C18 C17 C16 2.4(13) . . . . ?
C29 C30 C31 F15 -41.9(14) . . . . ?
C29 C30 C31 F14 -164.5(9) . . . . ?
C29 C30 C31 F13 80.1(11) . . . . ?
C1 O1 C3 C2 -161.2(8) . . . . ?
C1 O1 C3 C4 17.8(13) . . . . ?
C17 C18 C13 C14 -2.9(13) . . . . ?
C17 C18 C13 C12 175.0(8) . . . . ?
C19 O5 C17 C18 163.1(8) . . . . ?
C19 O5 C17 C16 -17.5(13) . . . . ?
C11 N2 C12 C13 176.9(10) . . . . ?
C11 C10 C9 N1 -46.4(15) . . . . ?
C9 N1 C8 C7 174.8(9) . . . . ?
C9 C10 C11 N2 70.5(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_m20160117b_sq_d_sq
_database_code_depnum_ccdc_archive 'CCDC 1484046'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H53 Eu N2 Ni O11, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H57 Cl4 Eu N2 Ni O11'
_chemical_formula_weight         1406.60
_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'
Eu Eu -0.1578 3.6682 '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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2622(8)
_cell_length_b                   12.6894(11)
_cell_length_c                   23.490(2)
_cell_angle_alpha                81.784(4)
_cell_angle_beta                 83.709(4)
_cell_angle_gamma                76.878(4)
_cell_volume                     3225.4(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10062
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.744
_exptl_transmission_factor_min   0.698
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       -13
_diffrn_reflns_limit_h_min       13
_diffrn_reflns_limit_k_max       -15
_diffrn_reflns_limit_k_min       15
_diffrn_reflns_limit_l_max       -28
_diffrn_reflns_limit_l_min       28
_diffrn_reflns_number            12674
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.038
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11638
_reflns_number_total             12674
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.931
_refine_diff_density_min         -3.863
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         12498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0620
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+30.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1878
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H32 of C32, H50 of C50, H64 of C64, H37 of C37, H23 of C23, H56 of C56, H47
  of C47, H49 of C49, H54 of C54, H39 of C39, H65 of C65, H8 of C8, H4 of C4,
  H41 of C41, H24 of C24, H55 of C55, H38 of C38, H43 of C43, H6 of C6, H14 of
  C14, H15 of C15, H5 of C5, H46 of C46, H10 of C10, H48 of C48, H31 of C31,
  H61 of C61, {H9A,H9B} of C9, H58 of C58, H12 of C12, H40 of C40, H21 of C21,
  H16 of C16, H35 of C35, H27 of C27, H52 of C52, H53 of C53, H62 of C62, H25
  of C25, {H67A,H67B} of C67, {H11A,H11B} of C11, H33 of C33, H63 of C63, H34
  of C34, H22 of C22, {H66A,H66B} of C66
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, H3 of O3, {H1A,H1B,H1C} of C1
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C67(H67A,H67B), C11(H11A,H11B), C66(H66A,H66B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C55(H55), C38(H38), C39(H39), C54(H54), C49(H49), C47(H47),
 C50(H50), C64(H64), C37(H37), C56(H56), C23(H23), C32(H32), C65(H65), C8(H8),
 C4(H4), C41(H41), C24(H24), C6(H6), C14(H14), C15(H15), C5(H5), C46(H46),
 C48(H48), C31(H31), C61(H61), C58(H58), C12(H12), C40(H40), C21(H21), C16(H16),
  C35(H35), C27(H27), C52(H52), C53(H53), C62(H62), C25(H25), C33(H33),
 C63(H63), C34(H34), C22(H22)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu Eu 0.77475(3) 0.21420(2) 0.28036(2) 0.01692(11) Uani 1 1 d . . . . .
Cl4 Cl 0.7314(3) 0.3712(2) 0.56747(17) 0.0823(10) Uani 1 1 d . . . . .
Cl3 Cl 0.9512(3) 0.2145(4) 0.53829(15) 0.0964(13) Uani 1 1 d . . . . .
Cl2 Cl 0.7575(4) -0.1338(3) 0.17975(19) 0.1032(12) Uani 1 1 d . . . . .
O2 O 0.7881(4) 0.1995(4) 0.17772(18) 0.0206(9) Uani 1 1 d . . . . .
O10 O 0.5733(4) 0.3071(4) 0.28606(19) 0.0208(9) Uani 1 1 d . . . . .
O9 O 0.8546(4) 0.0253(3) 0.28471(19) 0.0209(9) Uani 1 1 d . . . . .
O5 O 0.9793(4) 0.1563(4) 0.34156(19) 0.0250(10) Uani 1 1 d . . . . .
O4 O 0.9704(4) 0.2223(3) 0.23432(18) 0.0189(8) Uani 1 1 d . . . . .
O11 O 0.7604(4) 0.3504(4) 0.33961(19) 0.0215(9) Uani 1 1 d . . . . .
O8 O 0.7069(4) 0.1314(4) 0.36932(19) 0.0221(9) Uani 1 1 d . . . . .
O7 O 0.7924(4) 0.3942(4) 0.20302(19) 0.0220(9) Uani 1 1 d . . . . .
O1 O 0.6256(4) 0.1141(4) 0.23719(19) 0.0214(9) Uani 1 1 d . . . . .
O6 O 1.0316(4) 0.3988(4) 0.1465(2) 0.0257(10) Uani 1 1 d . . . . .
O3 O 1.1545(5) 0.3487(5) 0.0446(2) 0.0420(13) Uani 1 1 d . . . . .
H3 H 1.1493 0.3427 0.0799 0.063 Uiso 1 1 calc R U . . .
N1 N 0.8508(5) 0.3400(5) 0.0774(2) 0.0261(12) Uani 1 1 d . . . . .
C36 C 0.7066(6) 0.4784(5) 0.4074(3) 0.0228(13) Uani 1 1 d . . . . .
C43 C 0.5469(6) 0.4050(5) 0.3669(3) 0.0231(13) Uani 1 1 d . . . . .
H43 H 0.4901 0.4393 0.3939 0.028 Uiso 1 1 calc R U . . .
C3 C 0.5895(6) 0.1702(5) 0.1851(3) 0.0228(13) Uani 1 1 d . . . . .
C60 C 0.9379(6) -0.1624(5) 0.3060(3) 0.0218(12) Uani 1 1 d . . . . .
C30 C 0.6770(6) 0.5597(5) 0.2319(3) 0.0254(13) Uani 1 1 d . . . . .
N2 N 1.0590(5) 0.1819(5) 0.1180(2) 0.0263(12) Uani 1 1 d . . . . .
C55 C 0.6259(6) -0.0597(6) 0.5539(3) 0.0316(15) Uani 1 1 d . . . . .
H55 H 0.6171 -0.1243 0.5766 0.038 Uiso 1 1 calc R U . . .
C18 C 1.0655(6) 0.1429(5) 0.2474(3) 0.0209(12) Uani 1 1 d . . . . .
C45 C 0.3708(6) 0.3601(5) 0.3244(3) 0.0209(12) Uani 1 1 d . . . . .
C2 C 0.6827(6) 0.2183(5) 0.1541(3) 0.0213(12) Uani 1 1 d . . . . .
C38 C 0.8683(7) 0.5334(6) 0.4474(3) 0.0306(15) Uani 1 1 d . . . . .
H38 H 0.9512 0.5245 0.4518 0.037 Uiso 1 1 calc R U . . .
C44 C 0.5050(6) 0.3548(5) 0.3258(3) 0.0208(12) Uani 1 1 d . . . . .
C39 C 0.7841(7) 0.6145(6) 0.4730(3) 0.0286(14) Uani 1 1 d . . . . .
H39 H 0.8099 0.6603 0.4943 0.034 Uiso 1 1 calc R U . . .
C51 C 0.6834(5) 0.0349(5) 0.4622(3) 0.0218(13) Uani 1 1 d . . . . .
C54 C 0.5936(6) 0.0378(7) 0.5772(3) 0.0330(16) Uani 1 1 d . . . . .
H54 H 0.5634 0.0386 0.6156 0.040 Uiso 1 1 calc R U . . .
C49 C 0.2053(6) 0.3446(5) 0.2707(3) 0.0230(13) Uani 1 1 d . . . . .
H49 H 0.1772 0.3364 0.2361 0.028 Uiso 1 1 calc R U . . .
C47 C 0.1679(6) 0.3675(6) 0.3713(3) 0.0266(14) Uani 1 1 d . . . . .
H47 H 0.1148 0.3734 0.4044 0.032 Uiso 1 1 calc R U . . .
C50 C 0.3274(6) 0.3465(5) 0.2731(3) 0.0231(13) Uani 1 1 d . . . . .
H50 H 0.3809 0.3385 0.2401 0.028 Uiso 1 1 calc R U . . .
C64 C 1.1170(6) -0.2514(6) 0.2508(3) 0.0272(14) Uani 1 1 d . . . . .
H64 H 1.1845 -0.2469 0.2247 0.033 Uiso 1 1 calc R U . . .
C37 C 0.8298(6) 0.4658(6) 0.4153(3) 0.0279(14) Uani 1 1 d . . . . .
H37 H 0.8871 0.4112 0.3988 0.033 Uiso 1 1 calc R U . . .
C56 C 0.6714(6) -0.0614(6) 0.4968(3) 0.0292(15) Uani 1 1 d . . . . .
H56 H 0.6941 -0.1273 0.4814 0.035 Uiso 1 1 calc R U . . .
C42 C 0.6718(6) 0.4057(5) 0.3690(3) 0.0215(12) Uani 1 1 d . . . . .
C23 C 1.2669(10) 0.6898(9) 0.0933(4) 0.056(3) Uani 1 1 d . . . . .
H23 H 1.3255 0.7303 0.0796 0.068 Uiso 1 1 calc R U . . .
C32 C 0.4552(7) 0.6020(6) 0.2417(3) 0.0319(15) Uani 1 1 d . . . . .
H32 H 0.3812 0.5886 0.2338 0.038 Uiso 1 1 calc R U . . .
C65 C 1.0385(6) -0.1574(5) 0.2660(3) 0.0227(13) Uani 1 1 d . . . . .
H65 H 1.0528 -0.0899 0.2494 0.027 Uiso 1 1 calc R U . . .
C8 C 0.7485(6) 0.3293(6) 0.0634(3) 0.0300(15) Uani 1 1 d . . . . .
H8 H 0.7299 0.3550 0.0257 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4778(6) 0.1812(6) 0.1639(3) 0.0305(15) Uani 1 1 d . . . . .
H4 H 0.4183 0.1482 0.1849 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9866(7) 0.1345(7) 0.4022(3) 0.0332(16) Uani 1 1 d . . . . .
H19A H 0.9196 0.1816 0.4211 0.050 Uiso 1 1 calc R U . . .
H19B H 1.0625 0.1473 0.4117 0.050 Uiso 1 1 calc R U . . .
H19C H 0.9827 0.0599 0.4147 0.050 Uiso 1 1 calc R U . . .
C41 C 0.6231(7) 0.5574(7) 0.4334(3) 0.0351(17) Uani 1 1 d . . . . .
H41 H 0.5403 0.5657 0.4291 0.042 Uiso 1 1 calc R U . . .
C24 C 1.1456(10) 0.7404(8) 0.0984(4) 0.052(2) Uani 1 1 d . . . . .
H24 H 1.1215 0.8149 0.0872 0.063 Uiso 1 1 calc R U . . .
C13 C 1.1535(6) 0.0925(5) 0.2068(3) 0.0242(13) Uani 1 1 d . . . . .
C6 C 0.5428(7) 0.2911(7) 0.0792(3) 0.0342(16) Uani 1 1 d . . . . .
H6 H 0.5266 0.3313 0.0435 0.041 Uiso 1 1 calc R U . . .
C1 C 0.5408(6) 0.0604(6) 0.2726(3) 0.0295(15) Uani 1 1 d . . . . .
H1A H 0.5759 0.0263 0.3078 0.044 Uiso 1 1 calc R U . . .
H1B H 0.5223 0.0059 0.2525 0.044 Uiso 1 1 calc R U . . .
H1C H 0.4671 0.1126 0.2811 0.044 Uiso 1 1 calc R U . . .
C14 C 1.2527(6) 0.0109(6) 0.2274(3) 0.0294(15) Uani 1 1 d . . . . .
H14 H 1.3119 -0.0225 0.2010 0.035 Uiso 1 1 calc R U . . .
C20 C 1.0916(7) 0.5677(7) 0.1355(3) 0.0321(16) Uani 1 1 d . . . . .
C15 C 1.2637(6) -0.0200(6) 0.2854(3) 0.0303(15) Uani 1 1 d . . . . .
H15 H 1.3305 -0.0732 0.2976 0.036 Uiso 1 1 calc R U . . .
C57 C 0.7304(6) 0.0388(5) 0.3994(3) 0.0211(12) Uani 1 1 d . . . . .
C5 C 0.4546(7) 0.2427(7) 0.1103(3) 0.0345(16) Uani 1 1 d . . . . .
H5 H 0.3792 0.2508 0.0956 0.041 Uiso 1 1 calc R U . . .
C46 C 0.2894(6) 0.3712(6) 0.3735(3) 0.0255(13) Uani 1 1 d . . . . .
H46 H 0.3168 0.3811 0.4079 0.031 Uiso 1 1 calc R U . . .
C26 C 1.0001(6) 0.4979(6) 0.1572(3) 0.0250(13) Uani 1 1 d . . . . .
C29 C 0.7925(6) 0.4940(5) 0.2066(3) 0.0217(12) Uani 1 1 d . . . . .
C10 C 1.0609(7) 0.3066(8) 0.0260(3) 0.0388(18) Uani 1 1 d . . . . .
H10 H 1.0813 0.3013 -0.0153 0.047 Uiso 1 1 calc R U . . .
C48 C 0.1248(6) 0.3550(5) 0.3201(3) 0.0248(13) Uani 1 1 d . . . . .
H48 H 0.0429 0.3537 0.3187 0.030 Uiso 1 1 calc R U . . .
C31 C 0.5639(6) 0.5392(6) 0.2202(3) 0.0279(14) Uani 1 1 d . . . . .
H31 H 0.5627 0.4840 0.1983 0.033 Uiso 1 1 calc R U . . .
C61 C 0.9172(6) -0.2652(6) 0.3293(3) 0.0263(14) Uani 1 1 d . . . . .
H61 H 0.8506 -0.2701 0.3560 0.032 Uiso 1 1 calc R U . . .
C9 C 0.9338(7) 0.3825(7) 0.0311(3) 0.0352(17) Uani 1 1 d . . . . .
H9A H 0.9427 0.4533 0.0386 0.042 Uiso 1 1 calc R U . . .
H9B H 0.8974 0.3922 -0.0054 0.042 Uiso 1 1 calc R U . . .
C59 C 0.8586(6) -0.0574(5) 0.3220(3) 0.0213(12) Uani 1 1 d . . . . .
C58 C 0.7983(6) -0.0559(5) 0.3777(3) 0.0232(13) Uani 1 1 d . . . . .
H58 H 0.8038 -0.1217 0.4015 0.028 Uiso 1 1 calc R U . . .
C7 C 0.6575(6) 0.2808(6) 0.1006(3) 0.0253(13) Uani 1 1 d . . . . .
C12 C 1.1448(6) 0.1153(6) 0.1443(3) 0.0260(14) Uani 1 1 d . . . . .
H12 H 1.2082 0.0774 0.1213 0.031 Uiso 1 1 calc R U . . .
C17 C 1.0771(6) 0.1055(5) 0.3073(3) 0.0237(13) Uani 1 1 d . . . . .
C40 C 0.6609(7) 0.6259(7) 0.4663(3) 0.0361(17) Uani 1 1 d . . . . .
H40 H 0.6032 0.6790 0.4837 0.043 Uiso 1 1 calc R U . . .
C21 C 1.2157(7) 0.5169(8) 0.1295(3) 0.0381(18) Uani 1 1 d . . . . .
H21 H 1.2400 0.4420 0.1393 0.046 Uiso 1 1 calc R U . . .
C16 C 1.1754(6) 0.0277(6) 0.3262(3) 0.0282(14) Uani 1 1 d . . . . .
H16 H 1.1832 0.0070 0.3655 0.034 Uiso 1 1 calc R U . . .
C35 C 0.6770(7) 0.6430(6) 0.2643(3) 0.0324(15) Uani 1 1 d . . . . .
H35 H 0.7507 0.6582 0.2712 0.039 Uiso 1 1 calc R U . . .
C27 C 0.8899(6) 0.5455(6) 0.1856(3) 0.0276(14) Uani 1 1 d . . . . .
H27 H 0.8796 0.6182 0.1913 0.033 Uiso 1 1 calc R U . . .
C52 C 0.6500(6) 0.1330(6) 0.4863(3) 0.0269(14) Uani 1 1 d . . . . .
H52 H 0.6574 0.1979 0.4636 0.032 Uiso 1 1 calc R U . . .
C53 C 0.6059(7) 0.1342(7) 0.5437(3) 0.0316(15) Uani 1 1 d . . . . .
H53 H 0.5847 0.1996 0.5596 0.038 Uiso 1 1 calc R U . . .
C62 C 0.9940(7) -0.3589(6) 0.3134(3) 0.0306(15) Uani 1 1 d . . . . .
H62 H 0.9779 -0.4264 0.3287 0.037 Uiso 1 1 calc R U . . .
C25 C 1.0578(8) 0.6787(7) 0.1205(3) 0.0399(18) Uani 1 1 d . . . . .
H25 H 0.9758 0.7135 0.1251 0.048 Uiso 1 1 calc R U . . .
C67 C 0.8595(11) -0.0437(9) 0.1533(5) 0.065(3) Uani 1 1 d . . . . .
H67A H 0.8300 0.0258 0.1683 0.078 Uiso 1 1 calc R U . . .
H67B H 0.9404 -0.0752 0.1660 0.078 Uiso 1 1 calc R U . . .
C11 C 1.0666(7) 0.1898(6) 0.0550(3) 0.0317(15) Uani 1 1 d . . . . .
H11A H 0.9998 0.1630 0.0435 0.038 Uiso 1 1 calc R U . . .
H11B H 1.1427 0.1436 0.0416 0.038 Uiso 1 1 calc R U . . .
C33 C 0.4548(7) 0.6841(6) 0.2748(4) 0.0397(18) Uani 1 1 d . . . . .
H33 H 0.3811 0.7255 0.2889 0.048 Uiso 1 1 calc R U . . .
C63 C 1.0955(6) -0.3535(6) 0.2745(3) 0.0281(14) Uani 1 1 d . . . . .
H63 H 1.1483 -0.4170 0.2644 0.034 Uiso 1 1 calc R U . . .
C34 C 0.5661(8) 0.7046(7) 0.2868(4) 0.0431(19) Uani 1 1 d . . . . .
H34 H 0.5666 0.7587 0.3096 0.052 Uiso 1 1 calc R U . . .
C22 C 1.3021(8) 0.5781(10) 0.1088(4) 0.051(2) Uani 1 1 d . . . . .
H22 H 1.3845 0.5440 0.1053 0.061 Uiso 1 1 calc R U . . .
C66 C 0.8327(11) 0.2560(10) 0.5911(5) 0.067(3) Uani 1 1 d . . . . .
H66A H 0.7892 0.1977 0.6030 0.080 Uiso 1 1 calc R U . . .
H66B H 0.8681 0.2687 0.6247 0.080 Uiso 1 1 calc R U . . .
Ni1 Ni 0.91894(7) 0.29020(7) 0.15566(3) 0.01972(18) Uani 1 1 d . . . . .
Cl1 Cl 0.8663(7) -0.0240(5) 0.0768(2) 0.145(2) 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
Eu O2 2.430(4) . ?
Eu O10 2.307(4) . ?
Eu O9 2.353(4) . ?
Eu O5 2.751(5) . ?
Eu O4 2.363(4) . ?
Eu O11 2.337(4) . ?
Eu O8 2.333(4) . ?
Eu O7 2.738(4) . ?
Eu O1 2.679(4) . ?
Eu C18 3.231(6) . ?
Eu C2 3.238(6) . ?
Eu Ni1 3.3180(8) . ?
Cl4 C66 1.702(12) . ?
Cl3 C66 1.761(12) . ?
Cl2 C67 1.803(14) . ?
O2 C2 1.324(8) . ?
O2 Ni1 2.048(4) . ?
O10 C44 1.275(8) . ?
O9 C59 1.262(8) . ?
O5 C19 1.419(8) . ?
O5 C17 1.383(8) . ?
O4 C18 1.323(8) . ?
O4 Ni1 2.011(4) . ?
O11 C42 1.278(8) . ?
O8 C57 1.270(8) . ?
O7 C29 1.282(8) . ?
O7 Ni1 2.056(4) . ?
O1 C3 1.378(8) . ?
O1 C1 1.423(8) . ?
O6 C26 1.280(9) . ?
O6 Ni1 2.051(5) . ?
O3 H3 0.8200 . ?
O3 C10 1.418(10) . ?
N1 C8 1.272(9) . ?
N1 C9 1.478(8) . ?
N1 Ni1 2.032(6) . ?
C36 C37 1.390(9) . ?
C36 C42 1.517(9) . ?
C36 C41 1.372(10) . ?
C43 H43 0.9300 . ?
C43 C44 1.404(9) . ?
C43 C42 1.415(9) . ?
C3 C2 1.415(9) . ?
C3 C4 1.373(9) . ?
C60 C65 1.397(9) . ?
C60 C61 1.401(9) . ?
C60 C59 1.498(9) . ?
C30 C29 1.490(9) . ?
C30 C31 1.418(10) . ?
C30 C35 1.388(10) . ?
N2 C12 1.281(9) . ?
N2 C11 1.464(9) . ?
N2 Ni1 2.053(6) . ?
C55 H55 0.9300 . ?
C55 C54 1.382(11) . ?
C55 C56 1.383(10) . ?
C18 C13 1.407(9) . ?
C18 C17 1.429(9) . ?
C45 C44 1.502(8) . ?
C45 C50 1.395(9) . ?
C45 C46 1.395(9) . ?
C2 C7 1.407(9) . ?
C38 H38 0.9300 . ?
C38 C39 1.389(10) . ?
C38 C37 1.385(10) . ?
C39 H39 0.9300 . ?
C39 C40 1.386(11) . ?
C51 C56 1.393(9) . ?
C51 C57 1.510(9) . ?
C51 C52 1.397(10) . ?
C54 H54 0.9300 . ?
C54 C53 1.383(11) . ?
C49 H49 0.9300 . ?
C49 C50 1.388(9) . ?
C49 C48 1.395(9) . ?
C47 H47 0.9300 . ?
C47 C46 1.386(9) . ?
C47 C48 1.387(10) . ?
C50 H50 0.9300 . ?
C64 H64 0.9300 . ?
C64 C65 1.381(9) . ?
C64 C63 1.398(10) . ?
C37 H37 0.9300 . ?
C56 H56 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.371(16) . ?
C23 C22 1.389(16) . ?
C32 H32 0.9300 . ?
C32 C31 1.388(10) . ?
C32 C33 1.385(12) . ?
C65 H65 0.9300 . ?
C8 H8 0.9300 . ?
C8 C7 1.459(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.401(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C41 H41 0.9300 . ?
C41 C40 1.402(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.408(11) . ?
C13 C14 1.415(10) . ?
C13 C12 1.466(10) . ?
C6 H6 0.9300 . ?
C6 C5 1.373(11) . ?
C6 C7 1.408(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C15 1.373(11) . ?
C20 C26 1.509(9) . ?
C20 C21 1.401(12) . ?
C20 C25 1.377(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.400(11) . ?
C57 C58 1.400(9) . ?
C5 H5 0.9300 . ?
C46 H46 0.9300 . ?
C26 C27 1.394(10) . ?
C29 C27 1.410(9) . ?
C10 H10 0.9800 . ?
C10 C9 1.537(11) . ?
C10 C11 1.531(12) . ?
C48 H48 0.9300 . ?
C31 H31 0.9300 . ?
C61 H61 0.9300 . ?
C61 C62 1.376(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C59 C58 1.407(9) . ?
C58 H58 0.9300 . ?
C12 H12 0.9300 . ?
C17 C16 1.373(10) . ?
C40 H40 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.385(11) . ?
C16 H16 0.9300 . ?
C35 H35 0.9300 . ?
C35 C34 1.407(11) . ?
C27 H27 0.9300 . ?
C52 H52 0.9300 . ?
C52 C53 1.386(10) . ?
C53 H53 0.9300 . ?
C62 H62 0.9300 . ?
C62 C63 1.391(10) . ?
C25 H25 0.9300 . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C67 Cl1 1.774(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C33 H33 0.9300 . ?
C33 C34 1.401(13) . ?
C63 H63 0.9300 . ?
C34 H34 0.9300 . ?
C22 H22 0.9300 . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?

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 Eu O5 121.33(14) . . ?
O2 Eu O7 60.93(14) . . ?
O2 Eu O1 59.04(13) . . ?
O2 Eu C18 76.65(15) . . ?
O2 Eu C2 21.55(15) . . ?
O2 Eu Ni1 37.94(10) . . ?
O10 Eu O2 95.68(15) . . ?
O10 Eu O9 129.02(15) . . ?
O10 Eu O5 142.01(14) . . ?
O10 Eu O4 143.22(15) . . ?
O10 Eu O11 73.00(15) . . ?
O10 Eu O8 80.21(15) . . ?
O10 Eu O7 80.29(14) . . ?
O10 Eu O1 66.97(14) . . ?
O10 Eu C18 164.04(15) . . ?
O10 Eu C2 74.97(15) . . ?
O10 Eu Ni1 110.87(11) . . ?
O9 Eu O2 81.93(15) . . ?
O9 Eu O5 69.75(15) . . ?
O9 Eu O4 82.40(14) . . ?
O9 Eu O7 136.13(14) . . ?
O9 Eu O1 68.64(14) . . ?
O9 Eu C18 64.44(15) . . ?
O9 Eu C2 90.54(16) . . ?
O9 Eu Ni1 98.03(11) . . ?
O5 Eu C18 44.96(15) . . ?
O5 Eu C2 142.65(15) . . ?
O5 Eu Ni1 95.81(10) . . ?
O4 Eu O2 67.23(14) . . ?
O4 Eu O5 59.09(14) . . ?
O4 Eu O7 62.93(14) . . ?
O4 Eu O1 121.16(14) . . ?
O4 Eu C18 20.83(15) . . ?
O4 Eu C2 87.86(15) . . ?
O4 Eu Ni1 36.85(10) . . ?
O11 Eu O2 137.73(15) . . ?
O11 Eu O9 137.00(15) . . ?
O11 Eu O5 73.52(15) . . ?
O11 Eu O4 97.43(15) . . ?
O11 Eu O7 76.91(14) . . ?
O11 Eu O1 138.50(14) . . ?
O11 Eu C18 103.10(15) . . ?
O11 Eu C2 132.46(16) . . ?
O11 Eu Ni1 107.28(11) . . ?
O8 Eu O2 141.19(15) . . ?
O8 Eu O9 71.82(15) . . ?
O8 Eu O5 75.88(15) . . ?
O8 Eu O4 133.69(15) . . ?
O8 Eu O11 78.27(15) . . ?
O8 Eu O7 151.99(14) . . ?
O8 Eu O1 84.54(15) . . ?
O8 Eu C18 114.57(16) . . ?
O8 Eu C2 128.97(16) . . ?
O8 Eu Ni1 168.53(11) . . ?
O7 Eu O5 108.88(13) . . ?
O7 Eu C18 83.75(14) . . ?
O7 Eu C2 63.72(15) . . ?
O7 Eu Ni1 38.20(9) . . ?
O1 Eu O5 137.73(14) . . ?
O1 Eu O7 105.92(13) . . ?
O1 Eu C18 118.39(14) . . ?
O1 Eu C2 44.79(14) . . ?
O1 Eu Ni1 96.90(9) . . ?
C18 Eu C2 98.19(16) . . ?
C18 Eu Ni1 54.80(11) . . ?
C2 Eu Ni1 54.60(11) . . ?
C2 O2 Eu 116.0(4) . . ?
C2 O2 Ni1 124.8(4) . . ?
Ni1 O2 Eu 95.22(16) . . ?
C44 O10 Eu 132.6(4) . . ?
C59 O9 Eu 137.2(4) . . ?
C19 O5 Eu 128.9(4) . . ?
C17 O5 Eu 109.3(4) . . ?
C17 O5 C19 117.1(5) . . ?
C18 O4 Eu 119.7(4) . . ?
C18 O4 Ni1 128.2(4) . . ?
Ni1 O4 Eu 98.35(17) . . ?
C42 O11 Eu 133.7(4) . . ?
C57 O8 Eu 137.8(4) . . ?
C29 O7 Eu 135.4(4) . . ?
C29 O7 Ni1 126.3(4) . . ?
Ni1 O7 Eu 86.35(15) . . ?
C3 O1 Eu 109.9(3) . . ?
C3 O1 C1 117.7(5) . . ?
C1 O1 Eu 122.8(4) . . ?
C26 O6 Ni1 125.8(4) . . ?
C10 O3 H3 109.5 . . ?
C8 N1 C9 117.3(6) . . ?
C8 N1 Ni1 126.1(5) . . ?
C9 N1 Ni1 116.2(4) . . ?
C37 C36 C42 117.9(6) . . ?
C41 C36 C37 118.7(6) . . ?
C41 C36 C42 123.3(6) . . ?
C44 C43 H43 118.6 . . ?
C44 C43 C42 122.9(6) . . ?
C42 C43 H43 118.6 . . ?
O1 C3 C2 111.8(5) . . ?
C4 C3 O1 126.3(6) . . ?
C4 C3 C2 121.9(6) . . ?
C65 C60 C59 118.2(6) . . ?
C61 C60 C65 118.3(6) . . ?
C61 C60 C59 123.5(6) . . ?
C31 C30 C29 118.7(6) . . ?
C35 C30 C29 121.9(6) . . ?
C35 C30 C31 119.4(6) . . ?
C12 N2 C11 117.7(6) . . ?
C12 N2 Ni1 125.7(5) . . ?
C11 N2 Ni1 116.3(4) . . ?
C54 C55 H55 120.0 . . ?
C54 C55 C56 120.0(7) . . ?
C56 C55 H55 120.0 . . ?
O4 C18 Eu 39.4(3) . . ?
O4 C18 C13 124.8(6) . . ?
O4 C18 C17 116.8(6) . . ?
C13 C18 Eu 143.5(4) . . ?
C13 C18 C17 118.4(6) . . ?
C17 C18 Eu 87.0(4) . . ?
C50 C45 C44 118.8(6) . . ?
C50 C45 C46 118.9(6) . . ?
C46 C45 C44 122.1(6) . . ?
O2 C2 Eu 42.4(3) . . ?
O2 C2 C3 116.9(6) . . ?
O2 C2 C7 125.1(6) . . ?
C3 C2 Eu 84.3(4) . . ?
C7 C2 Eu 145.7(4) . . ?
C7 C2 C3 118.1(6) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C37 C38 C39 120.5(7) . . ?
O10 C44 C43 124.5(6) . . ?
O10 C44 C45 114.9(5) . . ?
C43 C44 C45 120.5(6) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 C38 118.9(6) . . ?
C40 C39 H39 120.5 . . ?
C56 C51 C57 123.0(6) . . ?
C52 C51 C56 119.0(6) . . ?
C52 C51 C57 118.0(6) . . ?
C55 C54 H54 119.8 . . ?
C55 C54 C53 120.3(6) . . ?
C53 C54 H54 119.8 . . ?
C50 C49 H49 120.0 . . ?
C50 C49 C48 120.0(6) . . ?
C48 C49 H49 120.0 . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C48 C47 C46 120.7(6) . . ?
C45 C50 H50 119.6 . . ?
C49 C50 C45 120.7(6) . . ?
C49 C50 H50 119.6 . . ?
C65 C64 H64 119.8 . . ?
C65 C64 C63 120.3(6) . . ?
C63 C64 H64 119.8 . . ?
C36 C37 C38 120.8(7) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C55 C56 C51 120.4(7) . . ?
C55 C56 H56 119.8 . . ?
C51 C56 H56 119.8 . . ?
O11 C42 C36 115.9(5) . . ?
O11 C42 C43 124.9(6) . . ?
C43 C42 C36 119.2(6) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.0(8) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C33 C32 C31 121.3(7) . . ?
C60 C65 H65 119.6 . . ?
C64 C65 C60 120.8(6) . . ?
C64 C65 H65 119.6 . . ?
N1 C8 H8 116.6 . . ?
N1 C8 C7 126.7(6) . . ?
C7 C8 H8 116.6 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.3(6) . . ?
C5 C4 H4 120.3 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C36 C41 H41 119.5 . . ?
C36 C41 C40 121.0(7) . . ?
C40 C41 H41 119.5 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.5(9) . . ?
C25 C24 H24 120.2 . . ?
C18 C13 C14 118.4(6) . . ?
C18 C13 C12 123.6(6) . . ?
C14 C13 C12 117.9(6) . . ?
C5 C6 H6 119.5 . . ?
C5 C6 C7 121.0(7) . . ?
C7 C6 H6 119.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.6(7) . . ?
C15 C14 H14 119.2 . . ?
C21 C20 C26 118.4(7) . . ?
C25 C20 C26 122.7(7) . . ?
C25 C20 C21 118.9(7) . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.7(6) . . ?
C16 C15 H15 119.7 . . ?
O8 C57 C51 116.2(6) . . ?
O8 C57 C58 123.7(6) . . ?
C58 C57 C51 120.1(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.3(7) . . ?
C6 C5 H5 119.9 . . ?
C45 C46 H46 119.9 . . ?
C47 C46 C45 120.3(6) . . ?
C47 C46 H46 119.9 . . ?
O6 C26 C20 115.5(6) . . ?
O6 C26 C27 125.9(6) . . ?
C27 C26 C20 118.6(6) . . ?
O7 C29 C30 115.9(6) . . ?
O7 C29 C27 124.8(6) . . ?
C27 C29 C30 119.2(6) . . ?
O3 C10 H10 106.1 . . ?
O3 C10 C9 113.6(7) . . ?
O3 C10 C11 109.7(6) . . ?
C9 C10 H10 106.1 . . ?
C11 C10 H10 106.1 . . ?
C11 C10 C9 114.6(6) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 C49 119.3(6) . . ?
C47 C48 H48 120.3 . . ?
C30 C31 H31 120.2 . . ?
C32 C31 C30 119.5(7) . . ?
C32 C31 H31 120.2 . . ?
C60 C61 H61 119.6 . . ?
C62 C61 C60 120.9(6) . . ?
C62 C61 H61 119.6 . . ?
N1 C9 C10 112.7(6) . . ?
N1 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O9 C59 C60 116.9(6) . . ?
O9 C59 C58 124.4(6) . . ?
C58 C59 C60 118.6(6) . . ?
C57 C58 C59 123.9(6) . . ?
C57 C58 H58 118.0 . . ?
C59 C58 H58 118.0 . . ?
C2 C7 C8 122.9(6) . . ?
C2 C7 C6 119.4(6) . . ?
C6 C7 C8 117.5(6) . . ?
N2 C12 C13 126.7(6) . . ?
N2 C12 H12 116.6 . . ?
C13 C12 H12 116.6 . . ?
O5 C17 C18 111.9(5) . . ?
C16 C17 O5 126.1(6) . . ?
C16 C17 C18 122.0(6) . . ?
C39 C40 C41 120.1(7) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.1(9) . . ?
C22 C21 H21 120.0 . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.8(7) . . ?
C17 C16 H16 120.6 . . ?
C30 C35 H35 119.8 . . ?
C30 C35 C34 120.4(7) . . ?
C34 C35 H35 119.8 . . ?
C26 C27 C29 126.3(6) . . ?
C26 C27 H27 116.9 . . ?
C29 C27 H27 116.9 . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.4(7) . . ?
C53 C52 H52 119.8 . . ?
C54 C53 C52 119.8(7) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C61 C62 H62 119.7 . . ?
C63 C62 C61 120.6(6) . . ?
C63 C62 H62 119.7 . . ?
C24 C25 H25 119.5 . . ?
C20 C25 C24 120.9(9) . . ?
C20 C25 H25 119.5 . . ?
Cl2 C67 H67A 109.9 . . ?
Cl2 C67 H67B 109.9 . . ?
H67A C67 H67B 108.3 . . ?
Cl1 C67 Cl2 108.8(6) . . ?
Cl1 C67 H67A 109.9 . . ?
Cl1 C67 H67B 109.9 . . ?
N2 C11 C10 112.6(6) . . ?
N2 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C32 C33 H33 120.2 . . ?
C32 C33 C34 119.5(7) . . ?
C34 C33 H33 120.2 . . ?
C64 C63 H63 120.5 . . ?
C62 C63 C64 119.1(6) . . ?
C62 C63 H63 120.5 . . ?
C35 C34 C33 119.8(8) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C23 C22 C21 120.5(9) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
Cl4 C66 Cl3 112.9(7) . . ?
Cl4 C66 H66A 109.0 . . ?
Cl4 C66 H66B 109.0 . . ?
Cl3 C66 H66A 109.0 . . ?
Cl3 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
O2 Ni1 Eu 46.84(12) . . ?
O2 Ni1 O7 79.85(17) . . ?
O2 Ni1 O6 168.41(19) . . ?
O2 Ni1 N2 102.0(2) . . ?
O4 Ni1 Eu 44.80(12) . . ?
O4 Ni1 O2 81.65(17) . . ?
O4 Ni1 O7 82.50(17) . . ?
O4 Ni1 O6 93.90(18) . . ?
O4 Ni1 N1 170.8(2) . . ?
O4 Ni1 N2 90.2(2) . . ?
O7 Ni1 Eu 55.45(12) . . ?
O6 Ni1 Eu 123.45(14) . . ?
O6 Ni1 O7 88.99(18) . . ?
O6 Ni1 N2 88.6(2) . . ?
N1 Ni1 Eu 128.72(16) . . ?
N1 Ni1 O2 89.4(2) . . ?
N1 Ni1 O7 98.3(2) . . ?
N1 Ni1 O6 95.3(2) . . ?
N1 Ni1 N2 89.3(2) . . ?
N2 Ni1 Eu 120.47(16) . . ?
N2 Ni1 O7 172.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu O2 C2 C3 -44.1(7) . . . . ?
Eu O2 C2 C7 136.7(6) . . . . ?
Eu O10 C44 C43 30.3(9) . . . . ?
Eu O10 C44 C45 -153.0(4) . . . . ?
Eu O9 C59 C60 -171.3(4) . . . . ?
Eu O9 C59 C58 5.7(10) . . . . ?
Eu O5 C17 C18 28.8(6) . . . . ?
Eu O5 C17 C16 -150.9(5) . . . . ?
Eu O4 C18 C13 134.1(5) . . . . ?
Eu O4 C18 C17 -45.0(6) . . . . ?
Eu O11 C42 C36 173.3(4) . . . . ?
Eu O11 C42 C43 -8.3(10) . . . . ?
Eu O8 C57 C51 163.9(4) . . . . ?
Eu O8 C57 C58 -14.6(10) . . . . ?
Eu O7 C29 C30 -64.9(8) . . . . ?
Eu O7 C29 C27 118.9(6) . . . . ?
Eu O1 C3 C2 33.7(6) . . . . ?
Eu O1 C3 C4 -146.0(6) . . . . ?
Eu C18 C13 C14 -132.1(6) . . . . ?
Eu C18 C13 C12 44.4(10) . . . . ?
Eu C18 C17 O5 -22.8(4) . . . . ?
Eu C18 C17 C16 156.9(6) . . . . ?
Eu C2 C7 C8 57.7(11) . . . . ?
Eu C2 C7 C6 -127.3(7) . . . . ?
O2 C2 C7 C8 2.5(11) . . . . ?
O2 C2 C7 C6 177.6(6) . . . . ?
O9 C59 C58 C57 -2.8(10) . . . . ?
O5 C17 C16 C15 176.5(6) . . . . ?
O4 C18 C13 C14 177.9(6) . . . . ?
O4 C18 C13 C12 -5.7(10) . . . . ?
O4 C18 C17 O5 3.9(7) . . . . ?
O4 C18 C17 C16 -176.4(6) . . . . ?
O8 C57 C58 C59 6.8(10) . . . . ?
O7 C29 C27 C26 0.8(11) . . . . ?
O1 C3 C2 Eu -25.7(5) . . . . ?
O1 C3 C2 O2 2.4(8) . . . . ?
O1 C3 C2 C7 -178.4(6) . . . . ?
O1 C3 C4 C5 179.0(7) . . . . ?
O6 C26 C27 C29 -1.4(12) . . . . ?
O3 C10 C9 N1 -109.3(7) . . . . ?
O3 C10 C11 N2 55.9(8) . . . . ?
N1 C8 C7 C2 -13.9(12) . . . . ?
N1 C8 C7 C6 171.0(8) . . . . ?
C36 C41 C40 C39 0.1(13) . . . . ?
C3 C2 C7 C8 -176.6(6) . . . . ?
C3 C2 C7 C6 -1.6(10) . . . . ?
C3 C4 C5 C6 0.2(12) . . . . ?
C60 C61 C62 C63 1.3(11) . . . . ?
C60 C59 C58 C57 174.2(6) . . . . ?
C30 C29 C27 C26 -175.2(6) . . . . ?
C30 C35 C34 C33 -2.2(13) . . . . ?
C55 C54 C53 C52 0.5(11) . . . . ?
C18 C13 C14 C15 0.6(10) . . . . ?
C18 C13 C12 N2 -0.1(11) . . . . ?
C18 C17 C16 C15 -3.1(9) . . . . ?
C2 C3 C4 C5 -0.7(11) . . . . ?
C38 C39 C40 C41 -1.0(12) . . . . ?
C44 C43 C42 O11 -9.4(10) . . . . ?
C44 C43 C42 C36 169.1(6) . . . . ?
C44 C45 C50 C49 176.4(6) . . . . ?
C44 C45 C46 C47 -175.1(6) . . . . ?
C39 C38 C37 C36 0.9(11) . . . . ?
C51 C57 C58 C59 -171.6(6) . . . . ?
C51 C52 C53 C54 -0.8(10) . . . . ?
C54 C55 C56 C51 -0.8(11) . . . . ?
C50 C45 C44 O10 -19.9(8) . . . . ?
C50 C45 C44 C43 156.9(6) . . . . ?
C50 C45 C46 C47 0.7(10) . . . . ?
C50 C49 C48 C47 0.2(10) . . . . ?
C37 C36 C42 O11 -10.7(9) . . . . ?
C37 C36 C42 C43 170.7(6) . . . . ?
C37 C36 C41 C40 1.3(12) . . . . ?
C37 C38 C39 C40 0.5(11) . . . . ?
C56 C55 C54 C53 0.3(11) . . . . ?
C56 C51 C57 O8 161.8(6) . . . . ?
C56 C51 C57 C58 -19.6(9) . . . . ?
C56 C51 C52 C53 0.2(10) . . . . ?
C42 C36 C37 C38 176.6(6) . . . . ?
C42 C36 C41 C40 -177.0(7) . . . . ?
C42 C43 C44 O10 -1.4(10) . . . . ?
C42 C43 C44 C45 -177.8(6) . . . . ?
C23 C24 C25 C20 -2.1(13) . . . . ?
C32 C33 C34 C35 1.2(13) . . . . ?
C65 C60 C61 C62 0.1(10) . . . . ?
C65 C60 C59 O9 27.4(8) . . . . ?
C65 C60 C59 C58 -149.9(6) . . . . ?
C65 C64 C63 C62 0.1(10) . . . . ?
C8 N1 C9 C10 -124.8(8) . . . . ?
C4 C3 C2 Eu 154.0(6) . . . . ?
C4 C3 C2 O2 -177.9(6) . . . . ?
C4 C3 C2 C7 1.4(10) . . . . ?
C19 O5 C17 C18 -173.5(5) . . . . ?
C19 O5 C17 C16 6.9(9) . . . . ?
C41 C36 C37 C38 -1.8(11) . . . . ?
C41 C36 C42 O11 167.5(7) . . . . ?
C41 C36 C42 C43 -11.0(10) . . . . ?
C24 C23 C22 C21 -0.1(13) . . . . ?
C13 C18 C17 O5 -175.2(5) . . . . ?
C13 C18 C17 C16 4.5(9) . . . . ?
C13 C14 C15 C16 0.9(10) . . . . ?
C1 O1 C3 C2 -179.2(6) . . . . ?
C1 O1 C3 C4 1.1(10) . . . . ?
C14 C13 C12 N2 176.4(6) . . . . ?
C14 C15 C16 C17 0.4(10) . . . . ?
C20 C26 C27 C29 177.3(6) . . . . ?
C20 C21 C22 C23 -0.7(12) . . . . ?
C57 C51 C56 C55 -179.0(6) . . . . ?
C57 C51 C52 C53 179.8(6) . . . . ?
C5 C6 C7 C2 1.2(12) . . . . ?
C5 C6 C7 C8 176.5(7) . . . . ?
C46 C45 C44 O10 155.9(6) . . . . ?
C46 C45 C44 C43 -27.3(9) . . . . ?
C46 C45 C50 C49 0.4(10) . . . . ?
C46 C47 C48 C49 0.9(10) . . . . ?
C26 C20 C21 C22 179.0(7) . . . . ?
C26 C20 C25 C24 -177.6(7) . . . . ?
C29 C30 C31 C32 -177.8(6) . . . . ?
C29 C30 C35 C34 179.0(7) . . . . ?
C48 C49 C50 C45 -0.8(10) . . . . ?
C48 C47 C46 C45 -1.3(11) . . . . ?
C31 C30 C29 O7 -35.5(9) . . . . ?
C31 C30 C29 C27 140.9(7) . . . . ?
C31 C30 C35 C34 1.8(11) . . . . ?
C31 C32 C33 C34 0.1(12) . . . . ?
C61 C60 C65 C64 -1.4(10) . . . . ?
C61 C60 C59 O9 -153.1(6) . . . . ?
C61 C60 C59 C58 29.6(9) . . . . ?
C61 C62 C63 C64 -1.4(11) . . . . ?
C9 N1 C8 C7 174.5(7) . . . . ?
C9 C10 C11 N2 -73.2(8) . . . . ?
C59 C60 C65 C64 178.1(6) . . . . ?
C59 C60 C61 C62 -179.4(6) . . . . ?
C7 C6 C5 C4 -0.5(13) . . . . ?
C12 N2 C11 C10 -124.6(7) . . . . ?
C12 C13 C14 C15 -176.1(6) . . . . ?
C17 C18 C13 C14 -3.1(9) . . . . ?
C17 C18 C13 C12 173.3(6) . . . . ?
C21 C20 C26 O6 -27.4(9) . . . . ?
C21 C20 C26 C27 153.8(7) . . . . ?
C21 C20 C25 C24 1.3(11) . . . . ?
C35 C30 C29 O7 147.3(7) . . . . ?
C35 C30 C29 C27 -36.3(10) . . . . ?
C35 C30 C31 C32 -0.6(10) . . . . ?
C52 C51 C56 C55 0.6(10) . . . . ?
C52 C51 C57 O8 -17.7(8) . . . . ?
C52 C51 C57 C58 160.9(6) . . . . ?
C25 C20 C26 O6 151.5(7) . . . . ?
C25 C20 C26 C27 -27.4(10) . . . . ?
C25 C20 C21 C22 0.1(11) . . . . ?
C11 N2 C12 C13 -178.2(6) . . . . ?
C11 C10 C9 N1 17.9(9) . . . . ?
C33 C32 C31 C30 -0.4(11) . . . . ?
C63 C64 C65 C60 1.3(10) . . . . ?
C22 C23 C24 C25 1.5(13) . . . . ?
Ni1 O2 C2 Eu -117.6(5) . . . . ?
Ni1 O2 C2 C3 -161.7(4) . . . . ?
Ni1 O2 C2 C7 19.1(9) . . . . ?
Ni1 O4 C18 Eu -131.5(6) . . . . ?
Ni1 O4 C18 C13 2.5(8) . . . . ?
Ni1 O4 C18 C17 -176.5(4) . . . . ?
Ni1 O7 C29 C30 166.0(4) . . . . ?
Ni1 O7 C29 C27 -10.2(9) . . . . ?
Ni1 O6 C26 C20 -167.7(4) . . . . ?
Ni1 O6 C26 C27 11.1(9) . . . . ?
Ni1 N1 C8 C7 1.0(11) . . . . ?
Ni1 N1 C9 C10 49.3(8) . . . . ?
Ni1 N2 C12 C13 8.1(10) . . . . ?
Ni1 N2 C11 C10 49.7(7) . . . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_p160615h_sq
_database_code_depnum_ccdc_archive 'CCDC 1527850'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H57 Cl4 Ho N2 Ni O11'
_chemical_formula_sum            'C66 H57 Cl4 Ho N2 Ni O11'
_chemical_formula_weight         1419.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHONNiHoCl
_chemical_oxdiff_usercomment     jianglinNiHo
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'
Ho Ho -0.2175 4.6783 '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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2770(4)
_cell_length_b                   12.6970(5)
_cell_length_c                   23.3931(8)
_cell_angle_alpha                81.822(3)
_cell_angle_beta                 83.284(3)
_cell_angle_gamma                76.675(3)
_cell_volume                     3213.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11845
_cell_measurement_temperature    128.75(10)
_cell_measurement_theta_max      28.8560
_cell_measurement_theta_min      3.2390
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         3.046
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      128.75(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.6107
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  92.00   1.00    7.00    --   18.94  19.00-120.00  109
  2  ω      1.00  60.00   1.00    7.00    --   18.94 -99.00-120.00   59
  3  ω     24.00  61.00   1.00    7.00    --   18.94 -99.00 120.00   37
  4  ω    -42.00  50.00   1.00    7.00    --  -19.25  77.00  60.00   92
  5  ω    -82.00  11.00   1.00    7.00    --  -19.25 -77.00 -60.00   93
  6  ω    -89.00 -64.00   1.00    7.00    --  -19.25-178.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0472782000
_diffrn_orient_matrix_UB_12      -0.0423244000
_diffrn_orient_matrix_UB_13      -0.0100710000
_diffrn_orient_matrix_UB_21      0.0347001000
_diffrn_orient_matrix_UB_22      0.0389373000
_diffrn_orient_matrix_UB_23      -0.0123469000
_diffrn_orient_matrix_UB_31      0.0277656000
_diffrn_orient_matrix_UB_32      -0.0059880000
_diffrn_orient_matrix_UB_33      0.0262993000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10319
_reflns_number_total             11450
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0382
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+3.8928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H6 of C6, H8 of C8, H5 of C5, H33 of C33, H23 of C23, H4 of C4, {H11A,H11B}
  of C11, H54 of C54, H15 of C15, {H9A,H9B} of C9, H32 of C32, H30 of C30, H61
  of C61, H62 of C62, H31 of C31, {H68A,H68B} of C68, {H67A,H67B,H67C,H67D} of
  C67, H27 of C27, H49 of C49, H47 of C47, H36 of C36, H53 of C53, H25 of C25,
  H24 of C24, H37 of C37, H42 of C42, H10 of C10, H14 of C14, H55 of C55, H26
  of C26, H57 of C57, H46 of C46, H22 of C22, H63 of C63, H40 of C40, H39 of
  C39, H52 of C52, H48 of C48, H34 of C34, H51 of C51, H38 of C38, H65 of C65,
  H45 of C45, H16 of C16, H60 of C60, H12 of C12
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, H3 of O3, {H19A,H19B,H19C} of C19
2. Others
 1-Sof(H67B)=1-Sof(H67B)=Sof(H67C)=Sof(H67D)
 1-Sof(Cl2B)=Sof(Cl2B)
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C68(H68A,H68B), C67(H67A,H67B), C67(H67C,H67D)
3.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C37(H37), C24(H24), C25(H25), C53(H53), C36(H36), C47(H47),
 C49(H49), C27(H27), C22(H22), C63(H63), C40(H40), C39(H39), C52(H52), C48(H48),
  C34(H34), C51(H51), C38(H38), C65(H65), C45(H45), C16(H16), C60(H60),
 C12(H12), C46(H46), C57(H57), C26(H26), C55(H55), C14(H14), C6(H6), C8(H8),
 C5(H5), C33(H33), C23(H23), C4(H4), C54(H54), C15(H15), C32(H32), C30(H30),
 C61(H61), C62(H62), C31(H31)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.72492(2) 0.78662(2) 0.21960(2) 0.01376(6) Uani 1 1 d . . . . .
Ni1 Ni 0.58275(4) 0.70811(4) 0.34344(2) 0.01654(12) Uani 1 1 d . . . . .
Cl4 Cl 0.54965(17) 0.78850(19) -0.03999(7) 0.0948(8) Uani 1 1 d . . . . .
Cl3 Cl 0.76628(17) 0.62862(13) -0.06904(8) 0.0797(5) Uani 1 1 d . . . . .
Cl1 Cl 0.7407(2) 1.13261(16) 0.32195(9) 0.0884(6) Uani 1 1 d . . . . .
Cl2A Cl 0.6399(4) 1.0221(3) 0.42284(12) 0.0615(16) Uani 0.494(10) 1 d . . P A 1
O4 O 0.7150(2) 0.7958(2) 0.32007(10) 0.0175(6) Uani 1 1 d . . . . .
O1 O 0.5242(2) 0.8423(2) 0.15760(10) 0.0202(6) Uani 1 1 d . . . . .
O2 O 0.5333(2) 0.7778(2) 0.26405(10) 0.0165(6) Uani 1 1 d . . . . .
O10 O 0.7941(2) 0.8651(2) 0.13248(10) 0.0194(6) Uani 1 1 d . . . . .
O9 O 0.7358(2) 0.6521(2) 0.16214(10) 0.0181(6) Uani 1 1 d . . . . .
O11 O 0.6439(2) 0.9713(2) 0.21692(10) 0.0161(6) Uani 1 1 d . . . . .
O5 O 0.8733(2) 0.8874(2) 0.26157(10) 0.0195(6) Uani 1 1 d . . . . .
O7 O 0.7076(2) 0.6026(2) 0.29654(10) 0.0197(6) Uani 1 1 d . . . . .
O6 O 0.4683(2) 0.6015(2) 0.35317(11) 0.0222(6) Uani 1 1 d . . . . .
O8 O 0.9216(2) 0.6940(2) 0.21589(10) 0.0178(6) Uani 1 1 d . . . . .
N2 N 0.6498(3) 0.6603(3) 0.42180(13) 0.0237(8) Uani 1 1 d . . . . .
O3 O 0.3476(3) 0.6520(3) 0.45579(12) 0.0383(8) Uani 1 1 d . . . . .
H3 H 0.3651 0.6391 0.4221 0.057 Uiso 1 1 calc R U . . .
C42 C 0.9475(4) 0.5978(3) 0.13452(15) 0.0198(9) Uani 1 1 d . . . . .
H42 H 1.0040 0.5646 0.1067 0.024 Uiso 1 1 calc R U . . .
C37 C 1.2882(4) 0.6555(3) 0.23072(16) 0.0208(9) Uani 1 1 d . . . . .
H37 H 1.3153 0.6636 0.2656 0.025 Uiso 1 1 calc R U . . .
C24 C 0.2292(7) 0.3153(6) 0.4073(2) 0.062(2) Uani 1 1 d . . . . .
H24 H 0.1704 0.2753 0.4215 0.075 Uiso 1 1 calc R U . . .
C25 C 0.3506(7) 0.2639(5) 0.4015(2) 0.0589(18) Uani 1 1 d . . . . .
H25 H 0.3738 0.1892 0.4122 0.071 Uiso 1 1 calc R U . . .
C53 C 0.9082(4) 0.9576(4) -0.07644(16) 0.0301(11) Uani 1 1 d . . . . .
H53 H 0.9387 0.9564 -0.1151 0.036 Uiso 1 1 calc R U . . .
C36 C 1.1677(4) 0.6535(3) 0.22832(15) 0.0194(9) Uani 1 1 d . . . . .
H36 H 1.1143 0.6608 0.2617 0.023 Uiso 1 1 calc R U . . .
C44 C 0.7894(4) 0.5255(3) 0.09408(15) 0.0183(8) Uani 1 1 d . . . . .
C59 C 0.5598(4) 1.1591(3) 0.19565(15) 0.0164(8) Uani 1 1 d . . . . .
C29 C 0.8222(4) 0.4370(3) 0.26705(16) 0.0219(9) Uani 1 1 d . . . . .
N1 N 0.4435(3) 0.8175(3) 0.38128(13) 0.0236(8) Uani 1 1 d . . . . .
C47 C 0.7123(4) 0.3904(4) 0.02812(17) 0.0292(10) Uani 1 1 d . . . . .
H47 H 0.6868 0.3446 0.0068 0.035 Uiso 1 1 calc R U . . .
C49 C 0.6666(4) 0.5362(3) 0.08678(16) 0.0246(9) Uani 1 1 d . . . . .
H49 H 0.6087 0.5895 0.1043 0.030 Uiso 1 1 calc R U . . .
C43 C 0.8244(4) 0.5967(3) 0.13269(14) 0.0169(8) Uani 1 1 d . . . . .
C35 C 1.1233(4) 0.6408(3) 0.17707(15) 0.0168(8) Uani 1 1 d . . . . .
C21 C 0.4058(4) 0.4345(4) 0.36453(16) 0.0316(11) Uani 1 1 d . . . . .
C27 C 0.6086(4) 0.4531(3) 0.31324(16) 0.0233(9) Uani 1 1 d . . . . .
H27 H 0.6179 0.3808 0.3071 0.028 Uiso 1 1 calc R U . . .
C22 C 0.2824(5) 0.4864(5) 0.37117(17) 0.0405(13) Uani 1 1 d . . . . .
H22 H 0.2589 0.5614 0.3616 0.049 Uiso 1 1 calc R U . . .
C63 C 0.3792(4) 1.2488(3) 0.25071(16) 0.0232(9) Uani 1 1 d . . . . .
H63 H 0.3112 1.2445 0.2769 0.028 Uiso 1 1 calc R U . . .
C40 C 1.2054(4) 0.6302(3) 0.12785(16) 0.0215(9) Uani 1 1 d . . . . .
H40 H 1.1785 0.6208 0.0932 0.026 Uiso 1 1 calc R U . . .
C28 C 0.7060(4) 0.5035(3) 0.29274(15) 0.0188(8) Uani 1 1 d . . . . .
C2 C 0.4373(3) 0.8541(3) 0.25180(15) 0.0175(8) Uani 1 1 d . . . . .
C20 C 0.4976(4) 0.5026(3) 0.34240(15) 0.0208(9) Uani 1 1 d . . . . .
C39 C 1.3270(4) 0.6336(3) 0.12987(17) 0.0252(9) Uani 1 1 d . . . . .
H39 H 1.3805 0.6277 0.0965 0.030 Uiso 1 1 calc R U . . .
C17 C 0.9094(4) 0.8309(3) 0.31416(15) 0.0178(8) Uani 1 1 d . . . . .
C52 C 0.8725(4) 1.0550(4) -0.05379(17) 0.0313(11) Uani 1 1 d . . . . .
H52 H 0.8792 1.1195 -0.0770 0.038 Uiso 1 1 calc R U . . .
C48 C 0.6280(4) 0.4699(4) 0.05411(17) 0.0288(10) Uani 1 1 d . . . . .
H48 H 0.5451 0.4790 0.0498 0.035 Uiso 1 1 calc R U . . .
C13 C 0.8429(4) 0.7208(3) 0.39867(16) 0.0251(9) Uani 1 1 d . . . . .
C34 C 0.9324(4) 0.4574(3) 0.27752(17) 0.0256(9) Uani 1 1 d . . . . .
H34 H 0.9334 0.5135 0.2989 0.031 Uiso 1 1 calc R U . . .
C41 C 0.9903(4) 0.6460(3) 0.17572(14) 0.0157(8) Uani 1 1 d . . . . .
C51 C 0.8265(4) 1.0573(3) 0.00383(16) 0.0247(9) Uani 1 1 d . . . . .
H51 H 0.8011 1.1237 0.0188 0.030 Uiso 1 1 calc R U . . .
C38 C 1.3694(4) 0.6458(3) 0.18193(17) 0.0222(9) Uani 1 1 d . . . . .
H38 H 1.4510 0.6474 0.1836 0.027 Uiso 1 1 calc R U . . .
C50 C 0.8179(4) 0.9613(3) 0.03939(15) 0.0188(8) Uani 1 1 d . . . . .
C65 C 0.4584(4) 1.1545(3) 0.23568(16) 0.0205(9) Uani 1 1 d . . . . .
H65 H 0.4441 1.0871 0.2524 0.025 Uiso 1 1 calc R U . . .
C45 C 0.8732(4) 0.4452(4) 0.06643(19) 0.0330(11) Uani 1 1 d . . . . .
H45 H 0.9563 0.4362 0.0701 0.040 Uiso 1 1 calc R U . . .
C58 C 0.6404(3) 1.0537(3) 0.17960(15) 0.0164(8) Uani 1 1 d . . . . .
C3 C 0.4254(4) 0.8917(3) 0.19171(16) 0.0183(8) Uani 1 1 d . . . . .
C19 C 0.9585(4) 0.9410(4) 0.22639(17) 0.0281(10) Uani 1 1 d . . . . .
H19A H 1.0315 0.8884 0.2167 0.042 Uiso 1 1 calc R U . . .
H19B H 0.9784 0.9937 0.2472 0.042 Uiso 1 1 calc R U . . .
H19C H 0.9231 0.9772 0.1915 0.042 Uiso 1 1 calc R U . . .
C16 C 1.0194(4) 0.8238(3) 0.33555(17) 0.0251(9) Uani 1 1 d . . . . .
H16 H 1.0776 0.8587 0.3145 0.030 Uiso 1 1 calc R U . . .
C60 C 0.5810(4) 1.2610(3) 0.17213(16) 0.0222(9) Uani 1 1 d . . . . .
H60 H 0.6483 1.2657 0.1456 0.027 Uiso 1 1 calc R U . . .
C12 C 0.7524(4) 0.6705(4) 0.43577(16) 0.0279(10) Uani 1 1 d . . . . .
H12 H 0.7714 0.6432 0.4734 0.033 Uiso 1 1 calc R U . . .
C46 C 0.8349(5) 0.3793(4) 0.03395(19) 0.0367(12) Uani 1 1 d . . . . .
H46 H 0.8923 0.3266 0.0157 0.044 Uiso 1 1 calc R U . . .
C57 C 0.7012(4) 1.0527(3) 0.12378(15) 0.0210(9) Uani 1 1 d . . . . .
H57 H 0.6953 1.1184 0.0998 0.025 Uiso 1 1 calc R U . . .
C26 C 0.4377(5) 0.3224(4) 0.38006(18) 0.0404(13) Uani 1 1 d . . . . .
H26 H 0.5195 0.2865 0.3758 0.048 Uiso 1 1 calc R U . . .
C55 C 0.8546(4) 0.8634(3) 0.01539(16) 0.0236(9) Uani 1 1 d . . . . .
H55 H 0.8491 0.7984 0.0384 0.028 Uiso 1 1 calc R U . . .
C14 C 0.9553(4) 0.7141(4) 0.42013(17) 0.0329(11) Uani 1 1 d . . . . .
H14 H 0.9710 0.6752 0.4562 0.039 Uiso 1 1 calc R U . . .
C10 C 0.4406(4) 0.6944(4) 0.47385(17) 0.0334(11) Uani 1 1 d . . . . .
H10 H 0.4206 0.6998 0.5154 0.040 Uiso 1 1 calc R U . . .
C6 C 0.2474(4) 0.9850(3) 0.27241(18) 0.0238(9) Uani 1 1 d . . . . .
H6 H 0.1876 1.0182 0.2990 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3480(4) 0.9044(3) 0.29255(16) 0.0202(9) Uani 1 1 d . . . . .
C18 C 0.8188(4) 0.7813(3) 0.34428(15) 0.0179(8) Uani 1 1 d . . . . .
C8 C 0.3571(4) 0.8829(3) 0.35474(17) 0.0237(9) Uani 1 1 d . . . . .
H8 H 0.2932 0.9206 0.3779 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2372(4) 1.0145(3) 0.21431(18) 0.0266(10) Uani 1 1 d . . . . .
H5 H 0.1693 1.0660 0.2019 0.032 Uiso 1 1 calc R U . . .
C33 C 1.0413(4) 0.3945(4) 0.2563(2) 0.0338(11) Uani 1 1 d . . . . .
H33 H 1.1152 0.4074 0.2643 0.041 Uiso 1 1 calc R U . . .
C23 C 0.1946(5) 0.4262(6) 0.39209(19) 0.0554(17) Uani 1 1 d . . . . .
H23 H 0.1124 0.4608 0.3958 0.067 Uiso 1 1 calc R U . . .
C4 C 0.3272(4) 0.9685(3) 0.17341(17) 0.0240(9) Uani 1 1 d . . . . .
H4 H 0.3203 0.9900 0.1340 0.029 Uiso 1 1 calc R U . . .
C11 C 0.5680(4) 0.6171(4) 0.46798(16) 0.0310(11) Uani 1 1 d . . . . .
H11A H 0.6046 0.6062 0.5045 0.037 Uiso 1 1 calc R U . . .
H11B H 0.5587 0.5468 0.4598 0.037 Uiso 1 1 calc R U . . .
C56 C 0.7702(3) 0.9578(3) 0.10232(15) 0.0167(8) Uani 1 1 d . . . . .
C1 C 0.5185(4) 0.8623(4) 0.09624(15) 0.0298(10) Uani 1 1 d . . . . .
H1A H 0.5174 0.9377 0.0834 0.045 Uiso 1 1 calc R U . . .
H1B H 0.4455 0.8448 0.0865 0.045 Uiso 1 1 calc R U . . .
H1C H 0.5888 0.8177 0.0776 0.045 Uiso 1 1 calc R U . . .
C54 C 0.8992(4) 0.8613(4) -0.04225(16) 0.0280(10) Uani 1 1 d . . . . .
H54 H 0.9229 0.7954 -0.0578 0.034 Uiso 1 1 calc R U . . .
C15 C 1.0430(4) 0.7633(4) 0.38947(18) 0.0346(11) Uani 1 1 d . . . . .
H15 H 1.1177 0.7565 0.4043 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4352(4) 0.8112(4) 0.44469(16) 0.0328(11) Uani 1 1 d . . . . .
H9A H 0.3591 0.8578 0.4581 0.039 Uiso 1 1 calc R U . . .
H9B H 0.5020 0.8378 0.4560 0.039 Uiso 1 1 calc R U . . .
C32 C 1.0410(5) 0.3126(4) 0.2235(2) 0.0409(12) Uani 1 1 d . . . . .
H32 H 1.1147 0.2708 0.2093 0.049 Uiso 1 1 calc R U . . .
C30 C 0.8213(4) 0.3534(4) 0.23413(18) 0.0315(11) Uani 1 1 d . . . . .
H30 H 0.7476 0.3383 0.2273 0.038 Uiso 1 1 calc R U . . .
C61 C 0.5024(4) 1.3553(3) 0.18814(17) 0.0265(10) Uani 1 1 d . . . . .
H61 H 0.5181 1.4229 0.1727 0.032 Uiso 1 1 calc R U . . .
C62 C 0.4007(4) 1.3498(3) 0.22689(16) 0.0248(10) Uani 1 1 d . . . . .
H62 H 0.3473 1.4134 0.2369 0.030 Uiso 1 1 calc R U . . .
C31 C 0.9324(5) 0.2926(4) 0.2116(2) 0.0453(14) Uani 1 1 d . . . . .
H31 H 0.9327 0.2386 0.1886 0.054 Uiso 1 1 calc R U . . .
C68 C 0.6687(5) 0.7470(5) -0.0923(2) 0.0552(15) Uani 1 1 d . . . . .
H68A H 0.6343 0.7371 -0.1268 0.066 Uiso 1 1 calc R U . . .
H68B H 0.7143 0.8040 -0.1028 0.066 Uiso 1 1 calc R U . . .
C67 C 0.6447(6) 1.0426(5) 0.3483(2) 0.0570(16) Uani 1 1 d . . . . .
H67A H 0.5630 1.0730 0.3364 0.068 Uiso 0.64(13) 1 calc R U P A 1
H67B H 0.6755 0.9737 0.3327 0.068 Uiso 0.64(13) 1 calc R U P A 1
H67C H 0.6904 0.9698 0.3422 0.068 Uiso 0.36(13) 1 calc R U P A 2
H67D H 0.5773 1.0595 0.3239 0.068 Uiso 0.36(13) 1 calc R U P A 2
Cl2B Cl 0.580(2) 1.0365(11) 0.4219(8) 0.471(17) Uani 0.506(10) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 Ni1 3.2841(5) . ?
Ho1 O4 2.358(2) . ?
Ho1 O1 2.732(3) . ?
Ho1 O2 2.306(3) . ?
Ho1 O10 2.272(2) . ?
Ho1 O9 2.293(2) . ?
Ho1 O11 2.307(2) . ?
Ho1 O5 2.670(3) . ?
Ho1 O7 2.770(3) . ?
Ho1 O8 2.257(3) . ?
Ni1 O4 2.040(3) . ?
Ni1 O2 2.022(2) . ?
Ni1 O7 2.042(3) . ?
Ni1 O6 2.049(3) . ?
Ni1 N2 2.024(3) . ?
Ni1 N1 2.049(3) . ?
Cl4 C68 1.746(6) . ?
Cl3 C68 1.706(6) . ?
Cl1 C67 1.752(7) . ?
Cl2A C67 1.722(6) . ?
O4 C18 1.324(4) . ?
O1 C3 1.372(5) . ?
O1 C1 1.428(4) . ?
O2 C2 1.305(4) . ?
O10 C56 1.272(4) . ?
O9 C43 1.274(4) . ?
O11 C58 1.260(4) . ?
O5 C17 1.388(4) . ?
O5 C19 1.421(5) . ?
O7 C28 1.278(5) . ?
O6 C20 1.276(5) . ?
O8 C41 1.277(4) . ?
N2 C12 1.277(5) . ?
N2 C11 1.466(5) . ?
O3 H3 0.8200 . ?
O3 C10 1.413(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.396(6) . ?
C42 C41 1.396(5) . ?
C37 H37 0.9300 . ?
C37 C36 1.374(6) . ?
C37 C38 1.378(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.374(9) . ?
C24 C23 1.377(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.373(7) . ?
C53 H53 0.9300 . ?
C53 C52 1.370(6) . ?
C53 C54 1.380(6) . ?
C36 H36 0.9300 . ?
C36 C35 1.395(5) . ?
C44 C49 1.388(6) . ?
C44 C43 1.507(5) . ?
C44 C45 1.397(5) . ?
C59 C65 1.397(6) . ?
C59 C58 1.504(5) . ?
C59 C60 1.394(6) . ?
C29 C28 1.497(5) . ?
C29 C34 1.381(6) . ?
C29 C30 1.401(6) . ?
N1 C8 1.283(5) . ?
N1 C9 1.467(5) . ?
C47 H47 0.9300 . ?
C47 C48 1.374(6) . ?
C47 C46 1.379(6) . ?
C49 H49 0.9300 . ?
C49 C48 1.383(6) . ?
C35 C40 1.392(5) . ?
C35 C41 1.490(5) . ?
C21 C22 1.396(7) . ?
C21 C20 1.500(6) . ?
C21 C26 1.390(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.399(6) . ?
C27 C20 1.409(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.390(7) . ?
C63 H63 0.9300 . ?
C63 C65 1.381(5) . ?
C63 C62 1.387(6) . ?
C40 H40 0.9300 . ?
C40 C39 1.387(6) . ?
C2 C3 1.430(5) . ?
C2 C7 1.409(5) . ?
C39 H39 0.9300 . ?
C39 C38 1.400(5) . ?
C17 C16 1.370(5) . ?
C17 C18 1.392(6) . ?
C52 H52 0.9300 . ?
C52 C51 1.389(5) . ?
C48 H48 0.9300 . ?
C13 C12 1.463(6) . ?
C13 C14 1.398(6) . ?
C13 C18 1.410(5) . ?
C34 H34 0.9300 . ?
C34 C33 1.382(6) . ?
C51 H51 0.9300 . ?
C51 C50 1.390(6) . ?
C38 H38 0.9300 . ?
C50 C55 1.393(5) . ?
C50 C56 1.505(5) . ?
C65 H65 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.374(6) . ?
C58 C57 1.402(5) . ?
C3 C4 1.361(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C16 H16 0.9300 . ?
C16 C15 1.400(6) . ?
C60 H60 0.9300 . ?
C60 C61 1.386(5) . ?
C12 H12 0.9300 . ?
C46 H46 0.9300 . ?
C57 H57 0.9300 . ?
C57 C56 1.399(5) . ?
C26 H26 0.9300 . ?
C55 H55 0.9300 . ?
C55 C54 1.384(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(7) . ?
C10 H10 0.9800 . ?
C10 C11 1.546(6) . ?
C10 C9 1.532(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.417(5) . ?
C6 C5 1.368(6) . ?
C7 C8 1.453(5) . ?
C8 H8 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.395(6) . ?
C33 H33 0.9300 . ?
C33 C32 1.378(7) . ?
C23 H23 0.9300 . ?
C4 H4 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C54 H54 0.9300 . ?
C15 H15 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C32 H32 0.9300 . ?
C32 C31 1.373(7) . ?
C30 H30 0.9300 . ?
C30 C31 1.399(6) . ?
C61 H61 0.9300 . ?
C61 C62 1.385(6) . ?
C62 H62 0.9300 . ?
C31 H31 0.9300 . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C67 H67C 0.9700 . ?
C67 H67D 0.9700 . ?
C67 Cl2B 1.788(14) . ?

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
O4 Ho1 Ni1 38.13(7) . . ?
O4 Ho1 O1 123.35(8) . . ?
O4 Ho1 O5 59.75(9) . . ?
O4 Ho1 O7 60.59(8) . . ?
O1 Ho1 Ni1 96.51(6) . . ?
O1 Ho1 O7 108.60(8) . . ?
O2 Ho1 Ni1 37.52(6) . . ?
O2 Ho1 O4 68.52(9) . . ?
O2 Ho1 O1 59.17(8) . . ?
O2 Ho1 O11 81.84(9) . . ?
O2 Ho1 O5 122.30(8) . . ?
O2 Ho1 O7 63.27(8) . . ?
O10 Ho1 Ni1 170.02(6) . . ?
O10 Ho1 O4 142.06(10) . . ?
O10 Ho1 O1 76.05(9) . . ?
O10 Ho1 O2 134.07(9) . . ?
O10 Ho1 O9 78.85(9) . . ?
O10 Ho1 O11 73.54(9) . . ?
O10 Ho1 O5 83.82(9) . . ?
O10 Ho1 O7 150.37(8) . . ?
O9 Ho1 Ni1 105.44(7) . . ?
O9 Ho1 O4 135.65(9) . . ?
O9 Ho1 O1 72.09(8) . . ?
O9 Ho1 O2 95.43(9) . . ?
O9 Ho1 O11 137.46(8) . . ?
O9 Ho1 O5 139.49(9) . . ?
O9 Ho1 O7 75.17(8) . . ?
O11 Ho1 Ni1 97.84(6) . . ?
O11 Ho1 O4 82.87(8) . . ?
O11 Ho1 O1 70.27(8) . . ?
O11 Ho1 O5 68.64(8) . . ?
O11 Ho1 O7 136.01(8) . . ?
O5 Ho1 Ni1 97.86(5) . . ?
O5 Ho1 O1 137.86(8) . . ?
O5 Ho1 O7 107.13(7) . . ?
O7 Ho1 Ni1 38.24(5) . . ?
O8 Ho1 Ni1 109.02(6) . . ?
O8 Ho1 O4 93.04(8) . . ?
O8 Ho1 O1 142.20(8) . . ?
O8 Ho1 O2 142.08(9) . . ?
O8 Ho1 O10 80.72(9) . . ?
O8 Ho1 O9 74.47(9) . . ?
O8 Ho1 O11 130.16(10) . . ?
O8 Ho1 O5 66.72(9) . . ?
O8 Ho1 O7 78.82(9) . . ?
O4 Ni1 Ho1 45.53(6) . . ?
O4 Ni1 O7 79.54(11) . . ?
O4 Ni1 O6 167.94(10) . . ?
O4 Ni1 N1 102.68(12) . . ?
O2 Ni1 Ho1 43.97(8) . . ?
O2 Ni1 O4 80.53(10) . . ?
O2 Ni1 O7 82.93(10) . . ?
O2 Ni1 O6 94.68(10) . . ?
O2 Ni1 N2 169.40(13) . . ?
O2 Ni1 N1 90.14(11) . . ?
O7 Ni1 Ho1 57.11(7) . . ?
O7 Ni1 O6 88.93(11) . . ?
O7 Ni1 N1 172.31(11) . . ?
O6 Ni1 Ho1 124.43(7) . . ?
O6 Ni1 N1 88.32(13) . . ?
N2 Ni1 Ho1 128.70(10) . . ?
N2 Ni1 O4 89.39(12) . . ?
N2 Ni1 O7 98.55(12) . . ?
N2 Ni1 O6 95.84(13) . . ?
N2 Ni1 N1 88.87(13) . . ?
N1 Ni1 Ho1 119.30(10) . . ?
Ni1 O4 Ho1 96.34(10) . . ?
C18 O4 Ho1 118.2(2) . . ?
C18 O4 Ni1 126.3(2) . . ?
C3 O1 Ho1 109.12(19) . . ?
C3 O1 C1 117.6(3) . . ?
C1 O1 Ho1 129.0(2) . . ?
Ni1 O2 Ho1 98.51(10) . . ?
C2 O2 Ho1 121.4(2) . . ?
C2 O2 Ni1 127.6(2) . . ?
C56 O10 Ho1 136.8(2) . . ?
C43 O9 Ho1 132.5(2) . . ?
C58 O11 Ho1 136.1(2) . . ?
C17 O5 Ho1 109.3(2) . . ?
C17 O5 C19 117.2(3) . . ?
C19 O5 Ho1 123.8(2) . . ?
Ni1 O7 Ho1 84.65(9) . . ?
C28 O7 Ho1 136.2(2) . . ?
C28 O7 Ni1 126.6(3) . . ?
C20 O6 Ni1 126.1(3) . . ?
C41 O8 Ho1 131.5(2) . . ?
C12 N2 Ni1 126.5(3) . . ?
C12 N2 C11 117.1(3) . . ?
C11 N2 Ni1 116.2(3) . . ?
C10 O3 H3 109.5 . . ?
C43 C42 H42 118.1 . . ?
C41 C42 H42 118.1 . . ?
C41 C42 C43 123.7(3) . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(3) . . ?
C38 C37 H37 119.7 . . ?
C25 C24 H24 120.0 . . ?
C25 C24 C23 120.0(6) . . ?
C23 C24 H24 120.0 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.3(6) . . ?
C26 C25 H25 119.8 . . ?
C52 C53 H53 119.8 . . ?
C52 C53 C54 120.4(4) . . ?
C54 C53 H53 119.8 . . ?
C37 C36 H36 119.2 . . ?
C37 C36 C35 121.6(4) . . ?
C35 C36 H36 119.2 . . ?
C49 C44 C43 119.0(3) . . ?
C49 C44 C45 117.2(4) . . ?
C45 C44 C43 123.8(4) . . ?
C65 C59 C58 118.4(3) . . ?
C60 C59 C65 118.6(3) . . ?
C60 C59 C58 123.0(4) . . ?
C34 C29 C28 118.9(4) . . ?
C34 C29 C30 119.7(4) . . ?
C30 C29 C28 121.4(4) . . ?
C8 N1 Ni1 125.2(3) . . ?
C8 N1 C9 117.8(3) . . ?
C9 N1 Ni1 116.6(3) . . ?
C48 C47 H47 120.3 . . ?
C48 C47 C46 119.5(4) . . ?
C46 C47 H47 120.3 . . ?
C44 C49 H49 119.1 . . ?
C48 C49 C44 121.8(4) . . ?
C48 C49 H49 119.1 . . ?
O9 C43 C42 124.7(3) . . ?
O9 C43 C44 115.4(3) . . ?
C42 C43 C44 119.8(3) . . ?
C36 C35 C41 119.6(3) . . ?
C40 C35 C36 117.8(4) . . ?
C40 C35 C41 122.4(3) . . ?
C22 C21 C20 118.5(4) . . ?
C26 C21 C22 118.3(5) . . ?
C26 C21 C20 123.2(4) . . ?
C28 C27 H27 117.2 . . ?
C28 C27 C20 125.6(4) . . ?
C20 C27 H27 117.2 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 H22 119.9 . . ?
C65 C63 H63 119.9 . . ?
C65 C63 C62 120.2(4) . . ?
C62 C63 H63 119.9 . . ?
C35 C40 H40 119.6 . . ?
C39 C40 C35 120.8(4) . . ?
C39 C40 H40 119.6 . . ?
O7 C28 C29 115.4(4) . . ?
O7 C28 C27 125.3(4) . . ?
C27 C28 C29 119.2(4) . . ?
O2 C2 C3 116.5(3) . . ?
O2 C2 C7 125.6(3) . . ?
C7 C2 C3 117.9(3) . . ?
O6 C20 C21 115.9(4) . . ?
O6 C20 C27 125.5(4) . . ?
C27 C20 C21 118.5(4) . . ?
C40 C39 H39 119.9 . . ?
C40 C39 C38 120.3(4) . . ?
C38 C39 H39 119.9 . . ?
O5 C17 C18 111.8(3) . . ?
C16 C17 O5 125.6(4) . . ?
C16 C17 C18 122.6(3) . . ?
C53 C52 H52 120.0 . . ?
C53 C52 C51 120.0(4) . . ?
C51 C52 H52 120.0 . . ?
C47 C48 C49 119.8(4) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C14 C13 C12 118.0(4) . . ?
C14 C13 C18 118.9(4) . . ?
C18 C13 C12 123.0(4) . . ?
C29 C34 H34 119.9 . . ?
C29 C34 C33 120.2(4) . . ?
C33 C34 H34 119.9 . . ?
O8 C41 C42 123.9(4) . . ?
O8 C41 C35 114.7(3) . . ?
C42 C41 C35 121.4(3) . . ?
C52 C51 H51 119.7 . . ?
C52 C51 C50 120.7(4) . . ?
C50 C51 H51 119.7 . . ?
C37 C38 C39 118.9(4) . . ?
C37 C38 H38 120.6 . . ?
C39 C38 H38 120.6 . . ?
C51 C50 C55 118.3(3) . . ?
C51 C50 C56 123.5(3) . . ?
C55 C50 C56 118.3(3) . . ?
C59 C65 H65 119.6 . . ?
C63 C65 C59 120.8(4) . . ?
C63 C65 H65 119.6 . . ?
C44 C45 H45 119.5 . . ?
C46 C45 C44 121.1(4) . . ?
C46 C45 H45 119.5 . . ?
O11 C58 C59 116.9(3) . . ?
O11 C58 C57 124.8(3) . . ?
C57 C58 C59 118.2(3) . . ?
O1 C3 C2 111.4(3) . . ?
C4 C3 O1 126.7(3) . . ?
C4 C3 C2 121.9(4) . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C16 H16 120.4 . . ?
C17 C16 C15 119.1(4) . . ?
C15 C16 H16 120.4 . . ?
C59 C60 H60 119.8 . . ?
C61 C60 C59 120.3(4) . . ?
C61 C60 H60 119.8 . . ?
N2 C12 C13 126.7(4) . . ?
N2 C12 H12 116.7 . . ?
C13 C12 H12 116.7 . . ?
C47 C46 H46 119.7 . . ?
C45 C46 C47 120.7(4) . . ?
C45 C46 H46 119.7 . . ?
C58 C57 H57 118.3 . . ?
C56 C57 C58 123.3(3) . . ?
C56 C57 H57 118.3 . . ?
C25 C26 C21 121.0(6) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
C50 C55 H55 119.5 . . ?
C54 C55 C50 121.0(4) . . ?
C54 C55 H55 119.5 . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.8(4) . . ?
C15 C14 H14 119.1 . . ?
O3 C10 H10 106.1 . . ?
O3 C10 C11 112.8(4) . . ?
O3 C10 C9 110.2(4) . . ?
C11 C10 H10 106.1 . . ?
C9 C10 H10 106.1 . . ?
C9 C10 C11 114.7(4) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.8(4) . . ?
C2 C7 C6 119.0(3) . . ?
C2 C7 C8 123.3(3) . . ?
C6 C7 C8 117.6(3) . . ?
O4 C18 C17 117.4(3) . . ?
O4 C18 C13 124.5(4) . . ?
C17 C18 C13 118.1(4) . . ?
N1 C8 C7 127.2(4) . . ?
N1 C8 H8 116.4 . . ?
C7 C8 H8 116.4 . . ?
C6 C5 H5 119.5 . . ?
C6 C5 C4 120.9(4) . . ?
C4 C5 H5 119.5 . . ?
C34 C33 H33 119.8 . . ?
C32 C33 C34 120.4(5) . . ?
C32 C33 H33 119.8 . . ?
C24 C23 C22 120.1(6) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C3 C4 C5 119.3(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N2 C11 C10 112.1(3) . . ?
N2 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O10 C56 C50 116.1(3) . . ?
O10 C56 C57 124.2(3) . . ?
C57 C56 C50 119.7(3) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C53 C54 C55 119.6(4) . . ?
C53 C54 H54 120.2 . . ?
C55 C54 H54 120.2 . . ?
C16 C15 H15 120.3 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.3 . . ?
N1 C9 C10 111.9(4) . . ?
N1 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C33 C32 H32 119.9 . . ?
C31 C32 C33 120.3(4) . . ?
C31 C32 H32 119.9 . . ?
C29 C30 H30 120.4 . . ?
C31 C30 C29 119.3(5) . . ?
C31 C30 H30 120.4 . . ?
C60 C61 H61 119.7 . . ?
C62 C61 C60 120.6(4) . . ?
C62 C61 H61 119.7 . . ?
C63 C62 H62 120.3 . . ?
C61 C62 C63 119.5(4) . . ?
C61 C62 H62 120.3 . . ?
C32 C31 C30 120.2(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
Cl4 C68 H68A 109.0 . . ?
Cl4 C68 H68B 109.0 . . ?
Cl3 C68 Cl4 112.8(3) . . ?
Cl3 C68 H68A 109.0 . . ?
Cl3 C68 H68B 109.0 . . ?
H68A C68 H68B 107.8 . . ?
Cl1 C67 H67A 109.9 . . ?
Cl1 C67 H67B 109.9 . . ?
Cl1 C67 H67C 107.2 . . ?
Cl1 C67 H67D 107.2 . . ?
Cl1 C67 Cl2B 120.7(6) . . ?
Cl2A C67 Cl1 108.9(4) . . ?
Cl2A C67 H67A 109.9 . . ?
Cl2A C67 H67B 109.9 . . ?
H67A C67 H67B 108.3 . . ?
H67C C67 H67D 106.8 . . ?
Cl2B C67 H67C 107.2 . . ?
Cl2B C67 H67D 107.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O4 C18 C17 41.8(4) . . . . ?
Ho1 O4 C18 C13 -139.2(3) . . . . ?
Ho1 O1 C3 C2 -28.2(4) . . . . ?
Ho1 O1 C3 C4 150.7(4) . . . . ?
Ho1 O2 C2 C3 44.7(4) . . . . ?
Ho1 O2 C2 C7 -132.9(3) . . . . ?
Ho1 O10 C56 C50 -163.6(3) . . . . ?
Ho1 O10 C56 C57 14.7(6) . . . . ?
Ho1 O9 C43 C42 8.3(6) . . . . ?
Ho1 O9 C43 C44 -172.2(2) . . . . ?
Ho1 O11 C58 C59 171.6(2) . . . . ?
Ho1 O11 C58 C57 -5.2(6) . . . . ?
Ho1 O5 C17 C16 148.6(3) . . . . ?
Ho1 O5 C17 C18 -32.0(3) . . . . ?
Ho1 O7 C28 C29 66.2(4) . . . . ?
Ho1 O7 C28 C27 -117.5(4) . . . . ?
Ho1 O8 C41 C42 -30.3(5) . . . . ?
Ho1 O8 C41 C35 152.0(2) . . . . ?
Ni1 O4 C18 C17 165.2(2) . . . . ?
Ni1 O4 C18 C13 -15.9(5) . . . . ?
Ni1 O2 C2 C3 178.2(2) . . . . ?
Ni1 O2 C2 C7 0.6(6) . . . . ?
Ni1 O7 C28 C29 -166.3(2) . . . . ?
Ni1 O7 C28 C27 10.0(5) . . . . ?
Ni1 O6 C20 C21 167.6(2) . . . . ?
Ni1 O6 C20 C27 -10.7(5) . . . . ?
Ni1 N2 C12 C13 1.3(7) . . . . ?
Ni1 N2 C11 C10 -51.2(4) . . . . ?
Ni1 N1 C8 C7 -9.2(7) . . . . ?
Ni1 N1 C9 C10 -49.5(5) . . . . ?
O1 C3 C4 C5 -176.7(4) . . . . ?
O2 C2 C3 O1 -3.2(5) . . . . ?
O2 C2 C3 C4 177.8(4) . . . . ?
O2 C2 C7 C6 -178.9(4) . . . . ?
O2 C2 C7 C8 5.0(7) . . . . ?
O11 C58 C57 C56 2.3(6) . . . . ?
O5 C17 C16 C15 -179.8(4) . . . . ?
O5 C17 C18 O4 -1.0(5) . . . . ?
O5 C17 C18 C13 180.0(3) . . . . ?
O3 C10 C11 N2 110.3(4) . . . . ?
O3 C10 C9 N1 -56.1(5) . . . . ?
C37 C36 C35 C40 -0.1(6) . . . . ?
C37 C36 C35 C41 -176.2(4) . . . . ?
C24 C25 C26 C21 0.9(7) . . . . ?
C25 C24 C23 C22 -0.4(7) . . . . ?
C53 C52 C51 C50 1.1(7) . . . . ?
C36 C37 C38 C39 -0.1(6) . . . . ?
C36 C35 C40 C39 -0.7(6) . . . . ?
C36 C35 C41 O8 20.4(5) . . . . ?
C36 C35 C41 C42 -157.3(4) . . . . ?
C44 C49 C48 C47 0.3(7) . . . . ?
C44 C45 C46 C47 -0.4(8) . . . . ?
C59 C58 C57 C56 -174.4(4) . . . . ?
C59 C60 C61 C62 -1.1(6) . . . . ?
C29 C34 C33 C32 1.5(7) . . . . ?
C29 C30 C31 C32 2.2(7) . . . . ?
C49 C44 C43 O9 9.1(5) . . . . ?
C49 C44 C43 C42 -171.4(4) . . . . ?
C49 C44 C45 C46 -0.6(7) . . . . ?
C43 C42 C41 O8 -0.1(6) . . . . ?
C43 C42 C41 C35 177.4(4) . . . . ?
C43 C44 C49 C48 -176.9(4) . . . . ?
C43 C44 C45 C46 176.9(4) . . . . ?
C35 C40 C39 C38 1.1(6) . . . . ?
C21 C22 C23 C24 1.1(7) . . . . ?
C22 C21 C20 O6 27.6(5) . . . . ?
C22 C21 C20 C27 -154.0(4) . . . . ?
C22 C21 C26 C25 -0.1(6) . . . . ?
C40 C35 C41 O8 -155.5(3) . . . . ?
C40 C35 C41 C42 26.7(6) . . . . ?
C40 C39 C38 C37 -0.7(6) . . . . ?
C28 C29 C34 C33 177.4(4) . . . . ?
C28 C29 C30 C31 -179.2(4) . . . . ?
C28 C27 C20 O6 1.8(6) . . . . ?
C28 C27 C20 C21 -176.4(3) . . . . ?
C2 C3 C4 C5 2.0(6) . . . . ?
C2 C7 C8 N1 -0.2(7) . . . . ?
C20 C21 C22 C23 -179.4(4) . . . . ?
C20 C21 C26 C25 178.3(4) . . . . ?
C20 C27 C28 O7 -1.4(6) . . . . ?
C20 C27 C28 C29 174.8(3) . . . . ?
C17 C16 C15 C14 -1.1(7) . . . . ?
C52 C53 C54 C55 -0.5(7) . . . . ?
C52 C51 C50 C55 -1.2(6) . . . . ?
C52 C51 C50 C56 179.4(4) . . . . ?
C48 C47 C46 C45 1.4(7) . . . . ?
C13 C14 C15 C16 1.2(7) . . . . ?
C34 C29 C28 O7 34.1(5) . . . . ?
C34 C29 C28 C27 -142.5(4) . . . . ?
C34 C29 C30 C31 -0.9(6) . . . . ?
C34 C33 C32 C31 -0.2(7) . . . . ?
C41 C42 C43 O9 10.9(6) . . . . ?
C41 C42 C43 C44 -168.6(3) . . . . ?
C41 C35 C40 C39 175.3(4) . . . . ?
C51 C50 C55 C54 0.4(6) . . . . ?
C51 C50 C56 O10 -164.0(4) . . . . ?
C51 C50 C56 C57 17.7(6) . . . . ?
C38 C37 C36 C35 0.5(6) . . . . ?
C50 C55 C54 C53 0.4(6) . . . . ?
C65 C59 C58 O11 -27.2(5) . . . . ?
C65 C59 C58 C57 149.8(4) . . . . ?
C65 C59 C60 C61 -0.3(5) . . . . ?
C65 C63 C62 C61 -0.2(6) . . . . ?
C45 C44 C49 C48 0.7(6) . . . . ?
C45 C44 C43 O9 -168.4(4) . . . . ?
C45 C44 C43 C42 11.2(6) . . . . ?
C58 C59 C65 C63 -178.1(3) . . . . ?
C58 C59 C60 C61 179.2(3) . . . . ?
C58 C57 C56 O10 -6.6(6) . . . . ?
C58 C57 C56 C50 171.6(4) . . . . ?
C3 C2 C7 C6 3.5(6) . . . . ?
C3 C2 C7 C8 -172.6(4) . . . . ?
C19 O5 C17 C16 1.1(5) . . . . ?
C19 O5 C17 C18 -179.5(3) . . . . ?
C16 C17 C18 O4 178.4(3) . . . . ?
C16 C17 C18 C13 -0.6(6) . . . . ?
C60 C59 C65 C63 1.5(5) . . . . ?
C60 C59 C58 O11 153.3(4) . . . . ?
C60 C59 C58 C57 -29.8(5) . . . . ?
C60 C61 C62 C63 1.4(6) . . . . ?
C12 N2 C11 C10 124.4(4) . . . . ?
C12 C13 C14 C15 -176.9(4) . . . . ?
C12 C13 C18 O4 -2.6(6) . . . . ?
C12 C13 C18 C17 176.3(4) . . . . ?
C46 C47 C48 C49 -1.3(7) . . . . ?
C26 C21 C22 C23 -0.9(6) . . . . ?
C26 C21 C20 O6 -150.8(4) . . . . ?
C26 C21 C20 C27 27.6(5) . . . . ?
C55 C50 C56 O10 16.5(5) . . . . ?
C55 C50 C56 C57 -161.8(4) . . . . ?
C14 C13 C12 N2 -173.6(4) . . . . ?
C14 C13 C18 O4 -178.3(4) . . . . ?
C14 C13 C18 C17 0.6(6) . . . . ?
C6 C7 C8 N1 -176.3(4) . . . . ?
C6 C5 C4 C3 1.1(6) . . . . ?
C7 C2 C3 O1 174.6(3) . . . . ?
C7 C2 C3 C4 -4.4(6) . . . . ?
C7 C6 C5 C4 -1.9(7) . . . . ?
C18 C17 C16 C15 0.8(6) . . . . ?
C18 C13 C12 N2 10.7(7) . . . . ?
C18 C13 C14 C15 -1.0(7) . . . . ?
C8 N1 C9 C10 123.8(4) . . . . ?
C5 C6 C7 C2 -0.6(6) . . . . ?
C5 C6 C7 C8 175.8(4) . . . . ?
C33 C32 C31 C30 -1.7(8) . . . . ?
C23 C24 C25 C26 -0.6(8) . . . . ?
C11 N2 C12 C13 -173.9(4) . . . . ?
C11 C10 C9 N1 72.5(5) . . . . ?
C56 C50 C55 C54 179.9(4) . . . . ?
C1 O1 C3 C2 172.8(3) . . . . ?
C1 O1 C3 C4 -8.3(6) . . . . ?
C54 C53 C52 C51 -0.3(7) . . . . ?
C9 N1 C8 C7 178.2(4) . . . . ?
C9 C10 C11 N2 -17.0(5) . . . . ?
C30 C29 C28 O7 -147.6(4) . . . . ?
C30 C29 C28 C27 35.8(5) . . . . ?
C30 C29 C34 C33 -0.9(6) . . . . ?
C62 C63 C65 C59 -1.2(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.712
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_p131231h_sq
_database_code_depnum_ccdc_archive 'CCDC 1555629'
_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H58 Er2 N4 Ni2 O22'
_chemical_formula_sum            'C48 H58 Er2 N4 Ni2 O22'
_chemical_formula_weight         1494.88
_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'
Er Er -0.2586 4.9576 '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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.8413(3)
_cell_length_b                   14.1659(5)
_cell_length_c                   17.3158(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.402(2)
_cell_angle_gamma                90
_cell_volume                     3147.12(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8133
_cell_measurement_temperature    128.55(10)
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.0960
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12321
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.876
_diffrn_ambient_temperature      128.55(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5080
_reflns_number_total             5549
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies,Version 1.171.36.28'
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         0.939
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5539
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+1.4598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H10 of C10, H6 of C6, H5 of C5, {H22a,H22b} of C22, H15 of C15, H12 of C12,
  H14 of C14, {H9a,H9b} of C9, {H11a,H11b} of C11, H8 of C8, H16 of C16, H4 of
  C4
 At 1.5 times of:
  {H23a,H23b,H23c} of C23, {H21a,H21b,H21c} of C21, H11 of O11, {H19a,H19b,
  H19c} of C19, {H1a,H1b,H1c} of C1, H3 of O3
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 C22-H11
 1.907709 with sigma of 0.02
 Ni1-H11
 2.716305 with sigma of 0.02
3. Rigid bond restraints
 C24, O7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C24, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O7, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C24, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C24 ~ O6 ~ O8 ~ O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Ternary CH refined with riding coordinates:
 C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C22(H22a,H22b), C9(H9a,H9b)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C8(H8), C6(H6), C5(H5), C15(H15), C12(H12), C14(H14)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.00567(2) 0.86126(2) 0.50647(2) 0.01136(7) Uani 1 1 d . . . . .
Ni1 Ni 0.24489(3) 0.84078(3) 0.43531(3) 0.01376(11) Uani 1 1 d D . . . .
O2 O 0.09360(17) 0.83451(16) 0.39822(14) 0.0135(5) Uani 1 1 d . . . . .
O9 O -0.01910(18) 0.70769(18) 0.50205(14) 0.0194(6) Uani 1 1 d . . . . .
O1 O -0.10560(17) 0.85700(16) 0.38621(14) 0.0153(6) Uani 1 1 d . . . . .
O4 O 0.17653(17) 0.83918(16) 0.53920(14) 0.0154(6) Uani 1 1 d . . . . .
O5 O 0.04918(18) 0.87584(17) 0.64607(14) 0.0164(6) Uani 1 1 d . . . . .
O7 O -0.24385(19) 1.01125(16) 0.57280(16) 0.0185(6) Uani 1 1 d . U . . .
O11 O 0.24428(18) 0.69300(17) 0.43866(15) 0.0199(6) Uani 1 1 d D . . . .
H11 H 0.1893(17) 0.6632(13) 0.4207(17) 0.030 Uiso 1 1 d D U . . .
O8 O -0.16556(18) 0.87079(16) 0.55877(15) 0.0172(6) Uani 1 1 d . U . . .
O6 O -0.08810(19) 0.99779(15) 0.52152(17) 0.0189(6) Uani 1 1 d . U . . .
C18 C 0.2203(3) 0.8672(2) 0.6060(2) 0.0153(8) Uani 1 1 d . . . . .
O10 O 0.0593(2) 0.61745(18) 0.41589(18) 0.0297(7) Uani 1 1 d . . . . .
O3 O 0.4388(2) 0.9781(2) 0.3616(2) 0.0444(9) Uani 1 1 d . . . . .
H3 H 0.3832 0.9838 0.3826 0.067 Uiso 1 1 calc R U . . .
C13 C 0.3281(3) 0.8789(2) 0.6197(2) 0.0169(8) Uani 1 1 d . . . . .
C17 C 0.1547(3) 0.8844(2) 0.6676(2) 0.0149(8) Uani 1 1 d . . . . .
N2 N 0.3884(2) 0.8509(2) 0.4891(2) 0.0196(7) Uani 1 1 d . . . . .
N1 N 0.2882(2) 0.8329(2) 0.32376(18) 0.0170(7) Uani 1 1 d . . . . .
C1 C -0.2181(3) 0.8591(3) 0.3794(2) 0.0244(10) Uani 1 1 d . . . . .
H1A H -0.2459 0.8524 0.4298 0.037 Uiso 1 1 calc R U . . .
H1B H -0.2425 0.8081 0.3469 0.037 Uiso 1 1 calc R U . . .
H1C H -0.2406 0.9181 0.3572 0.037 Uiso 1 1 calc R U . . .
C4 C -0.1028(3) 0.8613(3) 0.2444(2) 0.0212(9) Uani 1 1 d . . . . .
H4 H -0.1748 0.8684 0.2391 0.025 Uiso 1 1 calc R U . . .
C24 C -0.1697(3) 0.9615(3) 0.5521(2) 0.0146(7) Uani 1 1 d . U . . .
C2 C 0.0544(3) 0.8428(2) 0.3269(2) 0.0125(8) Uani 1 1 d . . . . .
C19 C -0.0218(3) 0.8863(3) 0.7083(2) 0.0216(9) Uani 1 1 d . . . . .
H19A H -0.0198 0.9503 0.7266 0.032 Uiso 1 1 calc R U . . .
H19B H -0.0014 0.8444 0.7498 0.032 Uiso 1 1 calc R U . . .
H19C H -0.0913 0.8712 0.6898 0.032 Uiso 1 1 calc R U . . .
C7 C 0.1135(3) 0.8418(2) 0.2612(2) 0.0156(8) Uani 1 1 d . . . . .
C16 C 0.1928(3) 0.9069(3) 0.7407(2) 0.0217(9) Uani 1 1 d . . . . .
H16 H 0.1477 0.9161 0.7808 0.026 Uiso 1 1 calc R U . . .
C8 C 0.2263(3) 0.8333(3) 0.2640(2) 0.0190(8) Uani 1 1 d . . . . .
H8 H 0.2573 0.8274 0.2166 0.023 Uiso 1 1 calc R U . . .
C11 C 0.4833(3) 0.8424(3) 0.4439(3) 0.0316(11) Uani 1 1 d . . . . .
H11A H 0.5031 0.7764 0.4416 0.038 Uiso 1 1 calc R U . . .
H11B H 0.5398 0.8762 0.4706 0.038 Uiso 1 1 calc R U . . .
C3 C -0.0548(3) 0.8541(2) 0.3166(2) 0.0153(8) Uani 1 1 d . . . . .
C6 C 0.0630(3) 0.8486(3) 0.1878(2) 0.0211(9) Uani 1 1 d . . . . .
H6 H 0.1024 0.8465 0.1440 0.025 Uiso 1 1 calc R U . . .
C5 C -0.0430(3) 0.8580(3) 0.1795(2) 0.0249(10) Uani 1 1 d . . . . .
H5 H -0.0748 0.8622 0.1303 0.030 Uiso 1 1 calc R U . . .
C20 C -0.0154(3) 0.6378(2) 0.4553(2) 0.0200(9) Uani 1 1 d . . . . .
C22 C 0.2817(3) 0.6410(3) 0.5065(3) 0.0329(11) Uani 1 1 d D . . . .
H22A H 0.2228 0.6181 0.5344 0.039 Uiso 1 1 calc R U . . .
H22B H 0.3220 0.6828 0.5406 0.039 Uiso 1 1 calc R U . . .
C15 C 0.3006(3) 0.9156(3) 0.7537(2) 0.0248(9) Uani 1 1 d . . . . .
H15 H 0.3278 0.9296 0.8030 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4052(3) 0.8695(2) 0.5609(2) 0.0190(9) Uani 1 1 d . . . . .
H12 H 0.4745 0.8780 0.5774 0.023 Uiso 1 1 calc R U . . .
C14 C 0.3654(3) 0.9038(3) 0.6949(2) 0.0225(9) Uani 1 1 d . . . . .
H14 H 0.4366 0.9124 0.7042 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4000(3) 0.8202(3) 0.3089(2) 0.0273(10) Uani 1 1 d . . . . .
H9A H 0.4121 0.8372 0.2558 0.033 Uiso 1 1 calc R U . . .
H9B H 0.4184 0.7542 0.3158 0.033 Uiso 1 1 calc R U . . .
C10 C 0.4698(3) 0.8802(3) 0.3627(3) 0.0335(11) Uani 1 1 d . . . . .
H10 H 0.5392 0.8784 0.3412 0.040 Uiso 1 1 calc R U . . .
C21 C -0.1091(3) 0.5743(3) 0.4526(3) 0.0369(12) Uani 1 1 d . . . . .
H21A H -0.1127 0.5411 0.5007 0.055 Uiso 1 1 calc R U . . .
H21B H -0.1035 0.5296 0.4112 0.055 Uiso 1 1 calc R U . . .
H21C H -0.1710 0.6114 0.4440 0.055 Uiso 1 1 calc R U . . .
C23 C 0.3472(4) 0.5603(4) 0.4847(3) 0.0596(16) Uani 1 1 d . . . . .
H23A H 0.3081 0.5200 0.4496 0.089 Uiso 1 1 calc R U . . .
H23B H 0.3682 0.5253 0.5302 0.089 Uiso 1 1 calc R U . . .
H23C H 0.4079 0.5832 0.4601 0.089 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 Er1 3.9396(3) 3_576 ?
Er1 Ni1 3.3699(5) . ?
Er1 O2 2.260(2) . ?
Er1 O9 2.199(3) . ?
Er1 O1 2.476(2) . ?
Er1 O4 2.265(2) . ?
Er1 O5 2.467(2) . ?
Er1 O8 2.417(2) . ?
Er1 O6 2.299(2) . ?
Er1 O6 2.321(2) 3_576 ?
Er1 C24 2.804(3) . ?
Ni1 O2 2.022(2) . ?
Ni1 O4 2.035(3) . ?
Ni1 O7 2.101(2) 3_576 ?
Ni1 O11 2.094(2) . ?
Ni1 N2 2.035(3) . ?
Ni1 N1 2.035(3) . ?
O2 C2 1.319(4) . ?
O9 C20 1.281(4) . ?
O1 C1 1.445(4) . ?
O1 C3 1.395(5) . ?
O4 C18 1.326(4) . ?
O5 C17 1.396(4) . ?
O5 C19 1.448(4) . ?
O7 Ni1 2.101(2) 3_576 ?
O7 C24 1.249(4) . ?
O11 C22 1.452(5) . ?
O8 C24 1.292(4) . ?
O6 Er1 2.321(2) 3_576 ?
O6 C24 1.299(4) . ?
C18 C13 1.404(5) . ?
C18 C17 1.408(5) . ?
O10 C20 1.234(5) . ?
O3 C10 1.443(5) . ?
C13 C12 1.456(5) . ?
C13 C14 1.414(5) . ?
C17 C16 1.375(5) . ?
N2 C11 1.481(5) . ?
N2 C12 1.280(5) . ?
N1 C8 1.278(5) . ?
N1 C9 1.481(4) . ?
C4 C3 1.374(5) . ?
C4 C5 1.390(6) . ?
C2 C7 1.394(5) . ?
C2 C3 1.415(5) . ?
C7 C8 1.452(5) . ?
C7 C6 1.406(5) . ?
C16 C15 1.399(5) . ?
C11 C10 1.508(6) . ?
C6 C5 1.368(5) . ?
C20 C21 1.502(5) . ?
C22 C23 1.478(6) . ?
C15 C14 1.351(5) . ?
C9 C10 1.524(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ni1 Er1 Er1 95.575(9) . 3_576 ?
O2 Er1 Er1 97.97(6) . 3_576 ?
O2 Er1 Ni1 35.68(6) . . ?
O2 Er1 O1 65.75(8) . . ?
O2 Er1 O4 70.85(9) . . ?
O2 Er1 O5 136.56(8) . . ?
O2 Er1 O8 144.50(9) . . ?
O2 Er1 O6 121.15(9) . . ?
O2 Er1 O6 73.92(9) . 3_576 ?
O2 Er1 C24 138.89(9) . . ?
O9 Er1 Er1 168.52(6) . 3_576 ?
O9 Er1 Ni1 92.00(6) . . ?
O9 Er1 O2 83.22(9) . . ?
O9 Er1 O1 82.48(8) . . ?
O9 Er1 O4 90.53(9) . . ?
O9 Er1 O5 98.24(8) . . ?
O9 Er1 O8 86.32(8) . . ?
O9 Er1 O6 139.50(8) . . ?
O9 Er1 O6 155.56(9) . 3_576 ?
O9 Er1 C24 113.22(10) . . ?
O1 Er1 Er1 87.59(5) . 3_576 ?
O1 Er1 Ni1 101.14(6) . . ?
O1 Er1 C24 78.89(9) . . ?
O4 Er1 Er1 100.67(6) . 3_576 ?
O4 Er1 Ni1 36.02(6) . . ?
O4 Er1 O1 136.55(8) . . ?
O4 Er1 O5 65.73(8) . . ?
O4 Er1 O8 143.23(9) . . ?
O4 Er1 O6 74.07(9) . 3_576 ?
O4 Er1 O6 126.47(9) . . ?
O4 Er1 C24 141.31(9) . . ?
O5 Er1 Er1 88.76(5) . 3_576 ?
O5 Er1 Ni1 101.13(6) . . ?
O5 Er1 O1 157.69(8) . . ?
O5 Er1 C24 80.40(9) . . ?
O8 Er1 Er1 86.19(5) . 3_576 ?
O8 Er1 Ni1 178.19(6) . . ?
O8 Er1 O1 79.31(8) . . ?
O8 Er1 O5 78.48(8) . . ?
O8 Er1 C24 27.38(9) . . ?
O6 Er1 Er1 31.65(6) . 3_576 ?
O6 Er1 Er1 31.31(6) 3_576 3_576 ?
O6 Er1 Ni1 64.34(6) 3_576 . ?
O6 Er1 Ni1 127.14(6) . . ?
O6 Er1 O1 95.59(9) 3_576 . ?
O6 Er1 O1 80.18(9) . . ?
O6 Er1 O5 85.22(9) . . ?
O6 Er1 O5 92.64(9) 3_576 . ?
O6 Er1 O8 54.64(8) . . ?
O6 Er1 O8 117.41(8) 3_576 . ?
O6 Er1 O6 62.96(10) . 3_576 ?
O6 Er1 C24 27.27(9) . . ?
O6 Er1 C24 90.09(9) 3_576 . ?
C24 Er1 Er1 58.82(7) . 3_576 ?
C24 Er1 Ni1 154.39(7) . . ?
O2 Ni1 Er1 40.68(7) . . ?
O2 Ni1 O4 80.56(10) . . ?
O2 Ni1 O7 91.10(10) . 3_576 ?
O2 Ni1 O11 87.72(9) . . ?
O2 Ni1 N2 171.09(12) . . ?
O2 Ni1 N1 89.60(11) . . ?
O4 Ni1 Er1 40.89(6) . . ?
O4 Ni1 O7 93.93(10) . 3_576 ?
O4 Ni1 O11 87.83(10) . . ?
O4 Ni1 N2 90.68(12) . . ?
O4 Ni1 N1 169.61(10) . . ?
O7 Ni1 Er1 86.29(7) 3_576 . ?
O11 Ni1 Er1 94.09(7) . . ?
O11 Ni1 O7 177.70(11) . 3_576 ?
N2 Ni1 Er1 130.42(10) . . ?
N2 Ni1 O7 87.92(11) . 3_576 ?
N2 Ni1 O11 93.55(11) . . ?
N2 Ni1 N1 99.24(12) . . ?
N1 Ni1 Er1 129.87(8) . . ?
N1 Ni1 O7 89.57(11) . 3_576 ?
N1 Ni1 O11 88.45(11) . . ?
Ni1 O2 Er1 103.65(10) . . ?
C2 O2 Er1 125.2(2) . . ?
C2 O2 Ni1 128.1(2) . . ?
C20 O9 Er1 141.0(2) . . ?
C1 O1 Er1 127.4(2) . . ?
C3 O1 Er1 116.9(2) . . ?
C3 O1 C1 115.7(3) . . ?
Ni1 O4 Er1 103.09(10) . . ?
C18 O4 Er1 123.2(2) . . ?
C18 O4 Ni1 125.8(2) . . ?
C17 O5 Er1 116.5(2) . . ?
C17 O5 C19 115.2(3) . . ?
C19 O5 Er1 127.9(2) . . ?
C24 O7 Ni1 123.1(2) . 3_576 ?
C22 O11 Ni1 121.9(2) . . ?
C24 O8 Er1 93.25(19) . . ?
Er1 O6 Er1 117.04(10) . 3_576 ?
C24 O6 Er1 143.9(2) . 3_576 ?
C24 O6 Er1 98.6(2) . . ?
O4 C18 C13 124.1(4) . . ?
O4 C18 C17 117.9(3) . . ?
C13 C18 C17 117.9(3) . . ?
C18 C13 C12 124.5(4) . . ?
C18 C13 C14 118.6(4) . . ?
C14 C13 C12 116.9(3) . . ?
O5 C17 C18 112.8(3) . . ?
C16 C17 O5 124.7(3) . . ?
C16 C17 C18 122.5(3) . . ?
C11 N2 Ni1 120.1(3) . . ?
C12 N2 Ni1 124.9(3) . . ?
C12 N2 C11 114.9(3) . . ?
C8 N1 Ni1 125.7(3) . . ?
C8 N1 C9 115.7(3) . . ?
C9 N1 Ni1 118.5(2) . . ?
C3 C4 C5 119.4(4) . . ?
O7 C24 Er1 176.0(3) . . ?
O7 C24 O8 124.4(3) . . ?
O7 C24 O6 122.1(3) . . ?
O8 C24 Er1 59.37(17) . . ?
O8 C24 O6 113.5(3) . . ?
O6 C24 Er1 54.16(16) . . ?
O2 C2 C7 124.3(3) . . ?
O2 C2 C3 117.7(3) . . ?
C7 C2 C3 118.0(3) . . ?
C2 C7 C8 123.4(3) . . ?
C2 C7 C6 119.3(3) . . ?
C6 C7 C8 117.3(4) . . ?
C17 C16 C15 118.6(4) . . ?
N1 C8 C7 127.8(4) . . ?
N2 C11 C10 113.5(3) . . ?
O1 C3 C2 113.1(3) . . ?
C4 C3 O1 125.1(3) . . ?
C4 C3 C2 121.8(4) . . ?
C5 C6 C7 121.5(4) . . ?
C6 C5 C4 119.9(4) . . ?
O9 C20 C21 115.6(3) . . ?
O10 C20 O9 125.5(3) . . ?
O10 C20 C21 118.8(4) . . ?
O11 C22 C23 111.0(4) . . ?
C14 C15 C16 120.4(4) . . ?
N2 C12 C13 127.3(3) . . ?
C15 C14 C13 121.9(3) . . ?
N1 C9 C10 112.1(3) . . ?
O3 C10 C11 112.0(4) . . ?
O3 C10 C9 111.9(4) . . ?
C11 C10 C9 114.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Er1 O2 C2 C7 168.6(2) . . . . ?
Er1 O2 C2 C3 -10.9(4) . . . . ?
Er1 O9 C20 O10 52.0(6) . . . . ?
Er1 O9 C20 C21 -131.0(3) . . . . ?
Er1 O1 C3 C4 -172.9(3) . . . . ?
Er1 O1 C3 C2 7.1(4) . . . . ?
Er1 O4 C18 C13 -161.4(3) . . . . ?
Er1 O4 C18 C17 20.0(4) . . . . ?
Er1 O5 C17 C18 -10.1(3) . . . . ?
Er1 O5 C17 C16 170.0(3) . . . . ?
Er1 O8 C24 O7 -178.2(3) . . . . ?
Er1 O8 C24 O6 1.5(3) . . . . ?
Er1 O6 C24 Er1 -170.5(5) 3_576 . . . ?
Er1 O6 C24 O7 178.1(3) . . . . ?
Er1 O6 C24 O7 7.6(6) 3_576 . . . ?
Er1 O6 C24 O8 -1.6(3) . . . . ?
Er1 O6 C24 O8 -172.1(3) 3_576 . . . ?
Ni1 O2 C2 C7 11.4(5) . . . . ?
Ni1 O2 C2 C3 -168.1(2) . . . . ?
Ni1 O4 C18 C13 -17.6(5) . . . . ?
Ni1 O4 C18 C17 163.8(2) . . . . ?
Ni1 O7 C24 O8 177.6(3) 3_576 . . . ?
Ni1 O7 C24 O6 -2.1(5) 3_576 . . . ?
Ni1 O11 C22 C23 -136.4(3) . . . . ?
Ni1 N2 C11 C10 32.5(5) . . . . ?
Ni1 N2 C12 C13 5.9(5) . . . . ?
Ni1 N1 C8 C7 1.8(6) . . . . ?
Ni1 N1 C9 C10 -41.2(4) . . . . ?
O2 C2 C7 C8 -1.2(6) . . . . ?
O2 C2 C7 C6 178.2(3) . . . . ?
O2 C2 C3 O1 1.4(4) . . . . ?
O2 C2 C3 C4 -178.7(3) . . . . ?
O4 C18 C13 C12 5.4(6) . . . . ?
O4 C18 C13 C14 -176.4(3) . . . . ?
O4 C18 C17 O5 -4.8(4) . . . . ?
O4 C18 C17 C16 175.1(3) . . . . ?
O5 C17 C16 C15 -178.3(3) . . . . ?
C18 C13 C12 N2 0.9(6) . . . . ?
C18 C13 C14 C15 0.8(6) . . . . ?
C18 C17 C16 C15 1.9(6) . . . . ?
C13 C18 C17 O5 176.5(3) . . . . ?
C13 C18 C17 C16 -3.6(5) . . . . ?
C17 C18 C13 C12 -176.0(3) . . . . ?
C17 C18 C13 C14 2.2(5) . . . . ?
C17 C16 C15 C14 1.2(6) . . . . ?
N2 C11 C10 O3 57.8(4) . . . . ?
N2 C11 C10 C9 -71.0(5) . . . . ?
N1 C9 C10 O3 -52.5(5) . . . . ?
N1 C9 C10 C11 76.3(5) . . . . ?
C1 O1 C3 C4 6.0(5) . . . . ?
C1 O1 C3 C2 -174.1(3) . . . . ?
C2 C7 C8 N1 -5.9(6) . . . . ?
C2 C7 C6 C5 1.4(6) . . . . ?
C19 O5 C17 C18 175.9(3) . . . . ?
C19 O5 C17 C16 -3.9(5) . . . . ?
C7 C2 C3 O1 -178.1(3) . . . . ?
C7 C2 C3 C4 1.8(5) . . . . ?
C7 C6 C5 C4 0.1(6) . . . . ?
C16 C15 C14 C13 -2.5(6) . . . . ?
C8 N1 C9 C10 142.1(4) . . . . ?
C8 C7 C6 C5 -179.2(3) . . . . ?
C11 N2 C12 C13 -177.9(3) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C3 C2 C7 C8 178.3(3) . . . . ?
C3 C2 C7 C6 -2.3(5) . . . . ?
C6 C7 C8 N1 174.7(4) . . . . ?
C5 C4 C3 O1 179.6(3) . . . . ?
C5 C4 C3 C2 -0.4(6) . . . . ?
C12 C13 C14 C15 179.2(3) . . . . ?
C12 N2 C11 C10 -144.0(4) . . . . ?
C14 C13 C12 N2 -177.3(4) . . . . ?
C9 N1 C8 C7 178.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_te
_audit_block_doi                 10.5517/ccdc.csd.cc1p7lcw
_database_code_depnum_ccdc_archive 'CCDC 1556428'

_audit_update_record             
;
2017-08-14 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2017-07-31
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_sum            'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_weight         1119.15
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.232(3)
_cell_length_b                   12.6716(17)
_cell_length_c                   16.639(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.967(3)
_cell_angle_gamma                90
_cell_volume                     3807.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11694
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    2.474
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear grayish gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37786
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.595
_diffrn_reflns_theta_min         3.033
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9850
	          2theta: -15.1058
scan:
	Number of images: 300
	           Slice: -105.0000 - 45.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9850
	          2theta: -15.1058
scan:
	Number of images: 200
	           Slice: -105.0000 - -5.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9850
	          2theta: -15.1058
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.033845
_diffrn_orient_matrix_UB_12      -0.035873
_diffrn_orient_matrix_UB_13      0.035362
_diffrn_orient_matrix_UB_21      -0.064793
_diffrn_orient_matrix_UB_22      -0.039141
_diffrn_orient_matrix_UB_23      0.022309
_diffrn_orient_matrix_UB_31      0.010968
_diffrn_orient_matrix_UB_32      -0.039426
_diffrn_orient_matrix_UB_33      -0.037319
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8076
_reflns_number_total             8747
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         2.183
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8747
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0716
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+40.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2158
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H6 of C6, {H11A,H11B} of C11, H29 of C29, H24 of C24, H5 of C5, H8 of C8,
  H4 of C4, H10 of C10, {H9A,H9B} of C9, H14 of C14, H15 of C15, H16 of C16,
  H12 of C12
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, H12A of O12, H3 of O3, {H1A,H1B,H1C} of C1
2.a Rotating group:
 O12(H12A)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B)
2.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C12(H12), C4(H4), C8(H8), C5(H5), C24(H24),
 C29(H29), C6(H6)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.26874(2) 0.50302(3) 0.13418(2) 0.03532(15) Uani 1 1 d . . . . .
Ni1 Ni 0.11186(6) 0.50810(7) 0.22637(6) 0.0321(2) Uani 1 1 d . . . . .
F15 F 0.2288(3) 0.1420(5) 0.2451(4) 0.0687(18) Uani 1 1 d . . . . .
F13 F 0.3179(5) 0.0633(5) 0.1997(5) 0.095(3) Uani 1 1 d . . . . .
F1 F 0.1144(5) 0.8724(7) 0.1971(6) 0.106(3) Uani 1 1 d . . . . .
F14 F 0.3351(4) 0.1491(7) 0.3092(4) 0.090(3) Uani 1 1 d . . . . .
F3 F 0.1347(5) 0.8532(7) 0.0744(5) 0.103(3) Uani 1 1 d . . . . .
F5 F 0.2859(4) 0.7453(5) -0.1549(3) 0.0641(16) Uani 1 1 d . . . . .
F7 F 0.4489(3) 0.8560(5) 0.0726(4) 0.0640(17) Uani 1 1 d . . . . .
F4 F 0.1812(4) 0.7085(7) -0.1182(4) 0.086(2) Uani 1 1 d . . . . .
F2 F 0.2233(5) 0.8764(6) 0.1662(6) 0.094(2) Uani 1 1 d . . . . .
F6 F 0.2449(5) 0.5858(5) -0.1595(4) 0.089(3) Uani 1 1 d . . . . .
F8 F 0.3973(4) 0.8474(6) 0.1801(5) 0.088(2) Uani 1 1 d . . . . .
F12 F 0.5101(5) 0.2258(7) 0.0916(6) 0.107(3) Uani 1 1 d . . . . .
F9 F 0.4859(3) 0.7463(5) 0.1637(4) 0.0666(17) Uani 1 1 d . . . . .
F10 F 0.4697(5) 0.3372(8) 0.0003(4) 0.095(3) Uani 1 1 d . . . . .
F11 F 0.5268(4) 0.3908(9) 0.1099(6) 0.116(3) Uani 1 1 d . . . . .
O3 O -0.0026(5) 0.7112(7) 0.2862(6) 0.072(2) Uani 1 1 d . . . . .
H3 H 0.0364 0.7056 0.2672 0.108 Uiso 1 1 calc R U . . .
O1 O 0.2167(3) 0.3656(5) 0.0225(3) 0.0389(12) Uani 1 1 d . . . . .
O4 O 0.2215(3) 0.5161(4) 0.2574(3) 0.0288(10) Uani 1 1 d . . . . .
O12 O 0.1220(3) 0.3421(5) 0.2562(3) 0.0381(12) Uani 1 1 d . . . . .
H12A H 0.0821 0.3091 0.2361 0.057 Uiso 1 1 d R U . . .
O2 O 0.1431(3) 0.4713(4) 0.1172(3) 0.0308(10) Uani 1 1 d . . . . .
O8 O 0.2602(3) 0.5720(4) 0.0012(3) 0.0373(12) Uani 1 1 d . . . . .
O9 O 0.3592(3) 0.6359(5) 0.1343(3) 0.0430(13) Uani 1 1 d . . . . .
O7 O 0.2126(3) 0.6723(4) 0.1357(4) 0.0439(13) Uani 1 1 d . . . . .
O11 O 0.2691(3) 0.3221(4) 0.1885(3) 0.0365(11) Uani 1 1 d . . . . .
O6 O 0.1126(3) 0.6689(4) 0.2012(3) 0.0367(12) Uani 1 1 d . . . . .
O5 O 0.3621(3) 0.4942(5) 0.2670(4) 0.0411(13) Uani 1 1 d . . . . .
O10 O 0.3735(3) 0.4174(5) 0.0980(4) 0.0467(14) Uani 1 1 d . . . . .
N2 N 0.0940(4) 0.5314(6) 0.3423(4) 0.0399(15) Uani 1 1 d . . . . .
N1 N 0.0035(4) 0.5008(6) 0.1790(4) 0.0404(15) Uani 1 1 d . . . . .
C21 C 0.1544(6) 0.8268(7) 0.1555(6) 0.057(3) Uani 1 1 d . . . . .
C31 C 0.2990(6) 0.1476(8) 0.2347(6) 0.052(2) Uani 1 1 d . . . . .
C19 C 0.4411(5) 0.5081(8) 0.2715(6) 0.051(2) Uani 1 1 d . . . . .
H19A H 0.4653 0.4412 0.2815 0.076 Uiso 1 1 calc R U . . .
H19B H 0.4581 0.5559 0.3149 0.076 Uiso 1 1 calc R U . . .
H19C H 0.4524 0.5366 0.2212 0.076 Uiso 1 1 calc R U . . .
C10 C -0.0321(5) 0.6096(8) 0.2968(6) 0.053(2) Uani 1 1 d . . . . .
H10 H -0.0782 0.6212 0.3196 0.063 Uiso 1 1 calc R U . . .
C9 C -0.0547(5) 0.5550(10) 0.2152(6) 0.056(2) Uani 1 1 d . . . . .
H9A H -0.0930 0.5040 0.2219 0.068 Uiso 1 1 calc R U . . .
H9B H -0.0766 0.6077 0.1768 0.068 Uiso 1 1 calc R U . . .
C14 C 0.2649(5) 0.4791(7) 0.4772(5) 0.0438(19) Uani 1 1 d . . . . .
H14 H 0.2424 0.4775 0.5240 0.053 Uiso 1 1 calc R U . . .
C15 C 0.3399(6) 0.4630(8) 0.4829(5) 0.051(2) Uani 1 1 d . . . . .
H15 H 0.3673 0.4491 0.5332 0.061 Uiso 1 1 calc R U . . .
C18 C 0.2570(5) 0.5000(6) 0.3310(5) 0.0350(16) Uani 1 1 d . . . . .
C3 C 0.1420(5) 0.3438(6) 0.0148(4) 0.0356(16) Uani 1 1 d . . . . .
C25 C 0.3697(4) 0.7085(6) 0.0880(5) 0.0358(16) Uani 1 1 d . . . . .
C23 C 0.2851(4) 0.6535(6) -0.0287(5) 0.0341(15) Uani 1 1 d . . . . .
C16 C 0.3755(5) 0.4674(7) 0.4137(6) 0.0450(19) Uani 1 1 d . . . . .
H16 H 0.4264 0.4572 0.4179 0.054 Uiso 1 1 calc R U . . .
C30 C 0.3162(5) 0.2495(6) 0.1898(5) 0.0390(17) Uani 1 1 d . . . . .
C12 C 0.1443(5) 0.5187(6) 0.4026(5) 0.0418(18) Uani 1 1 d . . . . .
H12 H 0.1289 0.5235 0.4535 0.050 Uiso 1 1 calc R U . . .
C20 C 0.1614(5) 0.7104(7) 0.1651(5) 0.0409(19) Uani 1 1 d . . . . .
C17 C 0.3341(5) 0.4871(6) 0.3385(5) 0.0382(17) Uani 1 1 d . . . . .
C4 C 0.1048(5) 0.2719(7) -0.0389(5) 0.0439(19) Uani 1 1 d . . . . .
H4 H 0.1303 0.2321 -0.0729 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1035(4) 0.4029(6) 0.0682(4) 0.0321(15) Uani 1 1 d . . . . .
C8 C -0.0194(5) 0.4470(7) 0.1151(5) 0.0392(17) Uani 1 1 d . . . . .
H8 H -0.0703 0.4435 0.0997 0.047 Uiso 1 1 calc R U . . .
C5 C 0.0284(6) 0.2602(7) -0.0412(6) 0.054(2) Uani 1 1 d . . . . .
H5 H 0.0032 0.2121 -0.0772 0.065 Uiso 1 1 calc R U . . .
C26 C 0.4255(5) 0.7918(7) 0.1272(6) 0.0448(19) Uani 1 1 d . . . . .
C24 C 0.3364(4) 0.7240(6) 0.0077(5) 0.0342(15) Uani 1 1 d . . . . .
H24 H 0.3492 0.7825 -0.0211 0.041 Uiso 1 1 calc R U . . .
C13 C 0.2216(5) 0.4979(6) 0.4023(5) 0.0399(18) Uani 1 1 d . . . . .
C22 C 0.2501(6) 0.6726(8) -0.1170(6) 0.055(2) Uani 1 1 d . . . . .
C29 C 0.3825(5) 0.2498(8) 0.1574(5) 0.048(2) Uani 1 1 d . . . . .
H29 H 0.4129 0.1907 0.1655 0.058 Uiso 1 1 calc R U . . .
C1 C 0.2532(6) 0.3349(9) -0.0453(5) 0.052(2) Uani 1 1 d . . . . .
H1A H 0.2238 0.3565 -0.0950 0.078 Uiso 1 1 calc R U . . .
H1B H 0.2593 0.2596 -0.0453 0.078 Uiso 1 1 calc R U . . .
H1C H 0.3009 0.3681 -0.0408 0.078 Uiso 1 1 calc R U . . .
C7 C 0.0268(4) 0.3907(6) 0.0641(5) 0.0350(16) Uani 1 1 d . . . . .
C27 C 0.4794(6) 0.3227(11) 0.0785(7) 0.068(3) Uani 1 1 d . . . . .
C11 C 0.0176(5) 0.5445(8) 0.3601(5) 0.0464(19) Uani 1 1 d . . . . .
H11A H 0.0191 0.5784 0.4126 0.056 Uiso 1 1 calc R U . . .
H11B H -0.0043 0.4753 0.3639 0.056 Uiso 1 1 calc R U . . .
C6 C -0.0102(5) 0.3176(8) 0.0084(5) 0.047(2) Uani 1 1 d . . . . .
H6 H -0.0611 0.3086 0.0056 0.057 Uiso 1 1 calc R U . . .
C28 C 0.4050(5) 0.3318(8) 0.1145(5) 0.048(2) Uani 1 1 d . . . . .
H12B H 0.153(5) 0.314(8) 0.234(6) 0.04(3) 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
Tb1 Ni1 3.4285(12) . ?
Tb1 O1 2.626(5) . ?
Tb1 O4 2.338(5) . ?
Tb1 O2 2.304(5) . ?
Tb1 O8 2.364(5) . ?
Tb1 O9 2.357(6) . ?
Tb1 O7 2.379(6) . ?
Tb1 O11 2.464(5) . ?
Tb1 O5 2.598(6) . ?
Tb1 O10 2.346(6) . ?
Ni1 O4 1.997(5) . ?
Ni1 O12 2.164(6) . ?
Ni1 O2 2.032(5) . ?
Ni1 O6 2.080(6) . ?
Ni1 N2 2.022(7) . ?
Ni1 N1 2.026(7) . ?
F15 C31 1.316(12) . ?
F13 C31 1.286(11) . ?
F1 C21 1.219(13) . ?
F14 C31 1.322(12) . ?
F3 C21 1.388(12) . ?
F5 C22 1.337(11) . ?
F7 C26 1.332(11) . ?
F4 C22 1.333(13) . ?
F2 C21 1.393(13) . ?
F6 C22 1.306(12) . ?
F8 C26 1.290(11) . ?
F12 C27 1.355(15) . ?
F9 C26 1.315(10) . ?
F10 C27 1.301(13) . ?
F11 C27 1.281(16) . ?
O3 H3 0.8200 . ?
O3 C10 1.416(14) . ?
O1 C3 1.378(10) . ?
O1 C1 1.442(9) . ?
O4 C18 1.320(9) . ?
O12 H12A 0.8641 . ?
O12 H12B 0.80(10) . ?
O2 C2 1.332(8) . ?
O8 C23 1.258(9) . ?
O9 C25 1.232(10) . ?
O7 C20 1.212(11) . ?
O11 C30 1.256(10) . ?
O6 C20 1.257(10) . ?
O5 C19 1.443(10) . ?
O5 C17 1.362(11) . ?
O10 C28 1.240(12) . ?
N2 C12 1.271(11) . ?
N2 C11 1.474(11) . ?
N1 C9 1.462(12) . ?
N1 C8 1.282(11) . ?
C21 C20 1.486(12) . ?
C31 C30 1.546(12) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C10 H10 0.9800 . ?
C10 C9 1.529(14) . ?
C10 C11 1.532(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14 0.9300 . ?
C14 C15 1.372(14) . ?
C14 C13 1.401(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(14) . ?
C18 C17 1.403(12) . ?
C18 C13 1.426(13) . ?
C3 C4 1.386(10) . ?
C3 C2 1.418(11) . ?
C25 C26 1.546(11) . ?
C25 C24 1.403(11) . ?
C23 C24 1.372(11) . ?
C23 C22 1.537(12) . ?
C16 H16 0.9300 . ?
C16 C17 1.391(11) . ?
C30 C29 1.390(12) . ?
C12 H12 0.9300 . ?
C12 C13 1.434(13) . ?
C4 H4 0.9300 . ?
C4 C5 1.396(14) . ?
C2 C7 1.399(11) . ?
C8 H8 0.9300 . ?
C8 C7 1.461(12) . ?
C5 H5 0.9300 . ?
C5 C6 1.367(14) . ?
C24 H24 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.356(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C7 C6 1.413(11) . ?
C27 C28 1.562(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 Ni1 94.97(12) . . ?
O4 Tb1 Ni1 34.36(12) . . ?
O4 Tb1 O1 121.77(17) . . ?
O4 Tb1 O8 144.15(19) . . ?
O4 Tb1 O9 106.94(19) . . ?
O4 Tb1 O7 73.43(19) . . ?
O4 Tb1 O11 74.15(17) . . ?
O4 Tb1 O5 62.26(19) . . ?
O4 Tb1 O10 132.05(19) . . ?
O2 Tb1 Ni1 35.04(12) . . ?
O2 Tb1 O1 62.73(18) . . ?
O2 Tb1 O4 68.83(18) . . ?
O2 Tb1 O8 90.85(18) . . ?
O2 Tb1 O9 143.97(19) . . ?
O2 Tb1 O7 74.72(19) . . ?
O2 Tb1 O11 80.48(18) . . ?
O2 Tb1 O5 128.28(18) . . ?
O2 Tb1 O10 135.9(2) . . ?
O8 Tb1 Ni1 117.47(14) . . ?
O8 Tb1 O1 67.21(17) . . ?
O8 Tb1 O7 72.8(2) . . ?
O8 Tb1 O11 133.14(18) . . ?
O8 Tb1 O5 139.67(18) . . ?
O9 Tb1 Ni1 127.84(16) . . ?
O9 Tb1 O1 131.21(19) . . ?
O9 Tb1 O8 72.06(18) . . ?
O9 Tb1 O7 70.0(2) . . ?
O9 Tb1 O11 134.26(19) . . ?
O9 Tb1 O5 69.76(18) . . ?
O7 Tb1 Ni1 65.86(15) . . ?
O7 Tb1 O1 119.5(2) . . ?
O7 Tb1 O11 144.51(19) . . ?
O7 Tb1 O5 105.2(2) . . ?
O11 Tb1 Ni1 79.24(13) . . ?
O11 Tb1 O1 67.96(18) . . ?
O11 Tb1 O5 71.32(18) . . ?
O5 Tb1 Ni1 96.26(14) . . ?
O5 Tb1 O1 134.67(19) . . ?
O10 Tb1 Ni1 151.95(15) . . ?
O10 Tb1 O1 74.9(2) . . ?
O10 Tb1 O8 83.2(2) . . ?
O10 Tb1 O9 74.7(2) . . ?
O10 Tb1 O7 141.9(2) . . ?
O10 Tb1 O11 72.7(2) . . ?
O10 Tb1 O5 74.8(2) . . ?
O4 Ni1 Tb1 41.36(15) . . ?
O4 Ni1 O12 86.6(2) . . ?
O4 Ni1 O2 81.3(2) . . ?
O4 Ni1 O6 88.2(2) . . ?
O4 Ni1 N2 91.9(3) . . ?
O4 Ni1 N1 172.2(3) . . ?
O12 Ni1 Tb1 91.99(18) . . ?
O2 Ni1 Tb1 40.62(14) . . ?
O2 Ni1 O12 87.5(2) . . ?
O2 Ni1 O6 92.0(2) . . ?
O6 Ni1 Tb1 84.24(16) . . ?
O6 Ni1 O12 174.7(2) . . ?
N2 Ni1 Tb1 133.2(2) . . ?
N2 Ni1 O12 86.7(3) . . ?
N2 Ni1 O2 171.3(3) . . ?
N2 Ni1 O6 93.1(3) . . ?
N2 Ni1 N1 95.8(3) . . ?
N1 Ni1 Tb1 130.9(2) . . ?
N1 Ni1 O12 95.3(3) . . ?
N1 Ni1 O2 91.2(3) . . ?
N1 Ni1 O6 90.0(3) . . ?
C10 O3 H3 109.5 . . ?
C3 O1 Tb1 117.0(4) . . ?
C3 O1 C1 115.6(6) . . ?
C1 O1 Tb1 124.9(5) . . ?
Ni1 O4 Tb1 104.3(2) . . ?
C18 O4 Tb1 127.6(5) . . ?
C18 O4 Ni1 125.2(5) . . ?
Ni1 O12 H12A 110.0 . . ?
Ni1 O12 H12B 112(7) . . ?
H12A O12 H12B 102.8 . . ?
Ni1 O2 Tb1 104.3(2) . . ?
C2 O2 Tb1 129.3(5) . . ?
C2 O2 Ni1 120.1(5) . . ?
C23 O8 Tb1 133.9(5) . . ?
C25 O9 Tb1 134.6(5) . . ?
C20 O7 Tb1 136.1(5) . . ?
C30 O11 Tb1 130.9(5) . . ?
C20 O6 Ni1 122.1(5) . . ?
C19 O5 Tb1 124.8(5) . . ?
C17 O5 Tb1 117.8(5) . . ?
C17 O5 C19 117.1(7) . . ?
C28 O10 Tb1 135.7(6) . . ?
C12 N2 Ni1 122.7(6) . . ?
C12 N2 C11 116.9(7) . . ?
C11 N2 Ni1 119.4(5) . . ?
C9 N1 Ni1 122.8(6) . . ?
C8 N1 Ni1 122.3(6) . . ?
C8 N1 C9 114.9(8) . . ?
F1 C21 F3 110.1(9) . . ?
F1 C21 F2 108.2(8) . . ?
F1 C21 C20 117.3(11) . . ?
F3 C21 F2 97.1(10) . . ?
F3 C21 C20 110.5(7) . . ?
F2 C21 C20 111.8(7) . . ?
F15 C31 F14 104.1(8) . . ?
F15 C31 C30 111.9(8) . . ?
F13 C31 F15 110.0(9) . . ?
F13 C31 F14 107.9(10) . . ?
F13 C31 C30 113.0(7) . . ?
F14 C31 C30 109.5(8) . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C10 H10 105.8 . . ?
O3 C10 C9 111.1(9) . . ?
O3 C10 C11 112.1(9) . . ?
C9 C10 H10 105.8 . . ?
C11 C10 H10 105.8 . . ?
C11 C10 C9 115.4(8) . . ?
N1 C9 C10 117.2(7) . . ?
N1 C9 H9A 108.0 . . ?
N1 C9 H9B 108.0 . . ?
C10 C9 H9A 108.0 . . ?
C10 C9 H9B 108.0 . . ?
H9A C9 H9B 107.2 . . ?
C15 C14 H14 119.3 . . ?
C15 C14 C13 121.4(9) . . ?
C13 C14 H14 119.3 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.5(8) . . ?
C16 C15 H15 119.8 . . ?
O4 C18 C17 117.2(7) . . ?
O4 C18 C13 123.6(8) . . ?
C17 C18 C13 119.2(8) . . ?
O1 C3 C4 125.5(8) . . ?
O1 C3 C2 113.8(6) . . ?
C4 C3 C2 120.7(8) . . ?
O9 C25 C26 113.3(7) . . ?
O9 C25 C24 128.0(7) . . ?
C24 C25 C26 118.6(7) . . ?
O8 C23 C24 128.4(7) . . ?
O8 C23 C22 112.5(7) . . ?
C24 C23 C22 119.1(7) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 C15 119.5(9) . . ?
C17 C16 H16 120.3 . . ?
O11 C30 C31 115.9(7) . . ?
O11 C30 C29 128.4(8) . . ?
C29 C30 C31 115.7(8) . . ?
N2 C12 H12 115.8 . . ?
N2 C12 C13 128.4(8) . . ?
C13 C12 H12 115.8 . . ?
O7 C20 O6 131.4(8) . . ?
O7 C20 C21 114.3(8) . . ?
O6 C20 C21 114.3(9) . . ?
O5 C17 C18 114.0(7) . . ?
O5 C17 C16 125.1(8) . . ?
C16 C17 C18 120.9(8) . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(8) . . ?
C5 C4 H4 120.5 . . ?
O2 C2 C3 117.0(7) . . ?
O2 C2 C7 123.6(7) . . ?
C7 C2 C3 119.3(7) . . ?
N1 C8 H8 116.8 . . ?
N1 C8 C7 126.4(7) . . ?
C7 C8 H8 116.8 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(8) . . ?
C6 C5 H5 119.3 . . ?
F7 C26 C25 112.6(7) . . ?
F8 C26 F7 109.2(8) . . ?
F8 C26 F9 108.1(8) . . ?
F8 C26 C25 111.1(7) . . ?
F9 C26 F7 104.8(7) . . ?
F9 C26 C25 110.8(7) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 C25 120.5(7) . . ?
C23 C24 H24 119.7 . . ?
C14 C13 C18 118.5(9) . . ?
C14 C13 C12 117.5(8) . . ?
C18 C13 C12 123.9(8) . . ?
F5 C22 C23 113.3(8) . . ?
F4 C22 F5 106.2(8) . . ?
F4 C22 C23 109.6(8) . . ?
F6 C22 F5 109.1(9) . . ?
F6 C22 F4 106.3(9) . . ?
F6 C22 C23 112.0(8) . . ?
C30 C29 H29 118.4 . . ?
C28 C29 C30 123.3(9) . . ?
C28 C29 H29 118.4 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C7 C8 124.8(7) . . ?
C2 C7 C6 119.1(8) . . ?
C6 C7 C8 116.1(7) . . ?
F12 C27 C28 111.5(9) . . ?
F10 C27 F12 106.6(11) . . ?
F10 C27 C28 111.7(9) . . ?
F11 C27 F12 107.7(11) . . ?
F11 C27 F10 107.7(11) . . ?
F11 C27 C28 111.5(10) . . ?
N2 C11 C10 114.1(7) . . ?
N2 C11 H11A 108.7 . . ?
N2 C11 H11B 108.7 . . ?
C10 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C5 C6 C7 120.4(8) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
O10 C28 C29 128.5(8) . . ?
O10 C28 C27 112.3(9) . . ?
C29 C28 C27 119.2(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C3 C4 -178.3(6) . . . . ?
Tb1 O1 C3 C2 1.8(8) . . . . ?
Tb1 O4 C18 C17 9.3(9) . . . . ?
Tb1 O4 C18 C13 -172.5(5) . . . . ?
Tb1 O2 C2 C3 -3.8(9) . . . . ?
Tb1 O2 C2 C7 179.5(5) . . . . ?
Tb1 O8 C23 C24 10.6(13) . . . . ?
Tb1 O8 C23 C22 -168.2(6) . . . . ?
Tb1 O9 C25 C26 164.3(6) . . . . ?
Tb1 O9 C25 C24 -14.1(14) . . . . ?
Tb1 O7 C20 O6 -8.1(14) . . . . ?
Tb1 O7 C20 C21 173.1(5) . . . . ?
Tb1 O11 C30 C31 176.2(5) . . . . ?
Tb1 O11 C30 C29 -2.4(13) . . . . ?
Tb1 O5 C17 C18 -8.2(8) . . . . ?
Tb1 O5 C17 C16 170.8(7) . . . . ?
Tb1 O10 C28 C29 6.9(16) . . . . ?
Tb1 O10 C28 C27 -173.8(7) . . . . ?
Ni1 O4 C18 C17 167.0(5) . . . . ?
Ni1 O4 C18 C13 -14.8(10) . . . . ?
Ni1 O2 C2 C3 -151.5(5) . . . . ?
Ni1 O2 C2 C7 31.8(9) . . . . ?
Ni1 O6 C20 O7 3.4(12) . . . . ?
Ni1 O6 C20 C21 -177.7(5) . . . . ?
Ni1 N2 C12 C13 7.2(13) . . . . ?
Ni1 N2 C11 C10 -38.9(10) . . . . ?
Ni1 N1 C9 C10 -6.4(13) . . . . ?
Ni1 N1 C8 C7 -4.7(12) . . . . ?
F15 C31 C30 O11 17.5(11) . . . . ?
F15 C31 C30 C29 -163.7(8) . . . . ?
F13 C31 C30 O11 142.3(9) . . . . ?
F13 C31 C30 C29 -38.9(13) . . . . ?
F1 C21 C20 O7 -165.5(9) . . . . ?
F1 C21 C20 O6 15.5(11) . . . . ?
F14 C31 C30 O11 -97.4(10) . . . . ?
F14 C31 C30 C29 81.4(10) . . . . ?
F3 C21 C20 O7 67.3(11) . . . . ?
F3 C21 C20 O6 -111.8(10) . . . . ?
F2 C21 C20 O7 -39.7(11) . . . . ?
F2 C21 C20 O6 141.2(8) . . . . ?
F12 C27 C28 O10 -175.2(10) . . . . ?
F12 C27 C28 C29 4.2(15) . . . . ?
F10 C27 C28 O10 -56.1(14) . . . . ?
F10 C27 C28 C29 123.3(11) . . . . ?
F11 C27 C28 O10 64.4(13) . . . . ?
F11 C27 C28 C29 -116.3(12) . . . . ?
O3 C10 C9 N1 83.2(11) . . . . ?
O3 C10 C11 N2 -56.9(11) . . . . ?
O1 C3 C4 C5 -178.5(8) . . . . ?
O1 C3 C2 O2 0.8(9) . . . . ?
O1 C3 C2 C7 177.7(6) . . . . ?
O4 C18 C17 O5 0.5(10) . . . . ?
O4 C18 C17 C16 -178.5(7) . . . . ?
O4 C18 C13 C14 179.4(7) . . . . ?
O4 C18 C13 C12 -3.4(12) . . . . ?
O2 C2 C7 C8 -3.0(11) . . . . ?
O2 C2 C7 C6 178.4(7) . . . . ?
O8 C23 C24 C25 1.6(13) . . . . ?
O8 C23 C22 F5 -167.1(8) . . . . ?
O8 C23 C22 F4 74.5(10) . . . . ?
O8 C23 C22 F6 -43.2(12) . . . . ?
O9 C25 C26 F7 165.8(7) . . . . ?
O9 C25 C26 F8 -71.4(10) . . . . ?
O9 C25 C26 F9 48.8(10) . . . . ?
O9 C25 C24 C23 0.1(13) . . . . ?
O11 C30 C29 C28 -3.1(15) . . . . ?
N2 C12 C13 C14 -175.3(9) . . . . ?
N2 C12 C13 C18 7.5(14) . . . . ?
N1 C8 C7 C2 -12.7(13) . . . . ?
N1 C8 C7 C6 165.9(8) . . . . ?
C31 C30 C29 C28 178.3(9) . . . . ?
C19 O5 C17 C18 165.0(7) . . . . ?
C19 O5 C17 C16 -16.0(12) . . . . ?
C9 N1 C8 C7 176.0(8) . . . . ?
C9 C10 C11 N2 71.7(11) . . . . ?
C14 C15 C16 C17 -0.7(14) . . . . ?
C15 C14 C13 C18 0.1(13) . . . . ?
C15 C14 C13 C12 -177.2(8) . . . . ?
C15 C16 C17 O5 179.4(8) . . . . ?
C15 C16 C17 C18 -1.7(13) . . . . ?
C3 C4 C5 C6 -0.2(14) . . . . ?
C3 C2 C7 C8 -179.6(7) . . . . ?
C3 C2 C7 C6 1.8(11) . . . . ?
C30 C29 C28 O10 1.1(16) . . . . ?
C30 C29 C28 C27 -178.2(9) . . . . ?
C12 N2 C11 C10 152.1(8) . . . . ?
C17 C18 C13 C14 -2.4(11) . . . . ?
C17 C18 C13 C12 174.7(7) . . . . ?
C4 C3 C2 O2 -179.2(7) . . . . ?
C4 C3 C2 C7 -2.3(11) . . . . ?
C4 C5 C6 C7 -0.3(15) . . . . ?
C2 C3 C4 C5 1.5(12) . . . . ?
C2 C7 C6 C5 -0.5(13) . . . . ?
C8 N1 C9 C10 173.0(9) . . . . ?
C8 C7 C6 C5 -179.2(8) . . . . ?
C26 C25 C24 C23 -178.3(7) . . . . ?
C24 C25 C26 F7 -15.6(11) . . . . ?
C24 C25 C26 F8 107.2(10) . . . . ?
C24 C25 C26 F9 -132.6(8) . . . . ?
C24 C23 C22 F5 13.9(13) . . . . ?
C24 C23 C22 F4 -104.4(9) . . . . ?
C24 C23 C22 F6 137.8(9) . . . . ?
C13 C14 C15 C16 1.4(14) . . . . ?
C13 C18 C17 O5 -177.8(7) . . . . ?
C13 C18 C17 C16 3.2(11) . . . . ?
C22 C23 C24 C25 -179.6(8) . . . . ?
C1 O1 C3 C4 19.0(11) . . . . ?
C1 O1 C3 C2 -161.0(7) . . . . ?
C11 N2 C12 C13 175.8(8) . . . . ?
C11 C10 C9 N1 -45.9(13) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
####################################################################### 
# 
# 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_y
_database_code_depnum_ccdc_archive 'CCDC 1522434'
_audit_update_record             
;
2017-01-02 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_audit_creation_date             2016-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_sum            'C31 H24 F15 N2 Ni O12 Tb'
_chemical_formula_weight         1119.14
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Ni 0.35663 1.12491 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410005569
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.01794 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Tb -0.07738 4.17970 25.89760 18.21850 14.31670 2.95354 2.24256 0.19614 12.66480
115.36200 3.5832400322
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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

_symmetry_Int_Tables_number      14
_cell_length_a                   18.2854(7)
_cell_length_b                   12.6822(4)
_cell_length_c                   16.6662(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.946(4)
_cell_angle_gamma                90
_cell_volume                     3827.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11694
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    2.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   Multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.9418
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       prism
_exptl_crystal_F_000             2194.9558
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37786
_diffrn_reflns_theta_full        25.9982
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -105.0000 - 75.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9850
	          2theta: -15.1058
scan:
	Number of images: 300
	           Slice: -105.0000 - 45.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9850
	          2theta: -15.1058
scan:
	Number of images: 200
	           Slice: -105.0000 - -5.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9850
	          2theta: -15.1058
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.033845
_diffrn_orient_matrix_UB_12      -0.035873
_diffrn_orient_matrix_UB_13      0.035362
_diffrn_orient_matrix_UB_21      -0.064793
_diffrn_orient_matrix_UB_22      -0.039141
_diffrn_orient_matrix_UB_23      0.022309
_diffrn_orient_matrix_UB_31      0.010968
_diffrn_orient_matrix_UB_32      -0.039426
_diffrn_orient_matrix_UB_33      -0.037319
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7118
_reflns_number_total             7514
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.7754
_refine_diff_density_min         -1.0448
_refine_diff_density_rms         0.1805
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.7270
_refine_ls_goodness_of_fit_ref   0.9983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0689
_refine_ls_restrained_S_all      0.9983
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)²+64.1247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1340
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O12(H12a,H12b)
2.b Ternary CH refined with riding coordinates:
 C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b)
2.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C16(H16), C6(H6), C24(H24), C5(H5), C4(H4), C8(H8),
 C15(H15), C29(H29)
2.e Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
Tb1 Tb 0.73131(2) 0.49686(3) 0.86582(2) 0.03641(12) Uani 1.000000 .
Ni1 Ni 0.88810(5) 0.49196(8) 0.77367(5) 0.0332(2) Uani 1.000000 .
O4 O 0.7783(3) 0.4839(4) 0.7424(3) 0.0297(11) Uani 1.000000 .
O5 O 0.6379(3) 0.5055(5) 0.7330(3) 0.0418(13) Uani 1.000000 .
N1 N 0.9965(4) 0.4993(6) 0.8211(4) 0.0414(15) Uani 1.000000 .
C13 C 0.7782(4) 0.5017(7) 0.5983(5) 0.0401(18) Uani 1.000000 .
C18 C 0.7430(4) 0.4998(6) 0.6687(4) 0.0360(16) Uani 1.000000 .
C17 C 0.6658(4) 0.5131(6) 0.6612(5) 0.0390(18) Uani 1.000000 .
O2 O 0.8569(3) 0.5289(4) 0.8828(3) 0.0320(11) Uani 1.000000 .
C19 C 0.5587(4) 0.4912(8) 0.7283(6) 0.051(2) Uani 1.000000 .
H19a H 0.5471(5) 0.466(5) 0.7794(14) 0.077(3) Uiso 1.000000 GR
H19b H 0.5343(5) 0.5574(13) 0.716(4) 0.077(3) Uiso 1.000000 GR
H19c H 0.5422(7) 0.441(4) 0.687(3) 0.077(3) Uiso 1.000000 GR
O12 O 0.8786(3) 0.6584(4) 0.7448(3) 0.0396(13) Uani 1.000000 .
H12a H 0.843(3) 0.6845(13) 0.767(4) 0.0594(19) Uiso 1.000000 GR
H12b H 0.870(4) 0.6669(5) 0.6938(3) 0.0594(19) Uiso 1.000000 GR
O1 O 0.7835(3) 0.6344(4) 0.9777(3) 0.0393(13) Uani 1.000000 .
C14 C 0.7350(5) 0.5206(7) 0.5231(5) 0.046(2) Uani 1.000000 .
H14 H 0.7575(5) 0.5220(7) 0.4764(5) 0.055(2) Uiso 1.000000 R
N2 N 0.9062(4) 0.4694(5) 0.6578(4) 0.0411(16) Uani 1.000000 .
O10 O 0.7307(3) 0.6775(4) 0.8115(3) 0.0377(12) Uani 1.000000 .
F51 F 0.5512(3) 0.1434(5) 0.9271(4) 0.0658(17) Uani 1.000000 .
O8 O 0.6409(3) 0.3642(5) 0.8656(3) 0.0436(14) Uani 1.000000 .
O9 O 0.7398(3) 0.4278(4) 0.9990(3) 0.0391(13) Uani 1.000000 .
F30 F 0.7713(3) 0.8579(5) 0.7546(4) 0.0698(17) Uani 1.000000 .
F43 F 0.7143(4) 0.2546(5) 1.1547(3) 0.0661(16) Uani 1.000000 .
O7 O 0.7875(3) 0.3278(5) 0.8644(4) 0.0458(14) Uani 1.000000 .
O11 O 0.6265(3) 0.5826(5) 0.9018(4) 0.0473(14) Uani 1.000000 .
O6 O 0.8878(3) 0.3314(4) 0.7987(3) 0.0381(12) Uani 1.000000 .
F50 F 0.5140(3) 0.2542(5) 0.8365(4) 0.0696(17) Uani 1.000000 .
C12 C 0.8557(5) 0.4817(6) 0.5976(5) 0.0422(19) Uani 1.000000 .
H12 H 0.8708(5) 0.4771(6) 0.5467(5) 0.051(2) Uiso 1.000000 R
O3 O 1.0031(5) 0.2894(7) 0.7140(5) 0.079(2) Uani 1.000000 .
H3 H 0.967(5) 0.2943(11) 0.738(8) 0.118(3) Uiso 1.000000 GR
F49 F 0.6024(4) 0.1520(6) 0.8201(5) 0.090(2) Uani 1.000000 .
F55 F 0.8184(4) 0.2914(6) 1.1188(4) 0.087(2) Uani 1.000000 .
C16 C 0.6248(5) 0.5323(7) 0.5863(5) 0.045(2) Uani 1.000000 .
H16 H 0.5740(5) 0.5421(7) 0.5820(5) 0.054(2) Uiso 1.000000 R
C6 C 1.0101(5) 0.6823(7) 0.9916(5) 0.048(2) Uani 1.000000 .
H6 H 1.0609(5) 0.6913(7) 0.9948(5) 0.057(3) Uiso 1.000000 R
C20 C 0.8387(5) 0.2887(7) 0.8351(5) 0.042(2) Uani 1.000000 .
C2 C 0.8965(4) 0.5970(6) 0.9319(4) 0.0331(16) Uani 1.000000 .
C23 C 0.6303(4) 0.2907(6) 0.9120(5) 0.0369(17) Uani 1.000000 .
F54 F 0.7541(5) 0.4139(5) 1.1596(3) 0.094(3) Uani 1.000000 .
C25 C 0.7149(4) 0.3467(6) 1.0290(5) 0.0350(17) Uani 1.000000 .
C3 C 0.8583(5) 0.6559(6) 0.9852(5) 0.0375(17) Uani 1.000000 .
F37 F 0.6818(5) 0.9368(5) 0.7997(5) 0.099(3) Uani 1.000000 .
F38 F 0.6649(4) 0.8509(7) 0.6906(4) 0.095(2) Uani 1.000000 .
C7 C 0.9733(4) 0.6095(6) 0.9354(5) 0.0361(17) Uani 1.000000 .
F36 F 0.5305(4) 0.6629(7) 0.9996(4) 0.099(3) Uani 1.000000 .
C21 C 0.8452(6) 0.1745(8) 0.8450(6) 0.059(3) Uani 1.000000 .
C24 C 0.6636(4) 0.2760(6) 0.9923(5) 0.0342(16) Uani 1.000000 .
H24 H 0.6508(4) 0.2177(6) 1.0212(5) 0.041(2) Uiso 1.000000 R
C26 C 0.7499(6) 0.3270(8) 1.1170(5) 0.055(2) Uani 1.000000 .
C9 C 1.0544(5) 0.4463(9) 0.7840(6) 0.059(3) Uani 1.000000 .
H9a H 1.0919(5) 0.4982(9) 0.7768(6) 0.071(3) Uiso 1.000000 R
H9b H 1.0772(5) 0.3942(9) 0.8221(6) 0.071(3) Uiso 1.000000 R
C5 C 0.9713(6) 0.7393(7) 1.0410(6) 0.055(2) Uani 1.000000 .
H5 H 0.9963(6) 0.7871(7) 1.0771(6) 0.065(3) Uiso 1.000000 R
C4 C 0.8954(5) 0.7280(7) 1.0389(5) 0.046(2) Uani 1.000000 .
H4 H 0.8699(5) 0.7679(7) 1.0728(5) 0.055(2) Uiso 1.000000 R
F42 F 0.4900(4) 0.7737(7) 0.9083(5) 0.110(3) Uani 1.000000 .
C8 C 1.0190(5) 0.5530(7) 0.8850(5) 0.0406(19) Uani 1.000000 .
H8 H 1.0698(5) 0.5560(7) 0.9007(5) 0.049(2) Uiso 1.000000 R
C28 C 0.6837(5) 0.7503(7) 0.8104(5) 0.0409(19) Uani 1.000000 .
F41 F 0.4732(4) 0.6089(9) 0.8894(6) 0.122(3) Uani 1.000000 .
C15 C 0.6602(6) 0.5369(7) 0.5174(5) 0.053(2) Uani 1.000000 .
H15 H 0.6329(6) 0.5512(7) 0.4672(5) 0.064(3) Uiso 1.000000 R
C10 C 1.0318(5) 0.3914(8) 0.7028(6) 0.055(2) Uani 1.000000 .
H10 H 1.0777(5) 0.3802(8) 0.6798(6) 0.066(3) Uiso 1.000000 R
C27 C 0.7012(6) 0.8517(8) 0.7655(6) 0.055(2) Uani 1.000000 .
C22 C 0.5746(5) 0.2081(7) 0.8732(5) 0.046(2) Uani 1.000000 .
C30 C 0.5951(5) 0.6687(8) 0.8856(5) 0.049(2) Uani 1.000000 .
C29 C 0.6179(5) 0.7507(8) 0.8429(5) 0.049(2) Uani 1.000000 .
H29 H 0.5879(5) 0.8101(8) 0.8351(5) 0.059(3) Uiso 1.000000 R
C1 C 0.7468(5) 0.6649(8) 1.0452(5) 0.051(2) Uani 1.000000 .
H1a H 0.6988(15) 0.633(4) 1.040(2) 0.076(3) Uiso 1.000000 GR
H1b H 0.7754(19) 0.642(5) 1.0948(6) 0.076(3) Uiso 1.000000 GR
H1c H 0.742(3) 0.7402(9) 1.046(2) 0.076(3) Uiso 1.000000 GR
C11 C 0.9820(5) 0.4554(8) 0.6401(5) 0.048(2) Uani 1.000000 .
H11a H 0.9802(5) 0.4210(8) 0.5879(5) 0.057(3) Uiso 1.000000 R
H11b H 1.0040(5) 0.5245(8) 0.6357(5) 0.057(3) Uiso 1.000000 R
C31 C 0.5207(6) 0.6786(11) 0.9212(7) 0.071(3) Uani 1.000000 .
F1 F 0.7773(4) 0.1224(6) 0.8348(5) 0.096(2) Uani 1.000000 .
F2 F 0.8655(5) 0.1467(7) 0.9251(5) 0.111(3) Uani 1.000000 .
F3 F 0.8857(5) 0.1297(7) 0.8046(6) 0.117(3) Uani 1.000000 .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Ni1 3.4350(10) . ?
Tb1 O4 2.342(5) . ?
Tb1 O5 2.604(5) . ?
Tb1 O2 2.310(5) . ?
Tb1 O1 2.635(5) . ?
Tb1 O10 2.463(5) . ?
Tb1 O8 2.359(5) . ?
Tb1 O9 2.371(5) . ?
Tb1 O7 2.379(6) . ?
Tb1 O11 2.352(6) . ?
Ni1 O4 2.005(5) . ?
Ni1 N1 2.032(6) . ?
Ni1 O2 2.036(5) . ?
Ni1 O12 2.167(5) . ?
Ni1 N2 2.024(7) . ?
Ni1 O6 2.079(6) . ?
O4 C18 1.322(8) . ?
O5 C17 1.368(10) . ?
O5 C19 1.451(9) . ?
N1 C9 1.462(11) . ?
N1 C8 1.283(10) . ?
C13 C18 1.414(11) . ?
C13 C14 1.407(11) . ?
C13 C12 1.441(12) . ?
C18 C17 1.409(11) . ?
C17 C16 1.386(10) . ?
O2 C2 1.333(8) . ?
O1 C3 1.384(10) . ?
O1 C1 1.440(9) . ?
C14 C15 1.374(13) . ?
N2 C12 1.275(10) . ?
N2 C11 1.468(11) . ?
O10 C28 1.259(10) . ?
F51 C22 1.331(10) . ?
O8 C23 1.243(9) . ?
O9 C25 1.257(9) . ?
F30 C27 1.320(11) . ?
F43 C26 1.332(11) . ?
O7 C20 1.220(11) . ?
O11 C30 1.246(11) . ?
O6 C20 1.271(10) . ?
F50 C22 1.324(10) . ?
O3 C10 1.418(13) . ?
F49 C22 1.294(11) . ?
F55 C26 1.327(12) . ?
C16 C15 1.395(13) . ?
C6 C7 1.417(11) . ?
C6 C5 1.367(13) . ?
C20 C21 1.460(12) . ?
C2 C3 1.416(11) . ?
C2 C7 1.407(11) . ?
C23 C24 1.404(11) . ?
C23 C22 1.541(11) . ?
F54 C26 1.307(11) . ?
C25 C24 1.377(10) . ?
C25 C26 1.539(11) . ?
C3 C4 1.388(11) . ?
F37 C27 1.293(11) . ?
F38 C27 1.330(11) . ?
C7 C8 1.452(12) . ?
F36 C31 1.309(13) . ?
C21 F1 1.395(13) . ?
C21 F2 1.381(12) . ?
C21 F3 1.210(12) . ?
C9 C10 1.528(13) . ?
C5 C4 1.391(13) . ?
F42 C31 1.336(14) . ?
C28 C27 1.545(12) . ?
C28 C29 1.386(12) . ?
F41 C31 1.300(15) . ?
C10 C11 1.522(12) . ?
C30 C29 1.357(13) . ?
C30 C31 1.563(13) . ?

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
O4 Tb1 Ni1 34.48(11) . . ?
O5 Tb1 Ni1 96.35(12) . . ?
O5 Tb1 O4 62.21(16) . . ?
O2 Tb1 Ni1 35.05(12) . . ?
O2 Tb1 O4 68.96(16) . . ?
O2 Tb1 O5 128.38(17) . . ?
O1 Tb1 Ni1 94.92(12) . . ?
O1 Tb1 O4 121.83(16) . . ?
O1 Tb1 O5 134.80(19) . . ?
O1 Tb1 O2 62.62(17) . . ?
O10 Tb1 Ni1 79.28(13) . . ?
O10 Tb1 O4 74.12(17) . . ?
O10 Tb1 O5 71.33(18) . . ?
O10 Tb1 O2 80.50(17) . . ?
O10 Tb1 O1 68.08(17) . . ?
O8 Tb1 Ni1 127.94(15) . . ?
O8 Tb1 O4 106.91(18) . . ?
O8 Tb1 O5 69.59(18) . . ?
O8 Tb1 O2 144.14(19) . . ?
O8 Tb1 O1 131.19(18) . . ?
O8 Tb1 O10 134.07(19) . . ?
O9 Tb1 Ni1 117.46(14) . . ?
O9 Tb1 O4 144.25(18) . . ?
O9 Tb1 O5 139.59(17) . . ?
O9 Tb1 O2 90.84(18) . . ?
O9 Tb1 O1 67.12(17) . . ?
O9 Tb1 O10 133.13(18) . . ?
O9 Tb1 O8 72.15(18) . . ?
O7 Tb1 Ni1 65.86(14) . . ?
O7 Tb1 O4 73.53(18) . . ?
O7 Tb1 O5 105.2(2) . . ?
O7 Tb1 O2 74.72(18) . . ?
O7 Tb1 O1 119.28(19) . . ?
O7 Tb1 O10 144.56(19) . . ?
O7 Tb1 O8 70.2(2) . . ?
O7 Tb1 O9 72.8(2) . . ?
O11 Tb1 Ni1 151.90(15) . . ?
O11 Tb1 O4 131.87(18) . . ?
O11 Tb1 O5 74.68(19) . . ?
O11 Tb1 O2 135.90(19) . . ?
O11 Tb1 O1 75.00(19) . . ?
O11 Tb1 O10 72.63(19) . . ?
O11 Tb1 O8 74.6(2) . . ?
O11 Tb1 O9 83.2(2) . . ?
O11 Tb1 O7 141.9(2) . . ?
O4 Ni1 Tb1 41.38(14) . . ?
N1 Ni1 Tb1 130.88(19) . . ?
N1 Ni1 O4 172.2(2) . . ?
O2 Ni1 Tb1 40.67(14) . . ?
O2 Ni1 O4 81.3(2) . . ?
O2 Ni1 N1 91.2(2) . . ?
O12 Ni1 Tb1 92.00(16) . . ?
O12 Ni1 O4 86.9(2) . . ?
O12 Ni1 N1 94.9(3) . . ?
O12 Ni1 O2 87.1(2) . . ?
N2 Ni1 Tb1 133.28(19) . . ?
N2 Ni1 O4 92.0(2) . . ?
N2 Ni1 N1 95.7(3) . . ?
N2 Ni1 O2 171.2(2) . . ?
N2 Ni1 O12 86.9(2) . . ?
O6 Ni1 Tb1 84.39(16) . . ?
O6 Ni1 O4 88.4(2) . . ?
O6 Ni1 N1 89.8(3) . . ?
O6 Ni1 O2 92.1(2) . . ?
O6 Ni1 O12 175.2(2) . . ?
O6 Ni1 N2 93.3(3) . . ?
Ni1 O4 Tb1 104.13(19) . . ?
C18 O4 Tb1 127.9(5) . . ?
C18 O4 Ni1 125.2(5) . . ?
C17 O5 Tb1 117.8(4) . . ?
C19 O5 Tb1 125.0(5) . . ?
C19 O5 C17 116.9(6) . . ?
C9 N1 Ni1 122.6(6) . . ?
C8 N1 Ni1 122.1(6) . . ?
C8 N1 C9 115.3(7) . . ?
C14 C13 C18 118.6(8) . . ?
C12 C13 C18 124.4(7) . . ?
C12 C13 C14 117.0(7) . . ?
C13 C18 O4 123.6(7) . . ?
C17 C18 O4 117.1(7) . . ?
C17 C18 C13 119.3(7) . . ?
C18 C17 O5 113.8(6) . . ?
C16 C17 O5 125.4(8) . . ?
C16 C17 C18 120.8(8) . . ?
Ni1 O2 Tb1 104.27(19) . . ?
C2 O2 Tb1 129.5(5) . . ?
C2 O2 Ni1 120.1(5) . . ?
C3 O1 Tb1 116.8(4) . . ?
C1 O1 Tb1 124.7(5) . . ?
C1 O1 C3 116.0(6) . . ?
C15 C14 C13 121.2(8) . . ?
C12 N2 Ni1 122.5(6) . . ?
C11 N2 Ni1 119.5(5) . . ?
C11 N2 C12 117.3(7) . . ?
C28 O10 Tb1 130.9(5) . . ?
C23 O8 Tb1 134.7(5) . . ?
C25 O9 Tb1 133.9(5) . . ?
C20 O7 Tb1 136.6(5) . . ?
C30 O11 Tb1 135.8(6) . . ?
C20 O6 Ni1 122.3(5) . . ?
N2 C12 C13 128.4(7) . . ?
C15 C16 C17 119.6(8) . . ?
C5 C6 C7 120.2(8) . . ?
O6 C20 O7 130.5(8) . . ?
C21 C20 O7 114.3(9) . . ?
C21 C20 O6 115.1(9) . . ?
C3 C2 O2 117.0(7) . . ?
C7 C2 O2 123.5(7) . . ?
C7 C2 C3 119.4(7) . . ?
C24 C23 O8 127.5(7) . . ?
C22 C23 O8 113.5(7) . . ?
C22 C23 C24 119.0(7) . . ?
C24 C25 O9 128.2(7) . . ?
C26 C25 O9 112.7(7) . . ?
C26 C25 C24 119.1(7) . . ?
C2 C3 O1 114.0(6) . . ?
C4 C3 O1 125.2(8) . . ?
C4 C3 C2 120.8(8) . . ?
C2 C7 C6 118.7(8) . . ?
C8 C7 C6 116.4(7) . . ?
C8 C7 C2 124.9(7) . . ?
F1 C21 C20 113.5(8) . . ?
F2 C21 C20 111.7(7) . . ?
F2 C21 F1 96.5(10) . . ?
F3 C21 C20 116.7(12) . . ?
F3 C21 F1 108.1(8) . . ?
F3 C21 F2 108.3(9) . . ?
C25 C24 C23 121.0(7) . . ?
F55 C26 F43 106.1(8) . . ?
F54 C26 F43 108.7(8) . . ?
F54 C26 F55 106.9(9) . . ?
C25 C26 F43 113.2(8) . . ?
C25 C26 F55 110.1(8) . . ?
C25 C26 F54 111.5(8) . . ?
C10 C9 N1 117.5(7) . . ?
C4 C5 C6 122.1(8) . . ?
C5 C4 C3 118.7(8) . . ?
C7 C8 N1 126.7(7) . . ?
C27 C28 O10 115.5(7) . . ?
C29 C28 O10 128.7(8) . . ?
C29 C28 C27 115.8(8) . . ?
C16 C15 C14 120.5(7) . . ?
C9 C10 O3 111.0(9) . . ?
C11 C10 O3 112.3(8) . . ?
C11 C10 C9 115.3(8) . . ?
F37 C27 F30 110.0(9) . . ?
F38 C27 F30 103.9(8) . . ?
F38 C27 F37 106.8(9) . . ?
C28 C27 F30 112.7(8) . . ?
C28 C27 F37 113.2(8) . . ?
C28 C27 F38 109.7(8) . . ?
F50 C22 F51 104.9(7) . . ?
F49 C22 F51 108.5(8) . . ?
F49 C22 F50 108.1(8) . . ?
C23 C22 F51 113.0(7) . . ?
C23 C22 F50 110.9(7) . . ?
C23 C22 F49 111.2(7) . . ?
C29 C30 O11 128.3(8) . . ?
C31 C30 O11 112.8(9) . . ?
C31 C30 C29 119.0(9) . . ?
C30 C29 C28 123.2(9) . . ?
C10 C11 N2 114.7(7) . . ?
F42 C31 F36 107.1(10) . . ?
F41 C31 F36 107.2(11) . . ?
F41 C31 F42 107.8(10) . . ?
C30 C31 F36 111.2(9) . . ?
C30 C31 F42 112.3(9) . . ?
C30 C31 F41 111.0(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
