# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_Cmpd_2
_database_code_depnum_ccdc_archive 'CCDC 1046875'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_date             2015-02-23T13:46:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C96 H96 Co2 N18 Ni4 O20 Tb2, 2(C3 H6 O), 2(O)'
_chemical_formula_sum            'C102 H108 Co2 N18 Ni4 O24 Tb2'
_chemical_formula_weight         2640.54
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.8968(7)
_cell_length_b                   22.2820(7)
_cell_length_c                   19.3332(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.728(4)
_cell_angle_gamma                90
_cell_volume                     6970.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    15275
_cell_measurement_theta_min      3.3602
_cell_measurement_theta_max      28.9745
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       platelet
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.978

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.1978
_diffrn_orient_matrix_ub_11      -0.0424574
_diffrn_orient_matrix_ub_12      -0.0080366
_diffrn_orient_matrix_ub_13      -0.0103316
_diffrn_orient_matrix_ub_21      0.0109359
_diffrn_orient_matrix_ub_22      -0.0301074
_diffrn_orient_matrix_ub_23      0.0103405
_diffrn_orient_matrix_ub_31      -0.0018644
_diffrn_orient_matrix_ub_32      0.0064654
_diffrn_orient_matrix_ub_33      0.0354028
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_number            54665
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             13197
_reflns_number_gt                7230
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.032 0.001 -0.016 1985 473 ' '
_platon_squeeze_details          
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1042P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         13197
_refine_ls_number_parameters     695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0673
_refine_ls_wR_factor_ref         0.1687
_refine_ls_wR_factor_gt          0.1599
_refine_ls_goodness_of_fit_ref   0.89
_refine_ls_restrained_S_all      0.89
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         11.322
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.186

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6351(5) -0.1056(5) 0.1704(5) 0.053(3) Uani 1 1 d . . .
H1A H 0.6311 -0.119 0.2182 0.064 Uiso 1 1 calc R . .
H1B H 0.6116 -0.1377 0.1351 0.064 Uiso 1 1 calc R . .
C2 C 0.5827(6) -0.0482(5) 0.1482(6) 0.060(3) Uani 1 1 d . . .
C3 C 0.6022(6) -0.0023(5) 0.2070(6) 0.054(3) Uani 1 1 d . . .
H3A H 0.5605 0.0301 0.1939 0.065 Uiso 1 1 calc R . .
H3B H 0.5972 -0.0213 0.2519 0.065 Uiso 1 1 calc R . .
C4 C 0.4901(6) -0.0666(7) 0.1356(7) 0.094(5) Uani 1 1 d . . .
H4A H 0.4542 -0.0325 0.1157 0.141 Uiso 1 1 calc R . .
H4B H 0.4815 -0.0787 0.1817 0.141 Uiso 1 1 calc R . .
H4C H 0.4766 -0.1003 0.1016 0.141 Uiso 1 1 calc R . .
C5 C 0.5946(8) -0.0217(6) 0.0789(6) 0.082(4) Uani 1 1 d . . .
H5A H 0.5577 0.0128 0.0636 0.123 Uiso 1 1 calc R . .
H5B H 0.5815 -0.0523 0.0408 0.123 Uiso 1 1 calc R . .
H5C H 0.652 -0.0088 0.0877 0.123 Uiso 1 1 calc R . .
C6 C 0.7529(6) -0.1368(4) 0.1411(4) 0.044(2) Uani 1 1 d . . .
H6 H 0.716 -0.1676 0.1177 0.052 Uiso 1 1 calc R . .
C7 C 0.8373(5) -0.1402(3) 0.1342(4) 0.0309(18) Uani 1 1 d . . .
C8 C 0.8559(6) -0.1865(3) 0.0917(4) 0.034(2) Uani 1 1 d . . .
H8 H 0.8146 -0.2151 0.0697 0.041 Uiso 1 1 calc R . .
C9 C 0.9326(6) -0.1908(4) 0.0819(4) 0.037(2) Uani 1 1 d . . .
H9 H 0.9439 -0.2222 0.0529 0.045 Uiso 1 1 calc R . .
C10 C 0.9920(5) -0.1514(3) 0.1126(4) 0.0317(19) Uani 1 1 d . . .
H10 H 1.0449 -0.1551 0.1051 0.038 Uiso 1 1 calc R . .
C11 C 0.9772(5) -0.1055(3) 0.1551(4) 0.0256(18) Uani 1 1 d . . .
C12 C 1.1145(5) -0.0643(4) 0.1743(4) 0.038(2) Uani 1 1 d . . .
H12A H 1.1454 -0.0996 0.1978 0.058 Uiso 1 1 calc R . .
H12B H 1.1457 -0.0279 0.1932 0.058 Uiso 1 1 calc R . .
H12C H 1.106 -0.0668 0.1221 0.058 Uiso 1 1 calc R . .
C13 C 0.8998(5) -0.0996(3) 0.1670(4) 0.0263(17) Uani 1 1 d . . .
C14 C 0.6898(6) 0.0818(4) 0.2319(5) 0.043(2) Uani 1 1 d . . .
H14 H 0.6386 0.1022 0.2238 0.051 Uiso 1 1 calc R . .
C15 C 0.7633(5) 0.1189(4) 0.2541(4) 0.0331(19) Uani 1 1 d . . .
C16 C 0.7511(6) 0.1811(4) 0.2588(5) 0.049(2) Uani 1 1 d . . .
H16 H 0.6963 0.1963 0.2452 0.059 Uiso 1 1 calc R . .
C18 C 0.8150(6) 0.2201(4) 0.2819(5) 0.051(3) Uani 1 1 d . . .
H18 H 0.8046 0.2619 0.2834 0.061 Uiso 1 1 calc R . .
C19 C 0.8963(6) 0.1986(3) 0.3036(4) 0.036(2) Uani 1 1 d . . .
H19 H 0.9415 0.2255 0.3199 0.043 Uiso 1 1 calc R . .
C20 C 0.9099(5) 0.1373(3) 0.3010(4) 0.0265(18) Uani 1 1 d . . .
C21 C 0.8446(5) 0.0969(3) 0.2750(4) 0.0269(18) Uani 1 1 d . . .
C22 C 1.0563(5) 0.1516(4) 0.3525(4) 0.039(2) Uani 1 1 d . . .
H22A H 1.0596 0.1825 0.3173 0.058 Uiso 1 1 calc R . .
H22B H 1.1081 0.1288 0.3666 0.058 Uiso 1 1 calc R . .
H22C H 1.0473 0.1707 0.3952 0.058 Uiso 1 1 calc R . .
C23 C 1.3952(5) 0.0031(4) 0.4056(4) 0.0372(19) Uani 1 1 d . . .
H23A H 1.4371 -0.0293 0.4142 0.045 Uiso 1 1 calc R . .
H23B H 1.3998 0.0227 0.4526 0.045 Uiso 1 1 calc R . .
C24 C 1.4147(5) 0.0489(4) 0.3550(5) 0.037(2) Uani 1 1 d . . .
C25 C 1.3610(5) 0.1056(4) 0.3490(5) 0.038(2) Uani 1 1 d . . .
H25A H 1.3658 0.1203 0.3984 0.046 Uiso 1 1 calc R . .
H25B H 1.3839 0.1371 0.3241 0.046 Uiso 1 1 calc R . .
C26 C 1.5061(6) 0.0678(5) 0.3866(6) 0.061(3) Uani 1 1 d . . .
H26A H 1.5144 0.085 0.4348 0.092 Uiso 1 1 calc R . .
H26B H 1.5201 0.0978 0.355 0.092 Uiso 1 1 calc R . .
H26C H 1.5418 0.0326 0.3899 0.092 Uiso 1 1 calc R . .
C27 C 1.4020(6) 0.0219(5) 0.2781(5) 0.057(3) Uani 1 1 d . . .
H27A H 1.4252 0.0493 0.2494 0.085 Uiso 1 1 calc R . .
H27B H 1.3428 0.0166 0.2545 0.085 Uiso 1 1 calc R . .
H27C H 1.43 -0.017 0.2822 0.085 Uiso 1 1 calc R . .
C28 C 1.2438(5) 0.1377(4) 0.2624(5) 0.038(2) Uani 1 1 d . . .
H28 H 1.2802 0.1687 0.2572 0.046 Uiso 1 1 calc R . .
C29 C 1.1602(5) 0.1409(3) 0.2141(4) 0.0270(17) Uani 1 1 d . . .
C30 C 1.0966(5) 0.1002(3) 0.2157(4) 0.0231(17) Uani 1 1 d . . .
C31 C 1.0181(5) 0.1073(3) 0.1650(4) 0.0258(17) Uani 1 1 d . . .
C32 C 1.0024(5) 0.1517(3) 0.1139(4) 0.0290(18) Uani 1 1 d . . .
H32 H 0.9498 0.1546 0.0791 0.035 Uiso 1 1 calc R . .
C33 C 1.0644(6) 0.1921(3) 0.1136(4) 0.034(2) Uani 1 1 d . . .
H33 H 1.0535 0.224 0.0796 0.041 Uiso 1 1 calc R . .
C34 C 1.1410(5) 0.1866(3) 0.1616(4) 0.0306(19) Uani 1 1 d . . .
H34 H 1.1827 0.2146 0.1597 0.037 Uiso 1 1 calc R . .
C35 C 0.8819(5) 0.0648(4) 0.1155(4) 0.038(2) Uani 1 1 d . . .
H35A H 0.8521 0.1013 0.1217 0.057 Uiso 1 1 calc R . .
H35B H 0.8495 0.0295 0.1204 0.057 Uiso 1 1 calc R . .
H35C H 0.8904 0.065 0.0675 0.057 Uiso 1 1 calc R . .
C36 C 1.3078(6) -0.0814(4) 0.3864(4) 0.042(2) Uani 1 1 d . . .
H36 H 1.3591 -0.1018 0.4037 0.05 Uiso 1 1 calc R . .
C37 C 1.2339(5) -0.1181(3) 0.3723(4) 0.0301(19) Uani 1 1 d . . .
C38 C 1.2473(6) -0.1803(4) 0.3840(5) 0.045(2) Uani 1 1 d . . .
H38 H 1.3021 -0.1955 0.3973 0.054 Uiso 1 1 calc R . .
C39 C 1.1815(6) -0.2193(4) 0.3762(5) 0.045(2) Uani 1 1 d . . .
H39 H 1.1914 -0.261 0.385 0.055 Uiso 1 1 calc R . .
C40 C 1.1016(6) -0.1976(3) 0.3557(4) 0.033(2) Uani 1 1 d . . .
H40 H 1.0565 -0.2245 0.3489 0.04 Uiso 1 1 calc R . .
C41 C 1.0870(5) -0.1372(3) 0.3449(4) 0.0258(17) Uani 1 1 d . . .
C42 C 1.1527(5) -0.0960(3) 0.3518(4) 0.0238(17) Uani 1 1 d . . .
C43 C 0.9420(6) -0.1514(4) 0.3249(5) 0.042(2) Uani 1 1 d . . .
H43A H 0.941 -0.1839 0.2904 0.063 Uiso 1 1 calc R . .
H43B H 0.8895 -0.1295 0.3103 0.063 Uiso 1 1 calc R . .
H43C H 0.9502 -0.1684 0.3732 0.063 Uiso 1 1 calc R . .
C50 C 0.7512(5) -0.0918(3) 0.5102(4) 0.0254(17) Uani 1 1 d . . .
C51 C 0.7521(5) -0.0919(3) 0.3656(4) 0.0302(19) Uani 1 1 d . . .
C52 C 0.6097(6) -0.1131(4) 0.4008(5) 0.043(2) Uani 1 1 d . . .
C53 C 0.6876(5) -0.2003(4) 0.3519(5) 0.036(2) Uani 1 1 d . . .
C54 C 0.6861(5) -0.1994(4) 0.4915(5) 0.035(2) Uani 1 1 d . . .
C55 C 0.8291(5) -0.1737(3) 0.4577(4) 0.0252(17) Uani 1 1 d . . .
C60 C 0.7584(7) 0.0674(4) 0.4399(5) 0.060(3) Uani 1 1 d . . .
H60A H 0.7103 0.0562 0.3998 0.09 Uiso 1 1 calc R . .
H60B H 0.7503 0.0536 0.4855 0.09 Uiso 1 1 calc R . .
H60C H 0.8081 0.0487 0.4331 0.09 Uiso 1 1 calc R . .
C61 C 0.7678(6) 0.1325(4) 0.4417(5) 0.045(2) Uani 1 1 d . . .
C62 C 0.6892(6) 0.1696(5) 0.4223(6) 0.065(3) Uani 1 1 d . . .
H62A H 0.6585 0.1619 0.4573 0.098 Uiso 1 1 calc R . .
H62B H 0.655 0.1585 0.3738 0.098 Uiso 1 1 calc R . .
H62C H 0.7033 0.2123 0.4231 0.098 Uiso 1 1 calc R . .
N1 N 0.7232(4) -0.0976(3) 0.1746(3) 0.0318(16) Uani 1 1 d . . .
N2 N 0.6851(4) 0.0246(4) 0.2218(4) 0.0374(17) Uani 1 1 d . . .
N3 N 1.3114(4) -0.0241(3) 0.3781(4) 0.0331(16) Uani 1 1 d . . .
N4 N 1.2748(4) 0.0982(3) 0.3113(3) 0.0275(15) Uani 1 1 d . . .
N5 N 0.7737(4) -0.0643(3) 0.3251(3) 0.0313(16) Uani 1 1 d . . .
N6 N 0.6647(5) -0.2324(4) 0.5281(5) 0.055(2) Uani 1 1 d . . .
N7 N 0.6659(5) -0.2340(4) 0.3057(5) 0.059(2) Uani 1 1 d . . .
N8 N 0.5428(6) -0.0972(4) 0.3809(7) 0.088(3) Uani 1 1 d . . .
N9 N 0.8989(4) -0.1862(3) 0.4752(3) 0.0293(15) Uani 1 1 d . . .
O1 O 0.8900(3) -0.0536(2) 0.2111(3) 0.0233(11) Uani 1 1 d . . .
O2 O 0.8636(3) 0.0392(2) 0.2720(3) 0.0273(12) Uani 1 1 d . . .
O3 O 1.0350(3) -0.0624(2) 0.1888(2) 0.0234(11) Uani 1 1 d . . .
O4 O 1.1083(3) 0.0550(2) 0.2654(3) 0.0227(11) Uani 1 1 d . . .
O5 O 0.9616(3) 0.0631(2) 0.1703(2) 0.0270(12) Uani 1 1 d . . .
O6 O 1.1340(3) -0.0382(2) 0.3394(3) 0.0265(12) Uani 1 1 d . . .
O7 O 1.0099(3) -0.1103(2) 0.3260(3) 0.0286(12) Uani 1 1 d . . .
O8 O 0.9883(3) 0.1114(2) 0.3204(3) 0.0274(12) Uani 1 1 d . . .
O9 O 0.9993(3) 0.0006(2) 0.4056(2) 0.0291(12) Uani 1 1 d . . .
N10 N 1.2259(4) 0.0647(3) 0.4379(3) 0.0293(15) Uani 1 1 d . . .
O20 O 0.9796(3) 0.0918(2) 0.4951(3) 0.0328(13) Uani 1 1 d . . .
O21 O 0.8342(4) 0.1593(3) 0.4571(3) 0.0464(15) Uani 1 1 d . . .
Co1 Co 0.71887(7) -0.14459(4) 0.42976(6) 0.0274(3) Uani 1 1 d . . .
Ni1 Ni 0.78489(6) -0.02890(5) 0.23420(5) 0.0278(2) Uani 1 1 d . . .
Ni2 Ni 1.21294(6) 0.02957(4) 0.34054(5) 0.0233(2) Uani 1 1 d . . .
Tb1 Tb 0.99898(2) 0.000386(16) 0.283611(17) 0.02030(11) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.479(10) . ?
C1 C2 1.545(15) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.494(13) . ?
C2 C5 1.528(15) . ?
C2 C4 1.568(13) . ?
C3 N2 1.476(11) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 N1 1.274(10) . ?
C6 C7 1.472(12) . ?
C6 H6 0.95 . ?
C7 C13 1.397(11) . ?
C7 C8 1.409(10) . ?
C8 C9 1.366(12) . ?
C8 H8 0.95 . ?
C9 C10 1.337(11) . ?
C9 H9 0.95 . ?
C10 C11 1.378(10) . ?
C10 H10 0.95 . ?
C11 O3 1.391(9) . ?
C11 C13 1.398(11) . ?
C12 O3 1.449(9) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 O1 1.372(8) . ?
C14 N2 1.287(11) . ?
C14 C15 1.450(12) . ?
C14 H14 0.95 . ?
C15 C21 1.404(11) . ?
C15 C16 1.409(12) . ?
C16 C18 1.357(13) . ?
C16 H16 0.95 . ?
C18 C19 1.401(12) . ?
C18 H18 0.95 . ?
C19 C20 1.389(10) . ?
C19 H19 0.95 . ?
C20 O8 1.394(9) . ?
C20 C21 1.400(11) . ?
C21 O2 1.330(8) . ?
C22 O8 1.449(9) . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 N3 1.491(10) . ?
C23 C24 1.514(11) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 C25 1.541(11) . ?
C24 C26 1.547(12) . ?
C24 C27 1.560(12) . ?
C25 N4 1.438(10) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 N4 1.288(10) . ?
C28 C29 1.454(12) . ?
C28 H28 0.95 . ?
C29 C34 1.408(10) . ?
C29 C30 1.412(10) . ?
C30 O4 1.368(8) . ?
C30 C31 1.413(11) . ?
C31 C32 1.369(10) . ?
C31 O5 1.397(9) . ?
C32 C33 1.381(11) . ?
C32 H32 0.95 . ?
C33 C34 1.364(11) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
C35 O5 1.455(9) . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C36 N3 1.290(10) . ?
C36 C37 1.451(12) . ?
C36 H36 0.95 . ?
C37 C42 1.404(11) . ?
C37 C38 1.411(11) . ?
C38 C39 1.385(12) . ?
C38 H38 0.95 . ?
C39 C40 1.381(12) . ?
C39 H39 0.95 . ?
C40 C41 1.372(10) . ?
C40 H40 0.95 . ?
C41 O7 1.385(9) . ?
C41 C42 1.417(10) . ?
C42 O6 1.332(8) . ?
C43 O7 1.462(9) . ?
C43 H43A 0.98 . ?
C43 H43B 0.98 . ?
C43 H43C 0.98 . ?
C50 N10 1.140(9) 3_756 ?
C50 Co1 1.900(8) . ?
C51 N5 1.135(9) . ?
C51 Co1 1.907(9) . ?
C52 N8 1.140(12) . ?
C52 Co1 1.901(10) . ?
C53 N7 1.141(10) . ?
C53 Co1 1.906(9) . ?
C54 N6 1.149(10) . ?
C54 Co1 1.898(9) . ?
C55 N9 1.164(9) . ?
C55 Co1 1.898(9) . ?
C60 C61 1.458(13) . ?
C60 H60A 0.98 . ?
C60 H60B 0.98 . ?
C60 H60C 0.98 . ?
C61 O21 1.229(11) . ?
C61 C62 1.517(14) . ?
C62 H62A 0.98 . ?
C62 H62B 0.98 . ?
C62 H62C 0.98 . ?
N1 Ni1 2.015(6) . ?
N2 Ni1 2.022(7) . ?
N3 Ni2 2.008(7) . ?
N4 Ni2 2.023(6) . ?
N5 Ni1 1.984(7) . ?
O1 Ni1 2.029(5) . ?
O1 Tb1 2.306(5) . ?
O2 Ni1 2.011(5) . ?
O2 Tb1 2.395(5) . ?
O3 Tb1 2.515(4) . ?
O4 Ni2 2.019(5) . ?
O4 Tb1 2.322(4) . ?
O5 Tb1 2.520(5) . ?
O6 Ni2 2.010(5) . ?
O6 Tb1 2.386(5) . ?
O7 Tb1 2.589(5) . ?
O8 Tb1 2.594(5) . ?
O9 Tb1 2.356(4) . ?
N10 C50 1.140(9) 3_756 ?
N10 Ni2 1.992(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
N1 C1 C2 113.7(8) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C5 110.4(10) . . ?
C3 C2 C1 111.8(9) . . ?
C5 C2 C1 110.8(8) . . ?
C3 C2 C4 106.8(8) . . ?
C5 C2 C4 110.0(9) . . ?
C1 C2 C4 107.0(9) . . ?
N2 C3 C2 114.5(8) . . ?
N2 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
N2 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 127.9(8) . . ?
N1 C6 H6 116 . . ?
C7 C6 H6 116 . . ?
C13 C7 C8 118.2(8) . . ?
C13 C7 C6 123.4(7) . . ?
C8 C7 C6 118.4(8) . . ?
C9 C8 C7 120.9(8) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C10 C9 C8 120.8(8) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.7(8) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 O3 124.6(7) . . ?
C10 C11 C13 120.5(7) . . ?
O3 C11 C13 114.9(6) . . ?
O3 C12 H12A 109.5 . . ?
O3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 C7 123.7(7) . . ?
O1 C13 C11 117.3(6) . . ?
C7 C13 C11 119.0(7) . . ?
N2 C14 C15 128.2(8) . . ?
N2 C14 H14 115.9 . . ?
C15 C14 H14 115.9 . . ?
C21 C15 C16 118.3(8) . . ?
C21 C15 C14 124.7(7) . . ?
C16 C15 C14 116.8(8) . . ?
C18 C16 C15 122.3(9) . . ?
C18 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C18 C19 119.9(8) . . ?
C16 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.0(8) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C19 C20 O8 123.5(7) . . ?
C19 C20 C21 121.6(7) . . ?
O8 C20 C21 114.9(6) . . ?
O2 C21 C20 117.5(7) . . ?
O2 C21 C15 123.6(7) . . ?
C20 C21 C15 118.9(7) . . ?
O8 C22 H22A 109.5 . . ?
O8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O8 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 C24 113.8(7) . . ?
N3 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
N3 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 C25 111.7(7) . . ?
C23 C24 C26 107.9(7) . . ?
C25 C24 C26 107.8(7) . . ?
C23 C24 C27 111.1(7) . . ?
C25 C24 C27 109.1(7) . . ?
C26 C24 C27 109.2(7) . . ?
N4 C25 C24 115.6(7) . . ?
N4 C25 H25A 108.4 . . ?
C24 C25 H25A 108.4 . . ?
N4 C25 H25B 108.4 . . ?
C24 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C29 128.3(7) . . ?
N4 C28 H28 115.8 . . ?
C29 C28 H28 115.8 . . ?
C34 C29 C30 117.5(7) . . ?
C34 C29 C28 118.6(7) . . ?
C30 C29 C28 124.0(7) . . ?
O4 C30 C29 122.1(7) . . ?
O4 C30 C31 119.1(6) . . ?
C29 C30 C31 118.8(6) . . ?
C32 C31 O5 124.7(7) . . ?
C32 C31 C30 121.9(7) . . ?
O5 C31 C30 113.3(6) . . ?
C31 C32 C33 118.9(8) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C34 C33 C32 120.7(7) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C29 122.1(7) . . ?
C33 C34 H34 119 . . ?
C29 C34 H34 119 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C36 C37 127.0(8) . . ?
N3 C36 H36 116.5 . . ?
C37 C36 H36 116.5 . . ?
C42 C37 C38 119.2(8) . . ?
C42 C37 C36 125.0(7) . . ?
C38 C37 C36 115.7(8) . . ?
C39 C38 C37 120.9(8) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C40 C39 C38 119.8(8) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C41 C40 C39 120.4(8) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 O7 125.4(7) . . ?
C40 C41 C42 121.3(7) . . ?
O7 C41 C42 113.3(6) . . ?
O6 C42 C37 123.5(7) . . ?
O6 C42 C41 118.2(7) . . ?
C37 C42 C41 118.3(7) . . ?
O7 C43 H43A 109.5 . . ?
O7 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O7 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N10 C50 Co1 173.5(7) 3_756 . ?
N5 C51 Co1 174.8(7) . . ?
N8 C52 Co1 175.9(10) . . ?
N7 C53 Co1 177.3(8) . . ?
N6 C54 Co1 178.6(8) . . ?
N9 C55 Co1 173.8(7) . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O21 C61 C60 125.1(9) . . ?
O21 C61 C62 117.9(8) . . ?
C60 C61 C62 117.0(9) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C6 N1 C1 115.2(7) . . ?
C6 N1 Ni1 126.7(6) . . ?
C1 N1 Ni1 118.0(5) . . ?
C14 N2 C3 116.4(8) . . ?
C14 N2 Ni1 123.6(6) . . ?
C3 N2 Ni1 119.7(6) . . ?
C36 N3 C23 115.6(7) . . ?
C36 N3 Ni2 124.8(6) . . ?
C23 N3 Ni2 119.3(5) . . ?
C28 N4 C25 115.6(7) . . ?
C28 N4 Ni2 126.0(6) . . ?
C25 N4 Ni2 118.4(5) . . ?
C51 N5 Ni1 163.2(6) . . ?
C13 O1 Ni1 127.5(5) . . ?
C13 O1 Tb1 123.3(4) . . ?
Ni1 O1 Tb1 108.73(19) . . ?
C21 O2 Ni1 127.0(5) . . ?
C21 O2 Tb1 125.5(5) . . ?
Ni1 O2 Tb1 106.0(2) . . ?
C11 O3 C12 117.0(5) . . ?
C11 O3 Tb1 116.2(4) . . ?
C12 O3 Tb1 126.1(4) . . ?
C30 O4 Ni2 129.2(4) . . ?
C30 O4 Tb1 122.2(4) . . ?
Ni2 O4 Tb1 108.30(19) . . ?
C31 O5 C35 115.8(5) . . ?
C31 O5 Tb1 116.7(4) . . ?
C35 O5 Tb1 126.6(4) . . ?
C42 O6 Ni2 127.1(5) . . ?
C42 O6 Tb1 125.1(5) . . ?
Ni2 O6 Tb1 106.25(19) . . ?
C41 O7 C43 114.0(6) . . ?
C41 O7 Tb1 118.1(4) . . ?
C43 O7 Tb1 127.5(4) . . ?
C20 O8 C22 115.8(6) . . ?
C20 O8 Tb1 117.2(4) . . ?
C22 O8 Tb1 126.7(4) . . ?
C50 N10 Ni2 163.3(6) 3_756 . ?
C55 Co1 C54 92.3(3) . . ?
C55 Co1 C50 87.2(3) . . ?
C54 Co1 C50 87.2(3) . . ?
C55 Co1 C52 178.2(4) . . ?
C54 Co1 C52 89.4(4) . . ?
C50 Co1 C52 92.2(4) . . ?
C55 Co1 C53 91.6(3) . . ?
C54 Co1 C53 90.7(4) . . ?
C50 Co1 C53 177.6(3) . . ?
C52 Co1 C53 89.0(4) . . ?
C55 Co1 C51 87.0(3) . . ?
C54 Co1 C51 177.9(3) . . ?
C50 Co1 C51 94.7(3) . . ?
C52 Co1 C51 91.4(4) . . ?
C53 Co1 C51 87.3(3) . . ?
N5 Ni1 O2 101.5(2) . . ?
N5 Ni1 N1 92.3(3) . . ?
O2 Ni1 N1 163.6(2) . . ?
N5 Ni1 N2 92.9(3) . . ?
O2 Ni1 N2 92.3(3) . . ?
N1 Ni1 N2 96.0(3) . . ?
N5 Ni1 O1 113.6(2) . . ?
O2 Ni1 O1 75.80(19) . . ?
N1 Ni1 O1 90.6(2) . . ?
N2 Ni1 O1 152.4(2) . . ?
N10 Ni2 N3 92.2(3) . . ?
N10 Ni2 O6 101.4(2) . . ?
N3 Ni2 O6 92.0(2) . . ?
N10 Ni2 O4 113.9(2) . . ?
N3 Ni2 O4 152.8(2) . . ?
O6 Ni2 O4 76.23(19) . . ?
N10 Ni2 N4 92.4(3) . . ?
N3 Ni2 N4 96.3(3) . . ?
O6 Ni2 N4 163.6(2) . . ?
O4 Ni2 N4 90.2(2) . . ?
O1 Tb1 O4 135.37(17) . . ?
O1 Tb1 O9 112.43(17) . . ?
O4 Tb1 O9 112.20(17) . . ?
O1 Tb1 O6 125.44(16) . . ?
O4 Tb1 O6 63.77(16) . . ?
O9 Tb1 O6 79.74(17) . . ?
O1 Tb1 O2 63.71(16) . . ?
O4 Tb1 O2 125.23(16) . . ?
O9 Tb1 O2 79.64(17) . . ?
O6 Tb1 O2 159.38(16) . . ?
O1 Tb1 O3 65.48(15) . . ?
O4 Tb1 O3 79.11(16) . . ?
O9 Tb1 O3 143.03(16) . . ?
O6 Tb1 O3 74.26(16) . . ?
O2 Tb1 O3 123.86(16) . . ?
O1 Tb1 O5 78.67(17) . . ?
O4 Tb1 O5 65.76(16) . . ?
O9 Tb1 O5 142.75(16) . . ?
O6 Tb1 O5 124.10(16) . . ?
O2 Tb1 O5 73.99(16) . . ?
O3 Tb1 O5 74.22(16) . . ?
O1 Tb1 O7 70.56(17) . . ?
O4 Tb1 O7 124.06(16) . . ?
O9 Tb1 O7 72.92(16) . . ?
O6 Tb1 O7 62.77(16) . . ?
O2 Tb1 O7 110.65(16) . . ?
O3 Tb1 O7 71.97(15) . . ?
O5 Tb1 O7 141.29(15) . . ?
O1 Tb1 O8 123.88(17) . . ?
O4 Tb1 O8 70.32(16) . . ?
O9 Tb1 O8 72.77(16) . . ?
O6 Tb1 O8 110.62(16) . . ?
O2 Tb1 O8 62.72(16) . . ?
O3 Tb1 O8 141.30(15) . . ?
O5 Tb1 O8 71.93(15) . . ?
O7 Tb1 O8 145.69(15) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1048760'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-25 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            'C120 H134 Dy2 N34 Ni4 O20 W2'
_chemical_formula_weight         3300.14

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   16.7120(10)
_cell_length_b                   20.624(2)
_cell_length_c                   20.852(3)
_cell_angle_alpha                87.814(2)
_cell_angle_beta                 89.178(3)
_cell_angle_gamma                74.215(2)
_cell_volume                     6910.9(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    232457
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.330
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.635
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_T_max  0.6350
_exptl_absorpt_process_details   scalepack
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55836
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.417
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             28139
_reflns_number_gt                20982
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+119.7330P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28139
_refine_ls_number_parameters     1637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1463
_refine_ls_wR_factor_gt          0.1374
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.003
_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
C56 C 0.2290(6) 0.0438(6) 0.2053(5) 0.031(2) Uani 1 1 d . . . . .
C57 C 0.2502(7) -0.0072(5) 0.0852(5) 0.031(2) Uiso 1 1 d . . . . .
C58 C 0.2474(7) -0.2213(6) 0.1776(5) 0.030(2) Uani 1 1 d . . . . .
H58 H 0.2195 -0.2224 0.2175 0.037 Uiso 1 1 calc R U . . .
C59 C 0.2766(6) 0.3570(5) 0.5732(5) 0.024(2) Uani 1 1 d . . . . .
C60 C 0.3306(6) 0.3568(5) 0.6246(5) 0.025(2) Uani 1 1 d . . . . .
C70 C 0.7002(7) 0.3421(5) 0.5970(5) 0.027(2) Uani 1 1 d . . . . .
C71 C 0.8292(7) 0.3292(5) 0.6683(5) 0.028(2) Uani 1 1 d . . . . .
C72 C 0.8852(7) 0.4324(5) 0.6178(5) 0.029(2) Uani 1 1 d . . . . .
C73 C 0.6370(7) 0.4600(5) 0.6443(5) 0.024(2) Uani 1 1 d . . . . .
C74 C 0.6976(7) 0.4580(5) 0.5242(5) 0.027(2) Uani 1 1 d . . . . .
C75 C 0.7769(7) 0.2017(5) 0.4538(6) 0.035(3) Uani 1 1 d . . . . .
H75 H 0.8326 0.1928 0.4387 0.042 Uiso 1 1 calc R U . . .
C76 C 0.7119(7) 0.2252(5) 0.4060(5) 0.030(2) Uani 1 1 d . . . . .
C77 C 0.4359(7) 0.3353(6) 0.3371(5) 0.036(3) Uani 1 1 d . . . . .
H77A H 0.3788 0.3484 0.3536 0.054 Uiso 1 1 calc R U . . .
H77B H 0.4541 0.3758 0.3268 0.054 Uiso 1 1 calc R U . . .
H77C H 0.4380 0.3095 0.2983 0.054 Uiso 1 1 calc R U . . .
C78 C 0.3040(7) 0.1862(6) 0.5653(5) 0.035(3) Uani 1 1 d . . . . .
H78A H 0.2751 0.2145 0.5294 0.053 Uiso 1 1 calc R U . . .
H78B H 0.3099 0.1387 0.5570 0.053 Uiso 1 1 calc R U . . .
H78C H 0.2718 0.1983 0.6049 0.053 Uiso 1 1 calc R U . . .
C79 C 0.8358(7) 0.3606(5) 0.5371(5) 0.030(2) Uani 1 1 d . . . . .
C80 C 0.1604(7) 0.1569(6) 0.0379(5) 0.032(2) Uani 1 1 d . . . . .
C81 C 0.5152(7) 0.1709(6) 0.1770(5) 0.036(3) Uani 1 1 d . . . . .
H81A H 0.4594 0.1948 0.1619 0.054 Uiso 1 1 calc R U . . .
H81B H 0.5182 0.1232 0.1855 0.054 Uiso 1 1 calc R U . . .
H81C H 0.5269 0.1907 0.2166 0.054 Uiso 1 1 calc R U . . .
C82 C 0.0666(6) -0.0978(6) 0.0450(5) 0.033(3) Uani 1 1 d . . . . .
H82A H 0.0194 -0.0990 0.0173 0.040 Uiso 1 1 calc R U . . .
H82B H 0.0599 -0.0502 0.0555 0.040 Uiso 1 1 calc R U . . .
C83 C 0.0615(6) -0.1371(6) 0.1059(6) 0.035(3) Uani 1 1 d . . . . .
C84 C 0.1285(6) -0.1342(6) 0.1548(5) 0.034(3) Uani 1 1 d . . . . .
H84A H 0.1297 -0.0868 0.1585 0.041 Uiso 1 1 calc R U . . .
H84B H 0.1136 -0.1505 0.1974 0.041 Uiso 1 1 calc R U . . .
C85 C 0.2090(7) 0.3712(6) 0.1603(5) 0.035(3) Uani 1 1 d . . . . .
H85A H 0.1965 0.4037 0.1952 0.041 Uiso 1 1 calc R U . . .
H85B H 0.2032 0.3276 0.1782 0.041 Uiso 1 1 calc R U . . .
C86 C 0.1437(7) 0.3963(5) 0.1074(6) 0.035(3) Uani 1 1 d . . . . .
C87 C 0.1482(6) 0.3426(5) 0.0590(5) 0.029(2) Uani 1 1 d . . . . .
H87A H 0.1011 0.3586 0.0289 0.035 Uiso 1 1 calc R U . . .
H87B H 0.1413 0.3016 0.0820 0.035 Uiso 1 1 calc R U . . .
C88 C 0.3991(7) 0.2279(5) -0.1807(5) 0.035(3) Uani 1 1 d . . . . .
H88 H 0.4378 0.2067 -0.2124 0.041 Uiso 1 1 calc R U . . .
C89 C 0.3153(8) 0.2585(6) -0.1965(5) 0.044(3) Uani 1 1 d . . . . .
H89 H 0.2972 0.2596 -0.2396 0.052 Uiso 1 1 calc R U . . .
C90 C 0.2604(8) 0.2866(6) -0.1498(6) 0.045(3) Uani 1 1 d . . . . .
H90 H 0.2038 0.3058 -0.1612 0.054 Uiso 1 1 calc R U . . .
C91 C 0.6860(8) 0.2524(6) 0.2927(5) 0.042(3) Uani 1 1 d . . . . .
H91 H 0.7062 0.2531 0.2500 0.051 Uiso 1 1 calc R U . . .
C92 C 0.6003(7) 0.2758(5) 0.3053(5) 0.032(2) Uani 1 1 d . . . . .
H92 H 0.5622 0.2936 0.2716 0.039 Uiso 1 1 calc R U . . .
C93 C 0.3022(7) 0.3824(6) 0.6830(5) 0.037(3) Uani 1 1 d . . . . .
H93 H 0.3397 0.3822 0.7168 0.044 Uiso 1 1 calc R U . . .
C94 C 0.2163(8) 0.4089(7) 0.6914(6) 0.047(3) Uani 1 1 d . . . . .
H94 H 0.1956 0.4263 0.7318 0.057 Uiso 1 1 calc R U . . .
C95 C 0.1613(7) 0.4104(6) 0.6427(6) 0.043(3) Uani 1 1 d . . . . .
H95 H 0.1035 0.4296 0.6494 0.052 Uiso 1 1 calc R U . . .
C96 C 0.1902(6) 0.3833(5) 0.5827(5) 0.027(2) Uani 1 1 d . . . . .
C97 C 0.8720(6) 0.6117(5) 0.4655(5) 0.027(2) Uani 1 1 d . . . . .
H97 H 0.9275 0.5909 0.4524 0.032 Uiso 1 1 calc R U . . .
C99 C -0.0216(7) -0.1041(7) 0.1382(6) 0.048(3) Uani 1 1 d . . . . .
H99A H -0.0266 -0.1290 0.1783 0.072 Uiso 1 1 calc R U . . .
H99B H -0.0243 -0.0574 0.1473 0.072 Uiso 1 1 calc R U . . .
H99C H -0.0673 -0.1049 0.1095 0.072 Uiso 1 1 calc R U . . .
C100 C 0.0666(8) -0.2120(6) 0.0942(6) 0.048(3) Uani 1 1 d . . . . .
H10D H 0.0630 -0.2357 0.1353 0.072 Uiso 1 1 calc R U . . .
H10E H 0.0206 -0.2144 0.0666 0.072 Uiso 1 1 calc R U . . .
H10F H 0.1196 -0.2334 0.0732 0.072 Uiso 1 1 calc R U . . .
C101 C 0.5520(7) 0.1458(6) -0.1333(6) 0.040(3) Uani 1 1 d . . . . .
H10A H 0.6070 0.1282 -0.1138 0.059 Uiso 1 1 calc R U . . .
H10B H 0.5244 0.1096 -0.1347 0.059 Uiso 1 1 calc R U . . .
H10C H 0.5581 0.1630 -0.1770 0.059 Uiso 1 1 calc R U . . .
C102 C 0.8393(8) 0.0567(6) 0.5789(7) 0.052(4) Uani 1 1 d . . . . .
H10J H 0.8812 0.0408 0.5456 0.078 Uiso 1 1 calc R U . . .
H10K H 0.8461 0.0223 0.6136 0.078 Uiso 1 1 calc R U . . .
H10L H 0.7836 0.0654 0.5605 0.078 Uiso 1 1 calc R U . . .
C103 C 0.9354(7) 0.1064(6) 0.6363(6) 0.044(3) Uani 1 1 d . . . . .
H10M H 0.9785 0.0889 0.6042 0.066 Uiso 1 1 calc R U . . .
H10N H 0.9434 0.1478 0.6533 0.066 Uiso 1 1 calc R U . . .
H10O H 0.9394 0.0727 0.6714 0.066 Uiso 1 1 calc R U . . .
C104 C 0.5516(8) 0.0983(6) 0.4685(6) 0.047(3) Uani 1 1 d . . . . .
H1A4 H 0.5274 0.0600 0.4725 0.071 Uiso 1 1 calc R U . . .
H1B4 H 0.5749 0.1047 0.5099 0.071 Uiso 1 1 calc R U . . .
H1C4 H 0.5958 0.0892 0.4360 0.071 Uiso 1 1 calc R U . . .
C105 C 0.0587(7) 0.4089(6) 0.1393(6) 0.043(3) Uani 1 1 d . . . . .
H10G H 0.0528 0.4435 0.1713 0.064 Uiso 1 1 calc R U . . .
H10H H 0.0152 0.4242 0.1068 0.064 Uiso 1 1 calc R U . . .
H10I H 0.0533 0.3670 0.1605 0.064 Uiso 1 1 calc R U . . .
C106 C 0.1524(8) 0.4625(6) 0.0767(7) 0.049(3) Uani 1 1 d . . . . .
H10P H 0.1490 0.4954 0.1101 0.074 Uiso 1 1 calc R U . . .
H10Q H 0.2061 0.4546 0.0547 0.074 Uiso 1 1 calc R U . . .
H10R H 0.1074 0.4801 0.0458 0.074 Uiso 1 1 calc R U . . .
C107 C 0.4511(7) 0.3995(5) -0.0394(5) 0.040(3) Uani 1 1 d . . . . .
H1A7 H 0.4751 0.4373 -0.0485 0.060 Uiso 1 1 calc R U . . .
H1B7 H 0.4333 0.3998 0.0056 0.060 Uiso 1 1 calc R U . . .
H1C7 H 0.4030 0.4041 -0.0672 0.060 Uiso 1 1 calc R U . . .
C108 C 0.7393(7) 0.2288(6) 0.3415(5) 0.036(3) Uani 1 1 d . . . . .
H108 H 0.7971 0.2141 0.3324 0.044 Uiso 1 1 calc R U . . .
C110 C 0.6863(8) 0.1212(6) 0.2037(5) 0.041(3) Uani 1 1 d . . . . .
H110 H 0.6483 0.1241 0.2384 0.050 Uiso 1 1 calc R U . . .
C111 C 0.7709(8) 0.0933(7) 0.2138(6) 0.048(3) Uani 1 1 d . . . . .
H111 H 0.7906 0.0766 0.2553 0.058 Uiso 1 1 calc R U . . .
C112 C 0.8258(7) 0.0899(6) 0.1635(6) 0.044(3) Uani 1 1 d . . . . .
H112 H 0.8837 0.0723 0.1711 0.052 Uiso 1 1 calc R U . . .
C113 C 0.0911(8) 0.2072(8) 0.5721(7) 0.052(3) Uani 1 1 d . . . . .
C114 C 0.0484(9) 0.2589(7) 0.6125(8) 0.067(4) Uani 1 1 d . . . . .
H11X H 0.0403 0.2393 0.6549 0.100 Uiso 1 1 calc R U . . .
H11W H -0.0059 0.2819 0.5938 0.100 Uiso 1 1 calc R U . . .
H11Z H 0.0810 0.2914 0.6169 0.100 Uiso 1 1 calc R U . . .
C115 C 0.7190(10) 0.9379(8) 0.5595(8) 0.060(4) Uani 1 1 d . . . . .
C116 C 0.7878(9) 0.8999(6) 0.5979(7) 0.058(4) Uani 1 1 d . . . . .
H11D H 0.7853 0.8531 0.6030 0.087 Uiso 1 1 calc R U . . .
H11E H 0.7850 0.9196 0.6402 0.087 Uiso 1 1 calc R U . . .
H11F H 0.8401 0.9011 0.5766 0.087 Uiso 1 1 calc R U . . .
C117 C 0.7926(12) 0.8643(12) 0.2249(10) 0.090(6) Uani 1 1 d . . . . .
C118 C 0.7515(12) 0.8980(10) 0.1680(10) 0.108(8) Uani 1 1 d . . . . .
H11G H 0.7689 0.9391 0.1587 0.163 Uiso 1 1 calc R U . . .
H11H H 0.6912 0.9099 0.1746 0.163 Uiso 1 1 calc R U . . .
H11I H 0.7664 0.8681 0.1318 0.163 Uiso 1 1 calc R U . . .
C119 C 0.3025(10) 0.5600(7) 0.0564(8) 0.059(4) Uani 1 1 d . . . . .
C120 C 0.2498(10) 0.6027(9) 0.0971(6) 0.070(5) Uani 1 1 d . . . . .
H12X H 0.2489 0.6494 0.0856 0.105 Uiso 1 1 calc R U . . .
H12W H 0.2692 0.5919 0.1414 0.105 Uiso 1 1 calc R U . . .
H12Z H 0.1936 0.5972 0.0935 0.105 Uiso 1 1 calc R U . . .
C121 C 0.7354(9) 0.5151(7) 0.1522(7) 0.049(3) Uani 1 1 d . . . . .
C122 C 0.8055(11) 0.4935(9) 0.1093(9) 0.087(6) Uani 1 1 d . . . . .
H12D H 0.8405 0.4495 0.1244 0.130 Uiso 1 1 calc R U . . .
H12E H 0.8381 0.5265 0.1084 0.130 Uiso 1 1 calc R U . . .
H12F H 0.7855 0.4899 0.0660 0.130 Uiso 1 1 calc R U . . .
C123 C 0.0237(11) 0.3865(8) 0.8256(10) 0.081(5) Uani 1 1 d . . . . .
C124 C -0.0129(13) 0.3582(9) 0.7782(9) 0.092(6) Uani 1 1 d . . . . .
C125 C 0.9069(9) 0.3022(9) 0.0657(9) 0.066(5) Uani 1 1 d . . . . .
C126 C 0.9456(10) 0.2478(8) 0.1097(9) 0.078(5) Uani 1 1 d . . . . .
H12G H 0.9060 0.2219 0.1215 0.118 Uiso 1 1 calc R U . . .
H12H H 0.9626 0.2660 0.1483 0.118 Uiso 1 1 calc R U . . .
H12I H 0.9945 0.2182 0.0893 0.118 Uiso 1 1 calc R U . . .
C127 C 0.2613(11) 0.9960(8) 0.6378(8) 0.063(4) Uani 1 1 d . . . . .
C128 C 0.1861(14) 1.0061(13) 0.6034(11) 0.133(10) Uani 1 1 d . . . . .
H12J H 0.1919 0.9699 0.5731 0.200 Uiso 1 1 calc R U . . .
H12K H 0.1738 1.0496 0.5797 0.200 Uiso 1 1 calc R U . . .
H12L H 0.1407 1.0057 0.6335 0.200 Uiso 1 1 calc R U . . .
C129 C 0.7710(6) 0.4485(6) 0.7104(5) 0.031(2) Uani 1 1 d . . . . .
C130 C 0.4720(7) 0.3394(6) 0.6550(5) 0.036(3) Uani 1 1 d . . . . .
H1A0 H 0.4624 0.3879 0.6603 0.054 Uiso 1 1 calc R U . . .
H1B0 H 0.5286 0.3203 0.6389 0.054 Uiso 1 1 calc R U . . .
H1C0 H 0.4653 0.3175 0.6965 0.054 Uiso 1 1 calc R U . . .
C131 C 1.0118(12) 0.1185(10) 0.2799(8) 0.091(6) Uani 1 1 d . . . . .
H13D H 0.9747 0.1120 0.2462 0.136 Uiso 1 1 calc R U . . .
H13E H 1.0673 0.0878 0.2739 0.136 Uiso 1 1 calc R U . . .
H13F H 1.0152 0.1652 0.2776 0.136 Uiso 1 1 calc R U . . .
C132 C 0.6969(6) 0.3066(6) 0.0674(6) 0.035(3) Uani 1 1 d . . . . .
H1A2 H 0.6970 0.3538 0.0603 0.053 Uiso 1 1 calc R U . . .
H1B2 H 0.7220 0.2807 0.0303 0.053 Uiso 1 1 calc R U . . .
H1C2 H 0.7290 0.2880 0.1060 0.053 Uiso 1 1 calc R U . . .
C135 C 0.7843(9) 0.3752(8) 0.2684(8) 0.061(4) Uani 1 1 d . . . . .
C136 C 0.7399(9) 0.4065(10) 0.3278(8) 0.087(6) Uani 1 1 d . . . . .
H13A H 0.6827 0.4028 0.3280 0.131 Uiso 1 1 calc R U . . .
H13B H 0.7394 0.4541 0.3280 0.131 Uiso 1 1 calc R U . . .
H13C H 0.7689 0.3828 0.3660 0.131 Uiso 1 1 calc R U . . .
C137 C 0.1601(6) 0.1708(5) 0.1714(5) 0.026(2) Uani 1 1 d . . . . .
C139 C 0.9801(9) 0.1047(8) 0.3406(9) 0.064(4) Uani 1 1 d . . . . .
C141 C 0.2868(6) 0.1745(5) 0.1119(5) 0.026(2) Uiso 1 1 d . . . . .
C142 C 0.7525(6) 0.5219(5) 0.6040(5) 0.024(2) Uiso 1 1 d . . . . .
N10 N 0.2247(6) 0.0164(5) 0.2541(5) 0.040(2) Uani 1 1 d . . . . .
N11 N 0.1226(6) 0.2145(5) 0.2030(4) 0.035(2) Uani 1 1 d . . . . .
N12 N 0.2113(5) -0.1749(4) 0.1364(4) 0.0263(19) Uani 1 1 d . . . . .
N13 N 0.1452(5) -0.1218(4) 0.0075(4) 0.0272(19) Uani 1 1 d . . . . .
N14 N 0.6701(5) 0.2986(4) 0.5878(4) 0.0243(18) Uani 1 1 d . . . . .
N15 N 0.2282(5) 0.3241(4) 0.0207(4) 0.030(2) Uani 1 1 d . . . . .
N16 N 0.2957(5) 0.3621(4) 0.1403(4) 0.0266(19) Uani 1 1 d . . . . .
N18 N 0.3179(5) 0.2190(4) 0.1070(4) 0.029(2) Uani 1 1 d . . . . .
N19 N 0.5686(6) 0.4832(4) 0.6587(4) 0.031(2) Uani 1 1 d . . . . .
N20 N 0.9510(6) 0.4411(5) 0.6220(5) 0.042(2) Uani 1 1 d . . . . .
N22 N 0.8712(6) 0.3287(5) 0.4970(5) 0.047(3) Uani 1 1 d . . . . .
N23 N 0.6615(6) 0.4819(5) 0.4793(4) 0.040(2) Uani 1 1 d . . . . .
N24 N 0.1224(7) 0.1905(5) -0.0012(5) 0.050(3) Uani 1 1 d . . . . .
N25 N 0.8631(6) 0.2822(4) 0.6972(4) 0.031(2) Uani 1 1 d . . . . .
N26 N 0.1241(8) 0.1649(7) 0.5402(7) 0.074(4) Uani 1 1 d . . . . .
N27 N 0.0520(11) 0.4104(8) 0.8641(11) 0.124(8) Uani 1 1 d . . . . .
N28 N 0.8760(11) 0.3445(9) 0.0321(8) 0.099(5) Uani 1 1 d . . . . .
N29 N 0.3198(9) 0.9871(8) 0.6675(8) 0.083(4) Uani 1 1 d . . . . .
N30 N 0.6650(11) 0.9673(8) 0.5278(8) 0.098(5) Uani 1 1 d . . . . .
N31 N 0.6787(8) 0.5325(7) 0.1837(6) 0.068(4) Uani 1 1 d . . . . .
N32 N 0.8257(13) 0.8388(12) 0.2684(10) 0.131(7) Uani 1 1 d . . . . .
N33 N 0.7757(7) 0.4672(5) 0.7612(5) 0.047(3) Uani 1 1 d . . . . .
N34 N 0.3444(11) 0.5266(8) 0.0199(9) 0.109(6) Uani 1 1 d . . . . .
N35 N 0.8146(9) 0.3520(8) 0.2220(7) 0.077(4) Uani 1 1 d . . . . .
N38 N 0.9535(11) 0.0948(7) 0.3872(9) 0.107(6) Uani 1 1 d . . . . .
O19 O 0.5573(5) 0.4221(4) 0.4082(4) 0.0397(19) Uani 1 1 d . . . . .
O20 O 0.4183(5) 0.9769(4) 0.8987(4) 0.0344(18) Uani 1 1 d . . . . .
O18 O 0.5133(5) 0.1274(4) 0.0218(4) 0.042(2) Uani 1 1 d . . . . .
H12A H -0.0416 0.3267 0.7979 0.080 Uiso 1 1 d . U . . .
H12B H 0.0306 0.3331 0.7489 0.080 Uiso 1 1 d . U . . .
H12C H -0.0527 0.3935 0.7536 0.080 Uiso 1 1 d . U . . .
C1 C 0.3718(6) 0.2059(5) 0.3851(4) 0.023(2) Uani 1 1 d . . . . .
C2 C 0.4442(6) 0.1541(5) 0.3935(4) 0.024(2) Uani 1 1 d . . . . .
C3 C 0.4693(7) 0.1024(5) 0.3513(5) 0.031(2) Uani 1 1 d . . . . .
H3 H 0.5187 0.0672 0.3587 0.037 Uiso 1 1 calc R U . . .
C4 C 0.4209(7) 0.1032(6) 0.2980(5) 0.036(3) Uani 1 1 d . . . . .
H4 H 0.4376 0.0686 0.2679 0.043 Uiso 1 1 calc R U . . .
C5 C 0.3483(7) 0.1539(6) 0.2881(5) 0.032(3) Uani 1 1 d . . . . .
H5 H 0.3152 0.1532 0.2516 0.039 Uiso 1 1 calc R U . . .
C6 C 0.3224(6) 0.2065(5) 0.3311(4) 0.025(2) Uani 1 1 d . . . . .
C7 C 0.2440(7) 0.2553(5) 0.3187(5) 0.030(2) Uani 1 1 d . . . . .
H7 H 0.2169 0.2508 0.2800 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8742(6) 0.6527(6) 0.6677(5) 0.031(2) Uani 1 1 d . . . . .
H8A H 0.8701 0.6060 0.6751 0.037 Uiso 1 1 calc R U . . .
H8B H 0.8877 0.6689 0.7092 0.037 Uiso 1 1 calc R U . . .
C9 C 0.9457(6) 0.6520(5) 0.6198(5) 0.029(2) Uani 1 1 d . . . . .
C10 C 0.9404(7) 0.6100(6) 0.5630(5) 0.034(3) Uani 1 1 d . . . . .
H10S H 0.9883 0.6096 0.5344 0.041 Uiso 1 1 calc R U . . .
H10T H 0.9468 0.5631 0.5790 0.041 Uiso 1 1 calc R U . . .
C11 C 0.9445(7) 0.7242(5) 0.5985(6) 0.037(3) Uani 1 1 d . . . . .
H11A H 0.9480 0.7501 0.6362 0.055 Uiso 1 1 calc R U . . .
H11B H 0.9920 0.7232 0.5701 0.055 Uiso 1 1 calc R U . . .
H11C H 0.8927 0.7454 0.5754 0.055 Uiso 1 1 calc R U . . .
C12 C 1.0272(7) 0.6172(6) 0.6551(6) 0.042(3) Uani 1 1 d . . . . .
H12M H 1.0327 0.6432 0.6924 0.063 Uiso 1 1 calc R U . . .
H12N H 1.0265 0.5716 0.6695 0.063 Uiso 1 1 calc R U . . .
H12P H 1.0744 0.6147 0.6260 0.063 Uiso 1 1 calc R U . . .
C13 C 0.6279(6) 0.2472(5) 0.4188(4) 0.023(2) Uani 1 1 d . . . . .
C14 C 0.5733(7) 0.2725(5) 0.3667(5) 0.028(2) Uani 1 1 d . . . . .
C15 C 0.8456(6) 0.1736(6) 0.5514(5) 0.031(2) Uani 1 1 d . . . . .
H15A H 0.8531 0.2151 0.5697 0.037 Uiso 1 1 calc R U . . .
H15B H 0.8926 0.1564 0.5216 0.037 Uiso 1 1 calc R U . . .
C16 C 0.8502(7) 0.1215(5) 0.6055(5) 0.032(2) Uani 1 1 d . . . . .
C17 C 0.7868(6) 0.1482(5) 0.6574(5) 0.030(2) Uani 1 1 d . . . . .
H17A H 0.7994 0.1171 0.6955 0.036 Uiso 1 1 calc R U . . .
H17B H 0.7925 0.1925 0.6701 0.036 Uiso 1 1 calc R U . . .
C18 C 0.6564(7) 0.1260(5) 0.6743(5) 0.032(3) Uani 1 1 d . . . . .
H18 H 0.6861 0.0990 0.7088 0.038 Uiso 1 1 calc R U . . .
C19 C 0.5708(6) 0.1270(5) 0.6703(4) 0.025(2) Uani 1 1 d . . . . .
C20 C 0.5155(6) 0.1659(5) 0.6233(4) 0.022(2) Uani 1 1 d . . . . .
C21 C 0.4339(6) 0.1599(5) 0.6218(5) 0.026(2) Uani 1 1 d . . . . .
C22 C 0.4064(7) 0.1181(5) 0.6647(5) 0.031(2) Uani 1 1 d . . . . .
H22 H 0.3508 0.1150 0.6631 0.037 Uiso 1 1 calc R U . . .
C23 C 0.4618(7) 0.0803(5) 0.7110(5) 0.033(3) Uani 1 1 d . . . . .
H23 H 0.4436 0.0518 0.7413 0.040 Uiso 1 1 calc R U . . .
C24 C 0.5417(7) 0.0846(5) 0.7125(5) 0.029(2) Uani 1 1 d . . . . .
H24 H 0.5788 0.0577 0.7434 0.035 Uiso 1 1 calc R U . . .
C30 C 0.4806(6) 0.3447(5) 0.1229(4) 0.022(2) Uani 1 1 d . . . . .
C31 C 0.5637(6) 0.3466(5) 0.1200(4) 0.023(2) Uani 1 1 d . . . . .
C32 C 0.5925(7) 0.3897(5) 0.1550(5) 0.029(2) Uani 1 1 d . . . . .
H32 H 0.6492 0.3898 0.1517 0.035 Uiso 1 1 calc R U . . .
C34 C 0.5390(7) 0.4337(5) 0.1958(5) 0.032(3) Uani 1 1 d . . . . .
H34 H 0.5591 0.4635 0.2208 0.039 Uiso 1 1 calc R U . . .
C35 C 0.4574(7) 0.4337(5) 0.1995(5) 0.031(2) Uani 1 1 d . . . . .
H35 H 0.4208 0.4642 0.2268 0.037 Uiso 1 1 calc R U . . .
C36 C 0.4258(6) 0.3889(5) 0.1633(5) 0.026(2) Uani 1 1 d . . . . .
C37 C 0.3392(7) 0.3926(5) 0.1723(5) 0.031(2) Uani 1 1 d . . . . .
H37 H 0.3109 0.4206 0.2054 0.038 Uiso 1 1 calc R U . . .
C38 C 0.3687(6) 0.2598(5) -0.0690(5) 0.025(2) Uani 1 1 d . . . . .
C39 C 0.2840(7) 0.2886(5) -0.0850(5) 0.030(2) Uani 1 1 d . . . . .
C40 C 0.2188(7) 0.3162(5) -0.0389(5) 0.033(3) Uani 1 1 d . . . . .
H40 H 0.1635 0.3297 -0.0547 0.039 Uiso 1 1 calc R U . . .
C41 C 0.4237(6) 0.2294(5) -0.1172(5) 0.026(2) Uani 1 1 d . . . . .
C42 C 0.5543(6) 0.3326(5) -0.1099(5) 0.027(2) Uani 1 1 d . . . . .
C43 C 0.6253(6) 0.2785(5) -0.1137(5) 0.023(2) Uani 1 1 d . . . . .
C44 C 0.5301(7) 0.3781(5) -0.1602(5) 0.033(3) Uani 1 1 d . . . . .
H44 H 0.4817 0.4147 -0.1562 0.040 Uiso 1 1 calc R U . . .
C45 C 0.5754(7) 0.3714(6) -0.2166(5) 0.037(3) Uani 1 1 d . . . . .
H45 H 0.5580 0.4024 -0.2518 0.045 Uiso 1 1 calc R U . . .
C46 C 0.3524(7) -0.3178(6) 0.2207(5) 0.033(3) Uani 1 1 d . . . . .
H46 H 0.3208 -0.3128 0.2593 0.040 Uiso 1 1 calc R U . . .
C47 C 0.3260(7) -0.2720(5) 0.1700(4) 0.025(2) Uani 1 1 d . . . . .
C48 C 0.6580(6) 0.1446(5) 0.1440(5) 0.027(2) Uani 1 1 d . . . . .
C49 C 0.7133(7) 0.1405(5) 0.0914(5) 0.027(2) Uani 1 1 d . . . . .
C50 C 0.7981(6) 0.1117(5) 0.1018(5) 0.031(2) Uani 1 1 d . . . . .
C51 C 0.1382(7) -0.1054(5) -0.0534(5) 0.032(2) Uani 1 1 d . . . . .
H51 H 0.0829 -0.0864 -0.0681 0.039 Uiso 1 1 calc R U . . .
C52 C 0.3602(6) 0.0463(5) 0.1432(5) 0.023(2) Uani 1 1 d . . . . .
C53 C 0.1128(6) 0.0734(5) 0.1184(5) 0.028(2) Uani 1 1 d . . . . .
C55 C 0.3118(7) 0.0858(5) 0.0275(5) 0.027(2) Uani 1 1 d . . . . .
Dy1 Dy 0.44942(3) 0.27048(2) 0.50165(2) 0.02022(11) Uani 1 1 d . . . . .
Dy2 Dy 0.54318(3) 0.22927(2) 0.01518(2) 0.01993(11) Uani 1 1 d . . . . .
N1 N 0.7444(5) 0.5811(4) 0.5955(4) 0.029(2) Uani 1 1 d . . . . .
N2 N 0.8638(5) 0.6314(4) 0.5241(4) 0.0267(19) Uani 1 1 d . . . . .
N3 N 0.7938(5) 0.6952(4) 0.6459(4) 0.0253(19) Uani 1 1 d . . . . .
N4 N 0.7672(5) 0.1915(4) 0.5141(4) 0.030(2) Uani 1 1 d . . . . .
N5 N 0.6996(5) 0.1562(4) 0.6383(4) 0.0273(19) Uani 1 1 d . . . . .
N6 N 0.4275(5) 0.0216(4) 0.1583(4) 0.0260(19) Uani 1 1 d . . . . .
N7 N 0.2604(5) -0.0638(4) 0.0686(4) 0.0280(19) Uani 1 1 d . . . . .
N8 N 0.3560(6) 0.0840(5) -0.0154(4) 0.036(2) Uani 1 1 d . . . . .
N9 N 0.0497(6) 0.0613(5) 0.1217(5) 0.038(2) Uani 1 1 d . . . . .
Ni1 Ni 0.75206(8) 0.67139(6) 0.56308(6) 0.0212(3) Uani 1 1 d . . . . .
Ni2 Ni 0.65584(8) 0.21229(6) 0.55850(6) 0.0217(3) Uani 1 1 d . . . . .
Ni3 Ni 0.33749(8) 0.30265(6) 0.06623(6) 0.0229(3) Uani 1 1 d . . . . .
Ni4 Ni 0.25642(8) -0.15687(6) 0.04935(6) 0.0213(3) Uani 1 1 d . . . . .
O1 O 0.4874(4) 0.1590(3) 0.4495(3) 0.0281(16) Uani 1 1 d . . . . .
O2 O 0.3520(4) 0.2536(3) 0.4296(3) 0.0248(15) Uani 1 1 d . . . . .
O3 O 0.3097(4) 0.3309(3) 0.5182(3) 0.0245(15) Uani 1 1 d . . . . .
O4 O 0.3859(4) 0.1969(3) 0.5725(3) 0.0252(15) Uani 1 1 d . . . . .
O5 O 0.5384(4) 0.2066(3) 0.5791(3) 0.0235(15) Uani 1 1 d . . . . .
O6 O 0.5938(4) 0.2468(3) 0.4777(3) 0.0226(14) Uani 1 1 d . . . . .
O7 O 0.4902(4) 0.2941(3) 0.3852(3) 0.0250(15) Uani 1 1 d . . . . .
O8 O 0.4605(4) 0.3787(4) 0.4930(4) 0.0385(19) Uani 1 1 d . . . . .
O9 O 0.4127(4) 0.3281(3) 0.6098(3) 0.0264(16) Uani 1 1 d . . . . .
O10 O 0.4563(4) 0.3014(3) 0.0856(3) 0.0239(15) Uani 1 1 d . . . . .
O11 O 0.6117(4) 0.3027(3) 0.0758(3) 0.0256(15) Uani 1 1 d . . . . .
O12 O 0.3992(4) 0.2597(3) -0.0101(3) 0.0208(14) Uani 1 1 d . . . . .
O13 O 0.5132(4) 0.3363(3) -0.0514(3) 0.0248(15) Uani 1 1 d . . . . .
O14 O 0.6449(4) 0.2362(3) -0.0622(3) 0.0232(15) Uani 1 1 d . . . . .
O15 O 0.6803(4) 0.1626(3) 0.0339(3) 0.0206(14) Uani 1 1 d . . . . .
O16 O 0.5028(4) 0.1994(3) -0.0958(3) 0.0266(16) Uani 1 1 d . . . . .
O17 O 0.5756(4) 0.1766(3) 0.1286(3) 0.0251(15) Uani 1 1 d . . . . .
W1 W 0.76333(2) 0.41876(2) 0.61287(2) 0.02078(10) Uani 1 1 d . . . . .
W2 W 0.23366(2) 0.09276(2) 0.11243(2) 0.02024(9) Uani 1 1 d . . . . .
H1O8 H 0.4300 0.4136 0.5113 0.050 Uiso 1 1 d . U . . .
H2O8 H 0.5102 0.3735 0.5072 0.050 Uiso 1 1 d . U . . .
H19A H 0.5897 0.4389 0.4301 0.050 Uiso 1 1 d . U . . .
H19B H 0.5268 0.4079 0.4360 0.050 Uiso 1 1 d . U . . .
H20A H 0.4663 0.9799 0.8859 0.050 Uiso 1 1 d . U . . .
H20B H 0.4012 1.0081 0.9259 0.050 Uiso 1 1 d . U . . .
H18A H 0.5070 0.0905 0.0395 0.050 Uiso 1 1 d . U . . .
H18B H 0.4914 0.1305 -0.0155 0.050 Uiso 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
C56 N10 1.157(13) . ?
C56 W2 2.159(11) . ?
C57 N7 1.196(13) . ?
C57 W2 2.104(11) . ?
C58 N12 1.286(13) . ?
C58 C47 1.451(15) . ?
C59 O3 1.333(11) . ?
C59 C60 1.410(13) . ?
C59 C96 1.411(14) . ?
C60 C93 1.373(14) . ?
C60 O9 1.374(12) . ?
C70 N14 1.164(12) . ?
C70 W1 2.163(11) . ?
C71 N25 1.136(13) . ?
C71 W1 2.174(11) . ?
C72 N20 1.165(13) . ?
C72 W1 2.135(11) . ?
C73 N19 1.153(13) . ?
C73 W1 2.153(11) . ?
C74 N23 1.142(13) . ?
C74 W1 2.177(11) . ?
C75 N4 1.282(14) . ?
C75 C76 1.455(15) . ?
C76 C13 1.379(14) . ?
C76 C108 1.420(14) . ?
C77 O7 1.448(12) . ?
C78 O4 1.455(12) . ?
C79 N22 1.140(13) . ?
C79 W1 2.168(10) . ?
C80 N24 1.132(14) . ?
C80 W2 2.163(12) . ?
C81 O17 1.442(12) . ?
C82 N13 1.492(13) . ?
C82 C83 1.494(16) . ?
C83 C99 1.529(15) . ?
C83 C84 1.540(15) . ?
C83 C100 1.553(15) . ?
C84 N12 1.465(13) . ?
C85 N16 1.465(13) . ?
C85 C86 1.535(16) . ?
C86 C87 1.511(15) . ?
C86 C105 1.522(14) . ?
C86 C106 1.528(15) . ?
C87 N15 1.512(13) . ?
C88 C41 1.396(14) . ?
C88 C89 1.409(16) . ?
C89 C90 1.363(16) . ?
C90 C39 1.418(15) . ?
C91 C108 1.347(16) . ?
C91 C92 1.405(16) . ?
C92 C14 1.356(14) . ?
C93 C94 1.401(16) . ?
C94 C95 1.374(16) . ?
C95 C96 1.415(14) . ?
C96 C97 1.437(14) 2_666 ?
C97 N2 1.296(13) . ?
C97 C96 1.437(14) 2_666 ?
C101 O16 1.436(12) . ?
C102 C16 1.522(15) . ?
C103 C16 1.519(15) . ?
C104 O1 1.456(12) . ?
C107 O13 1.457(12) . ?
C110 C48 1.361(14) . ?
C110 C111 1.389(16) . ?
C111 C112 1.375(17) . ?
C112 C50 1.390(15) . ?
C113 N26 1.130(18) . ?
C113 C114 1.41(2) . ?
C115 N30 1.143(19) . ?
C115 C116 1.44(2) . ?
C117 N32 1.11(2) . ?
C117 C118 1.44(2) . ?
C119 N34 1.143(19) . ?
C119 C120 1.37(2) . ?
C121 N31 1.128(17) . ?
C121 C122 1.45(2) . ?
C123 N27 1.13(2) . ?
C123 C124 1.39(2) . ?
C125 N28 1.11(2) . ?
C125 C126 1.44(2) . ?
C127 N29 1.13(2) . ?
C127 C128 1.42(2) . ?
C129 N33 1.152(13) . ?
C129 W1 2.162(11) . ?
C130 O9 1.447(11) . ?
C131 C139 1.41(2) . ?
C132 O11 1.456(12) . ?
C135 N35 1.146(18) . ?
C135 C136 1.51(2) . ?
C137 N11 1.168(13) . ?
C137 W2 2.155(10) . ?
C139 N38 1.097(19) . ?
C141 N18 1.171(12) . ?
C141 W2 2.109(10) . ?
C142 N1 1.197(12) . ?
C142 W1 2.087(10) . ?
N12 Ni4 2.016(8) . ?
N13 C51 1.300(13) . ?
N13 Ni4 2.002(8) . ?
N14 Ni2 1.980(8) . ?
N15 C40 1.277(13) . ?
N15 Ni3 2.003(9) . ?
N16 C37 1.290(13) . ?
N16 Ni3 2.007(8) . ?
N18 Ni3 1.998(9) . ?
O18 Dy2 2.287(8) . ?
C1 O2 1.348(11) . ?
C1 C2 1.388(14) . ?
C1 C6 1.405(13) . ?
C2 C3 1.380(14) . ?
C2 O1 1.401(11) . ?
C3 C4 1.381(15) . ?
C4 C5 1.382(15) . ?
C5 C6 1.406(14) . ?
C6 C7 1.438(14) . ?
C7 N3 1.295(13) 2_666 ?
C8 N3 1.459(13) . ?
C8 C9 1.543(15) . ?
C9 C10 1.511(15) . ?
C9 C11 1.532(14) . ?
C9 C12 1.540(14) . ?
C10 N2 1.480(13) . ?
C13 O6 1.346(11) . ?
C13 C14 1.419(14) . ?
C14 O7 1.391(12) . ?
C15 N4 1.485(13) . ?
C15 C16 1.516(15) . ?
C16 C17 1.513(15) . ?
C17 N5 1.479(13) . ?
C18 N5 1.291(13) . ?
C18 C19 1.429(14) . ?
C19 C24 1.391(14) . ?
C19 C20 1.421(13) . ?
C20 O5 1.345(11) . ?
C20 C21 1.403(14) . ?
C21 C22 1.379(14) . ?
C21 O4 1.381(12) . ?
C22 C23 1.404(15) . ?
C23 C24 1.363(15) . ?
C30 O10 1.351(11) . ?
C30 C31 1.400(14) . ?
C30 C36 1.401(13) . ?
C31 C32 1.360(13) . ?
C31 O11 1.400(11) . ?
C32 C34 1.393(15) . ?
C34 C35 1.365(15) . ?
C35 C36 1.425(14) . ?
C36 C37 1.438(15) . ?
C38 O12 1.338(11) . ?
C38 C41 1.397(14) . ?
C38 C39 1.418(14) . ?
C39 C40 1.453(15) . ?
C41 O16 1.371(12) . ?
C42 C44 1.370(14) . ?
C42 O13 1.385(12) . ?
C42 C43 1.394(14) . ?
C43 O14 1.344(11) . ?
C43 C47 1.407(13) 2_655 ?
C44 C45 1.380(15) . ?
C45 C46 1.400(16) 2_655 ?
C46 C47 1.384(14) . ?
C46 C45 1.400(16) 2_655 ?
C47 C43 1.407(13) 2_655 ?
C48 O17 1.391(12) . ?
C48 C49 1.414(14) . ?
C49 O15 1.338(11) . ?
C49 C50 1.396(14) . ?
C50 C51 1.440(15) 2_655 ?
C51 C50 1.440(15) 2_655 ?
C52 N6 1.145(12) . ?
C52 W2 2.166(10) . ?
C53 N9 1.149(13) . ?
C53 W2 2.163(10) . ?
C55 N8 1.148(13) . ?
C55 W2 2.171(11) . ?
Dy1 O8 2.290(8) . ?
Dy1 O5 2.323(6) . ?
Dy1 O2 2.334(6) . ?
Dy1 O3 2.356(6) . ?
Dy1 O6 2.378(6) . ?
Dy1 O1 2.500(6) . ?
Dy1 O4 2.505(6) . ?
Dy1 O7 2.576(6) . ?
Dy1 O9 2.578(6) . ?
Dy2 O10 2.326(6) . ?
Dy2 O14 2.355(6) . ?
Dy2 O15 2.358(6) . ?
Dy2 O12 2.377(6) . ?
Dy2 O13 2.497(6) . ?
Dy2 O11 2.516(6) . ?
Dy2 O16 2.564(7) . ?
Dy2 O17 2.567(7) . ?
N1 Ni1 1.993(9) . ?
N2 Ni1 1.999(8) . ?
N3 C7 1.295(13) 2_666 ?
N3 Ni1 2.000(8) . ?
N4 Ni2 2.012(9) . ?
N5 Ni2 2.018(9) . ?
N7 Ni4 1.995(9) . ?
Ni1 O2 1.997(7) 2_666 ?
Ni1 O3 2.006(7) 2_666 ?
Ni2 O6 1.995(6) . ?
Ni2 O5 2.036(6) . ?
Ni3 O12 1.985(6) . ?
Ni3 O10 2.025(7) . ?
Ni4 O14 1.995(7) 2_655 ?
Ni4 O15 2.010(6) 2_655 ?
O2 Ni1 1.997(7) 2_666 ?
O3 Ni1 2.006(7) 2_666 ?
O14 Ni4 1.995(7) 2_655 ?
O15 Ni4 2.010(6) 2_655 ?

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
N10 C56 W2 177.6(10) . . ?
N7 C57 W2 178.6(9) . . ?
N12 C58 C47 127.2(9) . . ?
O3 C59 C60 118.2(9) . . ?
O3 C59 C96 123.1(9) . . ?
C60 C59 C96 118.7(9) . . ?
C93 C60 O9 124.6(9) . . ?
C93 C60 C59 122.3(10) . . ?
O9 C60 C59 113.1(8) . . ?
N14 C70 W1 176.6(9) . . ?
N25 C71 W1 179.4(10) . . ?
N20 C72 W1 178.0(10) . . ?
N19 C73 W1 177.4(9) . . ?
N23 C74 W1 176.2(9) . . ?
N4 C75 C76 127.2(10) . . ?
C13 C76 C108 118.5(10) . . ?
C13 C76 C75 125.3(9) . . ?
C108 C76 C75 116.1(10) . . ?
N22 C79 W1 177.0(10) . . ?
N24 C80 W2 179.7(12) . . ?
N13 C82 C83 115.5(9) . . ?
C82 C83 C99 107.8(10) . . ?
C82 C83 C84 112.8(9) . . ?
C99 C83 C84 105.4(9) . . ?
C82 C83 C100 112.4(10) . . ?
C99 C83 C100 109.1(9) . . ?
C84 C83 C100 109.0(10) . . ?
N12 C84 C83 112.3(9) . . ?
N16 C85 C86 115.7(9) . . ?
C87 C86 C105 106.4(9) . . ?
C87 C86 C106 112.9(10) . . ?
C105 C86 C106 108.8(9) . . ?
C87 C86 C85 111.2(9) . . ?
C105 C86 C85 107.1(10) . . ?
C106 C86 C85 110.1(10) . . ?
C86 C87 N15 114.5(9) . . ?
C41 C88 C89 118.3(10) . . ?
C90 C89 C88 119.7(11) . . ?
C89 C90 C39 122.8(11) . . ?
C108 C91 C92 119.8(10) . . ?
C14 C92 C91 118.6(10) . . ?
C60 C93 C94 118.2(10) . . ?
C95 C94 C93 121.5(10) . . ?
C94 C95 C96 120.5(10) . . ?
C59 C96 C95 118.8(10) . . ?
C59 C96 C97 125.0(9) . 2_666 ?
C95 C96 C97 116.2(9) . 2_666 ?
N2 C97 C96 129.6(10) . 2_666 ?
C91 C108 C76 122.3(11) . . ?
C48 C110 C111 120.0(11) . . ?
C112 C111 C110 119.9(11) . . ?
C111 C112 C50 121.1(11) . . ?
N26 C113 C114 178.3(17) . . ?
N30 C115 C116 178.4(19) . . ?
N32 C117 C118 178(2) . . ?
N34 C119 C120 176.4(19) . . ?
N31 C121 C122 177.3(16) . . ?
N27 C123 C124 179(2) . . ?
N28 C125 C126 179(2) . . ?
N29 C127 C128 177.1(18) . . ?
N33 C129 W1 176.7(11) . . ?
N35 C135 C136 177.0(16) . . ?
N11 C137 W2 177.2(9) . . ?
N38 C139 C131 178(2) . . ?
N18 C141 W2 175.1(9) . . ?
N1 C142 W1 176.2(9) . . ?
C58 N12 C84 115.5(9) . . ?
C58 N12 Ni4 126.0(7) . . ?
C84 N12 Ni4 118.4(7) . . ?
C51 N13 C82 114.4(9) . . ?
C51 N13 Ni4 121.6(7) . . ?
C82 N13 Ni4 122.6(7) . . ?
C70 N14 Ni2 160.7(8) . . ?
C40 N15 C87 114.6(9) . . ?
C40 N15 Ni3 125.2(7) . . ?
C87 N15 Ni3 119.7(7) . . ?
C37 N16 C85 117.1(9) . . ?
C37 N16 Ni3 125.3(7) . . ?
C85 N16 Ni3 117.5(7) . . ?
C141 N18 Ni3 155.0(8) . . ?
O2 C1 C2 118.2(9) . . ?
O2 C1 C6 122.9(9) . . ?
C2 C1 C6 118.9(9) . . ?
C3 C2 C1 122.6(9) . . ?
C3 C2 O1 124.1(9) . . ?
C1 C2 O1 113.3(8) . . ?
C2 C3 C4 118.5(10) . . ?
C3 C4 C5 120.5(10) . . ?
C4 C5 C6 121.2(10) . . ?
C1 C6 C5 118.3(9) . . ?
C1 C6 C7 124.2(9) . . ?
C5 C6 C7 117.4(9) . . ?
N3 C7 C6 127.5(9) 2_666 . ?
N3 C8 C9 113.5(8) . . ?
C10 C9 C11 111.3(9) . . ?
C10 C9 C12 107.3(9) . . ?
C11 C9 C12 110.4(9) . . ?
C10 C9 C8 110.7(9) . . ?
C11 C9 C8 110.3(9) . . ?
C12 C9 C8 106.8(9) . . ?
N2 C10 C9 117.0(9) . . ?
O6 C13 C76 124.5(9) . . ?
O6 C13 C14 117.4(9) . . ?
C76 C13 C14 118.0(9) . . ?
C92 C14 O7 124.0(9) . . ?
C92 C14 C13 122.8(10) . . ?
O7 C14 C13 113.2(8) . . ?
N4 C15 C16 115.2(9) . . ?
C17 C16 C15 111.2(8) . . ?
C17 C16 C103 107.0(9) . . ?
C15 C16 C103 108.5(9) . . ?
C17 C16 C102 111.5(10) . . ?
C15 C16 C102 109.8(10) . . ?
C103 C16 C102 108.7(9) . . ?
N5 C17 C16 114.3(9) . . ?
N5 C18 C19 130.0(10) . . ?
C24 C19 C20 118.6(9) . . ?
C24 C19 C18 117.8(9) . . ?
C20 C19 C18 123.5(9) . . ?
O5 C20 C21 118.4(8) . . ?
O5 C20 C19 123.1(9) . . ?
C21 C20 C19 118.5(9) . . ?
C22 C21 O4 123.8(9) . . ?
C22 C21 C20 121.7(9) . . ?
O4 C21 C20 114.4(8) . . ?
C21 C22 C23 119.0(10) . . ?
C24 C23 C22 120.1(10) . . ?
C23 C24 C19 122.1(10) . . ?
O10 C30 C31 118.6(8) . . ?
O10 C30 C36 122.8(9) . . ?
C31 C30 C36 118.5(9) . . ?
C32 C31 O11 124.3(9) . . ?
C32 C31 C30 122.1(9) . . ?
O11 C31 C30 113.6(8) . . ?
C31 C32 C34 120.2(10) . . ?
C35 C34 C32 119.3(10) . . ?
C34 C35 C36 121.6(10) . . ?
C30 C36 C35 118.3(9) . . ?
C30 C36 C37 125.4(9) . . ?
C35 C36 C37 116.4(9) . . ?
N16 C37 C36 127.0(9) . . ?
O12 C38 C41 117.9(9) . . ?
O12 C38 C39 123.5(9) . . ?
C41 C38 C39 118.6(9) . . ?
C38 C39 C90 117.8(10) . . ?
C38 C39 C40 124.4(9) . . ?
C90 C39 C40 117.7(10) . . ?
N15 C40 C39 126.7(10) . . ?
O16 C41 C88 123.4(9) . . ?
O16 C41 C38 113.9(9) . . ?
C88 C41 C38 122.7(10) . . ?
C44 C42 O13 124.3(10) . . ?
C44 C42 C43 121.4(10) . . ?
O13 C42 C43 114.3(8) . . ?
O14 C43 C42 117.6(8) . . ?
O14 C43 C47 123.5(9) . 2_655 ?
C42 C43 C47 118.9(9) . 2_655 ?
C42 C44 C45 120.7(11) . . ?
C44 C45 C46 118.5(10) . 2_655 ?
C47 C46 C45 121.7(10) . 2_655 ?
C46 C47 C43 118.8(10) . 2_655 ?
C46 C47 C58 117.2(9) . . ?
C43 C47 C58 123.9(9) 2_655 . ?
C110 C48 O17 125.3(10) . . ?
C110 C48 C49 121.1(10) . . ?
O17 C48 C49 113.6(8) . . ?
O15 C49 C50 124.0(9) . . ?
O15 C49 C48 117.5(9) . . ?
C50 C49 C48 118.6(9) . . ?
C112 C50 C49 119.3(10) . . ?
C112 C50 C51 115.7(10) . 2_655 ?
C49 C50 C51 124.8(10) . 2_655 ?
N13 C51 C50 129.5(10) . 2_655 ?
N6 C52 W2 178.7(9) . . ?
N9 C53 W2 178.3(10) . . ?
N8 C55 W2 175.9(9) . . ?
O8 Dy1 O5 111.8(3) . . ?
O8 Dy1 O2 111.3(3) . . ?
O5 Dy1 O2 137.0(2) . . ?
O8 Dy1 O3 79.8(2) . . ?
O5 Dy1 O3 125.8(2) . . ?
O2 Dy1 O3 63.1(2) . . ?
O8 Dy1 O6 81.1(2) . . ?
O5 Dy1 O6 64.2(2) . . ?
O2 Dy1 O6 123.0(2) . . ?
O3 Dy1 O6 160.8(2) . . ?
O8 Dy1 O1 144.0(2) . . ?
O5 Dy1 O1 80.4(2) . . ?
O2 Dy1 O1 64.4(2) . . ?
O3 Dy1 O1 121.6(2) . . ?
O6 Dy1 O1 74.1(2) . . ?
O8 Dy1 O4 140.6(2) . . ?
O5 Dy1 O4 65.5(2) . . ?
O2 Dy1 O4 81.5(2) . . ?
O3 Dy1 O4 73.3(2) . . ?
O6 Dy1 O4 124.2(2) . . ?
O1 Dy1 O4 75.4(2) . . ?
O8 Dy1 O7 71.5(2) . . ?
O5 Dy1 O7 125.5(2) . . ?
O2 Dy1 O7 69.2(2) . . ?
O3 Dy1 O7 108.5(2) . . ?
O6 Dy1 O7 62.8(2) . . ?
O1 Dy1 O7 74.1(2) . . ?
O4 Dy1 O7 144.5(2) . . ?
O8 Dy1 O9 70.0(2) . . ?
O5 Dy1 O9 71.9(2) . . ?
O2 Dy1 O9 124.6(2) . . ?
O3 Dy1 O9 62.8(2) . . ?
O6 Dy1 O9 112.1(2) . . ?
O1 Dy1 O9 143.8(2) . . ?
O4 Dy1 O9 72.2(2) . . ?
O7 Dy1 O9 141.5(2) . . ?
O18 Dy2 O10 108.6(3) . . ?
O18 Dy2 O14 114.3(3) . . ?
O10 Dy2 O14 137.0(2) . . ?
O18 Dy2 O15 83.2(2) . . ?
O10 Dy2 O15 127.6(2) . . ?
O14 Dy2 O15 62.5(2) . . ?
O18 Dy2 O12 77.8(2) . . ?
O10 Dy2 O12 64.3(2) . . ?
O14 Dy2 O12 121.8(2) . . ?
O15 Dy2 O12 160.5(2) . . ?
O18 Dy2 O13 141.3(2) . . ?
O10 Dy2 O13 80.5(2) . . ?
O14 Dy2 O13 64.4(2) . . ?
O15 Dy2 O13 121.8(2) . . ?
O12 Dy2 O13 72.7(2) . . ?
O18 Dy2 O11 142.1(2) . . ?
O10 Dy2 O11 65.1(2) . . ?
O14 Dy2 O11 82.4(2) . . ?
O15 Dy2 O11 74.8(2) . . ?
O12 Dy2 O11 123.7(2) . . ?
O13 Dy2 O11 76.3(2) . . ?
O18 Dy2 O16 70.3(2) . . ?
O10 Dy2 O16 125.9(2) . . ?
O14 Dy2 O16 68.9(2) . . ?
O15 Dy2 O16 106.3(2) . . ?
O12 Dy2 O16 62.8(2) . . ?
O13 Dy2 O16 74.2(2) . . ?
O11 Dy2 O16 145.5(2) . . ?
O18 Dy2 O17 70.4(2) . . ?
O10 Dy2 O17 72.9(2) . . ?
O14 Dy2 O17 124.3(2) . . ?
O15 Dy2 O17 63.3(2) . . ?
O12 Dy2 O17 113.5(2) . . ?
O13 Dy2 O17 145.0(2) . . ?
O11 Dy2 O17 72.1(2) . . ?
O16 Dy2 O17 140.3(2) . . ?
C142 N1 Ni1 165.1(8) . . ?
C97 N2 C10 114.9(8) . . ?
C97 N2 Ni1 121.8(7) . . ?
C10 N2 Ni1 122.2(7) . . ?
C7 N3 C8 117.8(8) 2_666 . ?
C7 N3 Ni1 125.9(7) 2_666 . ?
C8 N3 Ni1 116.3(6) . . ?
C75 N4 C15 114.3(9) . . ?
C75 N4 Ni2 123.9(7) . . ?
C15 N4 Ni2 121.1(6) . . ?
C18 N5 C17 117.0(9) . . ?
C18 N5 Ni2 124.2(7) . . ?
C17 N5 Ni2 118.8(6) . . ?
C57 N7 Ni4 168.9(8) . . ?
N1 Ni1 O2 115.5(3) . 2_666 ?
N1 Ni1 N2 91.6(3) . . ?
O2 Ni1 N2 151.3(3) 2_666 . ?
N1 Ni1 N3 94.5(3) . . ?
O2 Ni1 N3 90.9(3) 2_666 . ?
N2 Ni1 N3 96.4(4) . . ?
N1 Ni1 O3 94.1(3) . 2_666 ?
O2 Ni1 O3 75.7(3) 2_666 2_666 ?
N2 Ni1 O3 94.0(3) . 2_666 ?
N3 Ni1 O3 166.2(3) . 2_666 ?
N14 Ni2 O6 98.5(3) . . ?
N14 Ni2 N4 91.0(3) . . ?
O6 Ni2 N4 93.2(3) . . ?
N14 Ni2 N5 97.1(3) . . ?
O6 Ni2 N5 162.6(3) . . ?
N4 Ni2 N5 94.3(3) . . ?
N14 Ni2 O5 109.7(3) . . ?
O6 Ni2 O5 76.6(3) . . ?
N4 Ni2 O5 157.8(3) . . ?
N5 Ni2 O5 90.8(3) . . ?
O12 Ni3 N18 96.8(3) . . ?
O12 Ni3 N15 92.4(3) . . ?
N18 Ni3 N15 91.4(3) . . ?
O12 Ni3 N16 164.5(3) . . ?
N18 Ni3 N16 96.2(3) . . ?
N15 Ni3 N16 95.6(4) . . ?
O12 Ni3 O10 77.2(3) . . ?
N18 Ni3 O10 107.2(3) . . ?
N15 Ni3 O10 159.5(3) . . ?
N16 Ni3 O10 91.0(3) . . ?
N7 Ni4 O14 121.6(3) . 2_655 ?
N7 Ni4 N13 91.5(3) . . ?
O14 Ni4 N13 145.7(3) 2_655 . ?
N7 Ni4 O15 96.2(3) . 2_655 ?
O14 Ni4 O15 75.2(3) 2_655 2_655 ?
N13 Ni4 O15 94.0(3) . 2_655 ?
N7 Ni4 N12 94.4(3) . . ?
O14 Ni4 N12 90.8(3) 2_655 . ?
N13 Ni4 N12 95.6(3) . . ?
O15 Ni4 N12 165.5(3) 2_655 . ?
C2 O1 C104 115.0(8) . . ?
C2 O1 Dy1 116.8(5) . . ?
C104 O1 Dy1 128.1(6) . . ?
C1 O2 Ni1 128.3(6) . 2_666 ?
C1 O2 Dy1 122.3(6) . . ?
Ni1 O2 Dy1 108.6(3) 2_666 . ?
C59 O3 Ni1 126.3(6) . 2_666 ?
C59 O3 Dy1 126.1(6) . . ?
Ni1 O3 Dy1 107.4(3) 2_666 . ?
C21 O4 C78 115.8(7) . . ?
C21 O4 Dy1 117.8(5) . . ?
C78 O4 Dy1 126.4(6) . . ?
C20 O5 Ni2 127.3(6) . . ?
C20 O5 Dy1 123.8(6) . . ?
Ni2 O5 Dy1 108.2(3) . . ?
C13 O6 Ni2 125.6(6) . . ?
C13 O6 Dy1 126.2(6) . . ?
Ni2 O6 Dy1 107.6(3) . . ?
C14 O7 C77 114.3(8) . . ?
C14 O7 Dy1 119.3(6) . . ?
C77 O7 Dy1 126.0(6) . . ?
C60 O9 C130 115.4(7) . . ?
C60 O9 Dy1 118.9(5) . . ?
C130 O9 Dy1 125.4(6) . . ?
C30 O10 Ni3 126.2(6) . . ?
C30 O10 Dy2 124.5(6) . . ?
Ni3 O10 Dy2 108.1(3) . . ?
C31 O11 C132 115.6(7) . . ?
C31 O11 Dy2 118.2(5) . . ?
C132 O11 Dy2 126.1(6) . . ?
C38 O12 Ni3 126.8(6) . . ?
C38 O12 Dy2 124.5(6) . . ?
Ni3 O12 Dy2 107.5(3) . . ?
C42 O13 C107 116.3(7) . . ?
C42 O13 Dy2 115.7(5) . . ?
C107 O13 Dy2 127.6(6) . . ?
C43 O14 Ni4 128.5(6) . 2_655 ?
C43 O14 Dy2 120.7(6) . . ?
Ni4 O14 Dy2 108.8(3) 2_655 . ?
C49 O15 Ni4 125.5(6) . 2_655 ?
C49 O15 Dy2 125.7(6) . . ?
Ni4 O15 Dy2 108.2(3) 2_655 . ?
C41 O16 C101 116.4(8) . . ?
C41 O16 Dy2 118.1(6) . . ?
C101 O16 Dy2 124.7(6) . . ?
C48 O17 C81 115.5(8) . . ?
C48 O17 Dy2 118.3(6) . . ?
C81 O17 Dy2 125.9(6) . . ?
C142 W1 C72 72.0(4) . . ?
C142 W1 C73 79.0(4) . . ?
C72 W1 C73 142.7(4) . . ?
C142 W1 C129 75.8(4) . . ?
C72 W1 C129 76.5(4) . . ?
C73 W1 C129 74.0(4) . . ?
C142 W1 C70 144.1(4) . . ?
C72 W1 C70 141.3(4) . . ?
C73 W1 C70 74.1(4) . . ?
C129 W1 C70 117.6(4) . . ?
C142 W1 C79 113.9(4) . . ?
C72 W1 C79 73.3(4) . . ?
C73 W1 C79 141.8(4) . . ?
C129 W1 C79 142.7(4) . . ?
C70 W1 C79 76.6(4) . . ?
C142 W1 C71 140.7(4) . . ?
C72 W1 C71 78.3(4) . . ?
C73 W1 C71 113.4(4) . . ?
C129 W1 C71 72.8(4) . . ?
C70 W1 C71 73.1(4) . . ?
C79 W1 C71 80.1(4) . . ?
C142 W1 C74 71.6(4) . . ?
C72 W1 C74 114.3(4) . . ?
C73 W1 C74 76.6(4) . . ?
C129 W1 C74 139.4(4) . . ?
C70 W1 C74 79.4(4) . . ?
C79 W1 C74 74.4(4) . . ?
C71 W1 C74 146.1(4) . . ?
C57 W2 C141 145.1(4) . . ?
C57 W2 C137 143.8(4) . . ?
C141 W2 C137 70.4(4) . . ?
C57 W2 C56 79.8(4) . . ?
C141 W2 C56 115.0(4) . . ?
C137 W2 C56 75.1(4) . . ?
C57 W2 C80 106.6(4) . . ?
C141 W2 C80 79.9(4) . . ?
C137 W2 C80 81.2(4) . . ?
C56 W2 C80 144.7(4) . . ?
C57 W2 C53 73.2(4) . . ?
C141 W2 C53 139.8(4) . . ?
C137 W2 C53 75.2(4) . . ?
C56 W2 C53 74.2(4) . . ?
C80 W2 C53 74.8(4) . . ?
C57 W2 C52 78.7(4) . . ?
C141 W2 C52 76.8(4) . . ?
C137 W2 C52 116.6(4) . . ?
C56 W2 C52 72.0(4) . . ?
C80 W2 C52 143.0(4) . . ?
C53 W2 C52 139.1(4) . . ?
C57 W2 C55 76.8(4) . . ?
C141 W2 C55 72.6(4) . . ?
C137 W2 C55 137.7(4) . . ?
C56 W2 C55 141.0(4) . . ?
C80 W2 C55 72.6(4) . . ?
C53 W2 C55 126.3(4) . . ?
C52 W2 C55 73.2(4) . . ?

_refine_diff_density_max         3.105
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.188

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1048761'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-25 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            'C120 H134 N34 Ni4 O20 Tb2 W2'
_chemical_formula_weight         3292.98

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'
Tb Tb -0.1723 4.1537 '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'
W W -0.8490 6.8722 '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                   16.7341(8)
_cell_length_b                   20.6199(8)
_cell_length_c                   20.8979(8)
_cell_angle_alpha                87.881(5)
_cell_angle_beta                 89.214(5)
_cell_angle_gamma                74.309(5)
_cell_volume                     6937.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    117542
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_F_000             3284
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.259
_shelx_estimated_absorpt_T_min   0.562
_shelx_estimated_absorpt_T_max   0.641
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5618
_exptl_absorpt_correction_T_max  0.6406
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            51437
_diffrn_reflns_av_unetI/netI     0.1131
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.417
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             28124
_reflns_number_gt                20696
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 
 Sample is made of fragmented crystals corresponding 
 of stacks of misaligned prism.No orientation matrix 
 for residual fragments could be obtained.

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

__computing_data_collection      'KappaCCD Server Software (Nonius, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+179.1914P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28124
_refine_ls_number_parameters     1633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0976
_refine_ls_wR_factor_ref         0.2307
_refine_ls_wR_factor_gt          0.2174
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
C56 C 0.2297(9) 0.0421(8) 0.2050(7) 0.037(3) Uani 1 1 d . . . . .
C57 C 0.2515(9) -0.0087(7) 0.0842(7) 0.036(3) Uiso 1 1 d . . . . .
C58 C 0.2463(9) -0.2198(8) 0.1770(6) 0.037(3) Uani 1 1 d . . . . .
H58 H 0.2184 -0.2198 0.2169 0.045 Uiso 1 1 calc R U . . .
C59 C 0.2766(9) 0.3573(7) 0.5723(7) 0.034(3) Uani 1 1 d . . . . .
C60 C 0.3298(8) 0.3573(7) 0.6244(6) 0.030(3) Uani 1 1 d . . . . .
C70 C 0.7002(9) 0.3414(7) 0.5966(7) 0.034(3) Uiso 1 1 d . . . . .
C71 C 0.8279(8) 0.3293(7) 0.6685(6) 0.031(3) Uani 1 1 d . . . . .
C72 C 0.8850(8) 0.4330(7) 0.6174(7) 0.035(3) Uani 1 1 d . . . . .
C73 C 0.6373(10) 0.4596(7) 0.6434(6) 0.033(3) Uani 1 1 d . . . . .
C74 C 0.6984(8) 0.4575(7) 0.5240(7) 0.032(3) Uani 1 1 d . . . . .
C75 C 0.7769(9) 0.2015(7) 0.4536(8) 0.041(3) Uani 1 1 d . . . . .
H75 H 0.8326 0.1918 0.4384 0.049 Uiso 1 1 calc R U . . .
C76 C 0.7130(10) 0.2250(7) 0.4056(7) 0.041(3) Uani 1 1 d . . . . .
C77 C 0.4363(9) 0.3341(8) 0.3369(7) 0.040(3) Uani 1 1 d . . . . .
H77A H 0.3795 0.3479 0.3537 0.060 Uiso 1 1 calc R U . . .
H77B H 0.4548 0.3743 0.3253 0.060 Uiso 1 1 calc R U . . .
H77C H 0.4379 0.3073 0.2990 0.060 Uiso 1 1 calc R U . . .
C78 C 0.3042(9) 0.1853(9) 0.5662(7) 0.042(4) Uani 1 1 d . . . . .
H78A H 0.2748 0.2139 0.5308 0.063 Uiso 1 1 calc R U . . .
H78B H 0.3105 0.1378 0.5572 0.063 Uiso 1 1 calc R U . . .
H78C H 0.2725 0.1965 0.6059 0.063 Uiso 1 1 calc R U . . .
C79 C 0.8366(10) 0.3600(8) 0.5379(7) 0.041(4) Uani 1 1 d . . . . .
C80 C 0.1597(9) 0.1568(7) 0.0384(8) 0.041(3) Uani 1 1 d . . . . .
C81 C 0.5169(9) 0.1698(8) 0.1762(7) 0.040(3) Uani 1 1 d . . . . .
H81A H 0.4612 0.1941 0.1614 0.060 Uiso 1 1 calc R U . . .
H81B H 0.5197 0.1220 0.1837 0.060 Uiso 1 1 calc R U . . .
H81C H 0.5288 0.1887 0.2162 0.060 Uiso 1 1 calc R U . . .
C82 C 0.0662(9) -0.0987(8) 0.0448(7) 0.042(4) Uani 1 1 d . . . . .
H82A H 0.0195 -0.1009 0.0171 0.050 Uiso 1 1 calc R U . . .
H82B H 0.0583 -0.0508 0.0549 0.050 Uiso 1 1 calc R U . . .
C83 C 0.0617(9) -0.1382(9) 0.1066(8) 0.047(4) Uani 1 1 d . . . . .
C84 C 0.1292(9) -0.1333(8) 0.1539(8) 0.042(4) Uani 1 1 d . . . . .
H84A H 0.1310 -0.0858 0.1554 0.051 Uiso 1 1 calc R U . . .
H84B H 0.1150 -0.1477 0.1973 0.051 Uiso 1 1 calc R U . . .
C85 C 0.2083(9) 0.3707(8) 0.1594(8) 0.041(4) Uani 1 1 d . . . . .
H85A H 0.1955 0.4026 0.1949 0.049 Uiso 1 1 calc R U . . .
H85B H 0.2033 0.3266 0.1767 0.049 Uiso 1 1 calc R U . . .
C86 C 0.1433(10) 0.3957(7) 0.1078(8) 0.042(4) Uani 1 1 d . . . . .
C87 C 0.1475(9) 0.3428(8) 0.0573(8) 0.045(4) Uani 1 1 d . . . . .
H87A H 0.1389 0.3016 0.0788 0.054 Uiso 1 1 calc R U . . .
H87B H 0.1015 0.3602 0.0266 0.054 Uiso 1 1 calc R U . . .
C88 C 0.3967(10) 0.2277(8) -0.1798(7) 0.041(3) Uani 1 1 d . . . . .
H88 H 0.4349 0.2059 -0.2115 0.049 Uiso 1 1 calc R U . . .
C89 C 0.3146(10) 0.2588(8) -0.1959(8) 0.048(4) Uani 1 1 d . . . . .
H89 H 0.2966 0.2602 -0.2390 0.057 Uiso 1 1 calc R U . . .
C90 C 0.2612(11) 0.2866(9) -0.1500(7) 0.051(4) Uani 1 1 d . . . . .
H90 H 0.2048 0.3056 -0.1615 0.061 Uiso 1 1 calc R U . . .
C91 C 0.6870(11) 0.2520(9) 0.2931(7) 0.049(4) Uani 1 1 d . . . . .
H91 H 0.7071 0.2535 0.2504 0.058 Uiso 1 1 calc R U . . .
C92 C 0.6021(10) 0.2750(8) 0.3056(7) 0.042(3) Uani 1 1 d . . . . .
H92 H 0.5643 0.2929 0.2718 0.050 Uiso 1 1 calc R U . . .
C93 C 0.3018(10) 0.3828(8) 0.6823(7) 0.046(4) Uani 1 1 d . . . . .
H93 H 0.3395 0.3826 0.7159 0.055 Uiso 1 1 calc R U . . .
C94 C 0.2173(10) 0.4089(10) 0.6909(7) 0.054(5) Uani 1 1 d . . . . .
H94 H 0.1975 0.4262 0.7314 0.065 Uiso 1 1 calc R U . . .
C95 C 0.1604(10) 0.4109(10) 0.6430(8) 0.056(5) Uani 1 1 d . . . . .
H95 H 0.1028 0.4300 0.6502 0.067 Uiso 1 1 calc R U . . .
C96 C 0.1899(10) 0.3836(8) 0.5823(7) 0.040(3) Uani 1 1 d . . . . .
C97 C 0.8734(8) 0.6110(7) 0.4649(6) 0.033(3) Uani 1 1 d . . . . .
H97 H 0.9287 0.5912 0.4513 0.039 Uiso 1 1 calc R U . . .
C99 C -0.0223(10) -0.1044(11) 0.1375(10) 0.068(6) Uani 1 1 d . . . . .
H99A H -0.0281 -0.1284 0.1779 0.102 Uiso 1 1 calc R U . . .
H99B H -0.0251 -0.0574 0.1458 0.102 Uiso 1 1 calc R U . . .
H99C H -0.0672 -0.1059 0.1084 0.102 Uiso 1 1 calc R U . . .
C100 C 0.0662(11) -0.2114(9) 0.0941(9) 0.055(4) Uani 1 1 d . . . . .
H10D H 0.0631 -0.2357 0.1348 0.083 Uiso 1 1 calc R U . . .
H10E H 0.0197 -0.2132 0.0668 0.083 Uiso 1 1 calc R U . . .
H10F H 0.1187 -0.2324 0.0725 0.083 Uiso 1 1 calc R U . . .
C101 C 0.5515(10) 0.1468(8) -0.1336(9) 0.051(4) Uani 1 1 d . . . . .
H10A H 0.6065 0.1294 -0.1143 0.077 Uiso 1 1 calc R U . . .
H10B H 0.5244 0.1104 -0.1355 0.077 Uiso 1 1 calc R U . . .
H10C H 0.5572 0.1647 -0.1770 0.077 Uiso 1 1 calc R U . . .
C102 C 0.8402(11) 0.0547(9) 0.5803(10) 0.061(5) Uani 1 1 d . . . . .
H10J H 0.7859 0.0633 0.5598 0.091 Uiso 1 1 calc R U . . .
H10K H 0.8840 0.0358 0.5493 0.091 Uiso 1 1 calc R U . . .
H10L H 0.8434 0.0227 0.6167 0.091 Uiso 1 1 calc R U . . .
C103 C 0.9353(9) 0.1065(8) 0.6353(9) 0.052(4) Uani 1 1 d . . . . .
H10M H 0.9397 0.0720 0.6696 0.078 Uiso 1 1 calc R U . . .
H10N H 0.9790 0.0906 0.6035 0.078 Uiso 1 1 calc R U . . .
H10O H 0.9415 0.1481 0.6534 0.078 Uiso 1 1 calc R U . . .
C104 C 0.5490(11) 0.0978(8) 0.4684(9) 0.052(4) Uani 1 1 d . . . . .
H1G0 H 0.5238 0.0601 0.4713 0.079 Uiso 1 1 calc R U . . .
H1H0 H 0.5716 0.1034 0.5103 0.079 Uiso 1 1 calc R U . . .
H1I0 H 0.5938 0.0886 0.4366 0.079 Uiso 1 1 calc R U . . .
C105 C 0.0576(9) 0.4077(9) 0.1393(9) 0.052(4) Uani 1 1 d . . . . .
H10G H 0.0519 0.3654 0.1591 0.078 Uiso 1 1 calc R U . . .
H10H H 0.0516 0.4415 0.1721 0.078 Uiso 1 1 calc R U . . .
H10I H 0.0146 0.4240 0.1068 0.078 Uiso 1 1 calc R U . . .
C106 C 0.1523(11) 0.4608(8) 0.0772(10) 0.058(5) Uani 1 1 d . . . . .
H10P H 0.1101 0.4766 0.0439 0.087 Uiso 1 1 calc R U . . .
H10Q H 0.1449 0.4949 0.1099 0.087 Uiso 1 1 calc R U . . .
H10R H 0.2076 0.4534 0.0580 0.087 Uiso 1 1 calc R U . . .
C107 C 0.4517(10) 0.3989(8) -0.0385(8) 0.048(4) Uani 1 1 d . . . . .
H1S0 H 0.4754 0.4369 -0.0475 0.072 Uiso 1 1 calc R U . . .
H1T0 H 0.4348 0.3986 0.0065 0.072 Uiso 1 1 calc R U . . .
H1U0 H 0.4033 0.4034 -0.0659 0.072 Uiso 1 1 calc R U . . .
C108 C 0.7397(11) 0.2280(9) 0.3408(7) 0.047(4) Uani 1 1 d . . . . .
H108 H 0.7972 0.2122 0.3313 0.057 Uiso 1 1 calc R U . . .
C110 C 0.6883(11) 0.1201(10) 0.2037(7) 0.052(4) Uani 1 1 d . . . . .
H110 H 0.6500 0.1227 0.2381 0.062 Uiso 1 1 calc R U . . .
C111 C 0.7724(11) 0.0927(10) 0.2140(8) 0.059(5) Uani 1 1 d . . . . .
H111 H 0.7924 0.0765 0.2555 0.070 Uiso 1 1 calc R U . . .
C112 C 0.8265(11) 0.0893(10) 0.1638(8) 0.054(4) Uani 1 1 d . . . . .
H112 H 0.8844 0.0714 0.1710 0.064 Uiso 1 1 calc R U . . .
C113 C 0.0914(12) 0.2074(11) 0.5720(10) 0.064(5) Uani 1 1 d . . . . .
C114 C 0.0494(12) 0.2596(11) 0.6133(12) 0.079(7) Uani 1 1 d . . . . .
H11X H 0.0310 0.2395 0.6521 0.118 Uiso 1 1 calc R U . . .
H11W H 0.0011 0.2891 0.5912 0.118 Uiso 1 1 calc R U . . .
H11Z H 0.0872 0.2861 0.6251 0.118 Uiso 1 1 calc R U . . .
C115 C 0.7162(14) 0.9401(10) 0.5591(10) 0.062(5) Uani 1 1 d . . . . .
C116 C 0.7886(13) 0.8985(9) 0.5968(9) 0.062(5) Uani 1 1 d . . . . .
H11D H 0.7909 0.8507 0.5942 0.093 Uiso 1 1 calc R U . . .
H11E H 0.7823 0.9114 0.6417 0.093 Uiso 1 1 calc R U . . .
H11F H 0.8400 0.9063 0.5793 0.093 Uiso 1 1 calc R U . . .
C117 C 0.7921(16) 0.8652(16) 0.2253(15) 0.095(8) Uani 1 1 d . . . . .
C118 C 0.7513(16) 0.9011(16) 0.1678(15) 0.124(12) Uani 1 1 d . . . . .
H11G H 0.7649 0.9444 0.1622 0.185 Uiso 1 1 calc R U . . .
H11H H 0.6910 0.9092 0.1723 0.185 Uiso 1 1 calc R U . . .
H11I H 0.7706 0.8739 0.1303 0.185 Uiso 1 1 calc R U . . .
C119 C 0.3021(14) 0.5600(9) 0.0554(11) 0.065(5) Uani 1 1 d . . . . .
C120 C 0.2469(15) 0.6043(12) 0.0963(10) 0.080(7) Uani 1 1 d . . . . .
H12X H 0.2472 0.6509 0.0852 0.120 Uiso 1 1 calc R U . . .
H12W H 0.2646 0.5934 0.1409 0.120 Uiso 1 1 calc R U . . .
H12Z H 0.1907 0.5995 0.0913 0.120 Uiso 1 1 calc R U . . .
C121 C 0.7343(12) 0.5159(9) 0.1524(10) 0.059(5) Uani 1 1 d . . . . .
C122 C 0.8055(16) 0.4952(13) 0.1099(13) 0.097(9) Uani 1 1 d . . . . .
H12D H 0.8277 0.4461 0.1130 0.145 Uiso 1 1 calc R U . . .
H12E H 0.8485 0.5164 0.1224 0.145 Uiso 1 1 calc R U . . .
H12F H 0.7884 0.5092 0.0657 0.145 Uiso 1 1 calc R U . . .
C123 C 0.0231(13) 0.3865(13) 0.8247(13) 0.081(7) Uani 1 1 d . . . . .
C124 C -0.0147(18) 0.3591(13) 0.7792(13) 0.103(9) Uani 1 1 d . . . . .
H12A H -0.0264 0.3896 0.7414 0.155 Uiso 1 1 calc R U . . .
H12B H -0.0668 0.3525 0.7965 0.155 Uiso 1 1 calc R U . . .
H12C H 0.0220 0.3156 0.7672 0.155 Uiso 1 1 calc R U . . .
C125 C 0.9072(13) 0.2998(12) 0.0673(12) 0.071(6) Uani 1 1 d . . . . .
C126 C 0.9448(13) 0.2467(11) 0.1101(13) 0.089(8) Uani 1 1 d . . . . .
H12G H 0.9171 0.2107 0.1076 0.134 Uiso 1 1 calc R U . . .
H12H H 0.9402 0.2631 0.1538 0.134 Uiso 1 1 calc R U . . .
H12I H 1.0035 0.2292 0.0987 0.134 Uiso 1 1 calc R U . . .
C127 C 0.2615(14) 0.9962(11) 0.6382(11) 0.065(5) Uani 1 1 d . . . . .
C128 C 0.1850(19) 1.0046(17) 0.6022(16) 0.135(13) Uani 1 1 d . . . . .
H12J H 0.1901 0.9653 0.5759 0.203 Uiso 1 1 calc R U . . .
H12K H 0.1753 1.0454 0.5744 0.203 Uiso 1 1 calc R U . . .
H12L H 0.1384 1.0089 0.6320 0.203 Uiso 1 1 calc R U . . .
C129 C 0.7709(9) 0.4489(7) 0.7111(7) 0.036(3) Uani 1 1 d . . . . .
C130 C 0.4712(9) 0.3393(9) 0.6558(8) 0.048(4) Uani 1 1 d . . . . .
H1AA H 0.4605 0.3876 0.6626 0.072 Uiso 1 1 calc R U . . .
H1BB H 0.5279 0.3216 0.6396 0.072 Uiso 1 1 calc R U . . .
H1CC H 0.4649 0.3158 0.6964 0.072 Uiso 1 1 calc R U . . .
C131 C 1.0112(17) 0.1157(17) 0.2790(13) 0.112(10) Uani 1 1 d . . . . .
H13D H 0.9871 0.0928 0.2472 0.167 Uiso 1 1 calc R U . . .
H13E H 1.0719 0.0993 0.2774 0.167 Uiso 1 1 calc R U . . .
H13F H 0.9942 0.1644 0.2697 0.167 Uiso 1 1 calc R U . . .
C132 C 0.6957(9) 0.3074(8) 0.0686(7) 0.041(4) Uani 1 1 d . . . . .
H1A7 H 0.6963 0.3546 0.0619 0.062 Uiso 1 1 calc R U . . .
H1B7 H 0.7215 0.2816 0.0317 0.062 Uiso 1 1 calc R U . . .
H1C7 H 0.7267 0.2885 0.1075 0.062 Uiso 1 1 calc R U . . .
C135 C 0.7831(13) 0.3758(11) 0.2669(13) 0.072(6) Uani 1 1 d . . . . .
C136 C 0.7413(14) 0.4068(14) 0.3247(12) 0.093(8) Uani 1 1 d . . . . .
H13A H 0.6865 0.3984 0.3285 0.139 Uiso 1 1 calc R U . . .
H13B H 0.7348 0.4555 0.3218 0.139 Uiso 1 1 calc R U . . .
H13C H 0.7746 0.3873 0.3624 0.139 Uiso 1 1 calc R U . . .
C137 C 0.1605(9) 0.1710(7) 0.1713(7) 0.038(3) Uani 1 1 d . . . . .
C139 C 0.9822(14) 0.1015(13) 0.3425(13) 0.082(7) Uani 1 1 d . . . . .
C141 C 0.2840(9) 0.1738(8) 0.1131(7) 0.039(3) Uiso 1 1 d . . . . .
C142 C 0.7547(10) 0.5212(8) 0.6045(8) 0.042(4) Uiso 1 1 d . . . . .
N10 N 0.2256(9) 0.0162(7) 0.2541(7) 0.051(3) Uani 1 1 d . . . . .
N11 N 0.1229(8) 0.2139(6) 0.2030(6) 0.042(3) Uani 1 1 d . . . . .
N12 N 0.2105(7) -0.1749(6) 0.1357(5) 0.032(3) Uani 1 1 d . . . . .
N13 N 0.1441(7) -0.1216(6) 0.0081(6) 0.037(3) Uani 1 1 d . . . . .
N14 N 0.6702(7) 0.2992(6) 0.5868(6) 0.035(3) Uani 1 1 d . . . . .
N15 N 0.2275(7) 0.3245(6) 0.0212(6) 0.034(3) Uani 1 1 d . . . . .
N16 N 0.2953(7) 0.3629(6) 0.1392(6) 0.037(3) Uani 1 1 d . . . . .
N18 N 0.3174(8) 0.2194(6) 0.1077(6) 0.038(3) Uani 1 1 d . . . . .
N19 N 0.5684(8) 0.4827(6) 0.6590(6) 0.040(3) Uani 1 1 d . . . . .
N20 N 0.9514(8) 0.4423(6) 0.6213(7) 0.047(3) Uani 1 1 d . . . . .
N22 N 0.8721(9) 0.3298(7) 0.4967(7) 0.053(4) Uani 1 1 d . . . . .
N23 N 0.6619(8) 0.4816(7) 0.4797(6) 0.047(3) Uani 1 1 d . . . . .
N24 N 0.1211(9) 0.1901(8) -0.0011(8) 0.061(4) Uani 1 1 d . . . . .
N25 N 0.8634(8) 0.2825(6) 0.6970(6) 0.039(3) Uani 1 1 d . . . . .
N26 N 0.1258(12) 0.1649(11) 0.5419(10) 0.084(6) Uani 1 1 d . . . . .
N27 N 0.0521(15) 0.4105(11) 0.8626(15) 0.126(10) Uani 1 1 d . . . . .
N28 N 0.8766(15) 0.3432(12) 0.0332(10) 0.101(7) Uani 1 1 d . . . . .
N29 N 0.3188(12) 0.9863(11) 0.6661(10) 0.087(6) Uani 1 1 d . . . . .
N30 N 0.6642(15) 0.9683(11) 0.5286(12) 0.103(7) Uani 1 1 d . . . . .
N31 N 0.6776(11) 0.5325(10) 0.1825(9) 0.075(5) Uani 1 1 d . . . . .
N32 N 0.8262(19) 0.8385(16) 0.2685(15) 0.146(12) Uani 1 1 d . . . . .
N33 N 0.7757(9) 0.4675(7) 0.7605(7) 0.050(3) Uani 1 1 d . . . . .
N34 N 0.3448(17) 0.5271(11) 0.0204(14) 0.127(10) Uani 1 1 d . . . . .
N35 N 0.8158(13) 0.3533(11) 0.2222(10) 0.085(6) Uani 1 1 d . . . . .
N38 N 0.9547(16) 0.0938(12) 0.3880(14) 0.124(9) Uani 1 1 d . . . . .
O18 O 0.5147(7) 0.1278(6) 0.0217(5) 0.056(3) Uani 1 1 d . . . . .
O19 O 0.5569(6) 0.4221(5) 0.4082(5) 0.043(2) Uani 1 1 d . . . . .
O20 O 0.4184(6) 0.9766(5) 0.8984(5) 0.040(2) Uani 1 1 d . . . . .
C1 C 0.3706(9) 0.2065(7) 0.3848(6) 0.030(3) Uani 1 1 d . . . . .
C2 C 0.4438(8) 0.1534(6) 0.3935(7) 0.030(3) Uani 1 1 d . . . . .
C3 C 0.4679(9) 0.1031(7) 0.3504(7) 0.037(3) Uani 1 1 d . . . . .
H3 H 0.5177 0.0683 0.3571 0.044 Uiso 1 1 calc R U . . .
C4 C 0.4195(10) 0.1031(7) 0.2971(7) 0.041(3) Uani 1 1 d . . . . .
H4 H 0.4355 0.0679 0.2676 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3479(10) 0.1547(8) 0.2872(7) 0.041(3) Uani 1 1 d . . . . .
H5 H 0.3155 0.1549 0.2502 0.049 Uiso 1 1 calc R U . . .
C6 C 0.3220(9) 0.2069(7) 0.3306(6) 0.031(3) Uani 1 1 d . . . . .
C7 C 0.2442(8) 0.2558(7) 0.3187(6) 0.030(3) Uani 1 1 d . . . . .
H7 H 0.2176 0.2521 0.2797 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8743(10) 0.6538(8) 0.6668(7) 0.042(4) Uani 1 1 d . . . . .
H8A H 0.8704 0.6070 0.6741 0.050 Uiso 1 1 calc R U . . .
H8B H 0.8876 0.6700 0.7083 0.050 Uiso 1 1 calc R U . . .
C9 C 0.9457(9) 0.6530(8) 0.6198(7) 0.039(3) Uani 1 1 d . . . . .
C10 C 0.9413(9) 0.6099(8) 0.5626(8) 0.042(4) Uani 1 1 d . . . . .
H10S H 0.9889 0.6100 0.5340 0.051 Uiso 1 1 calc R U . . .
H10T H 0.9486 0.5629 0.5787 0.051 Uiso 1 1 calc R U . . .
C11 C 0.9447(10) 0.7248(8) 0.5997(8) 0.048(4) Uani 1 1 d . . . . .
H11A H 0.9476 0.7504 0.6378 0.072 Uiso 1 1 calc R U . . .
H11B H 0.9925 0.7242 0.5719 0.072 Uiso 1 1 calc R U . . .
H11C H 0.8933 0.7462 0.5764 0.072 Uiso 1 1 calc R U . . .
C12 C 1.0271(9) 0.6170(10) 0.6540(9) 0.054(5) Uani 1 1 d . . . . .
H12M H 1.0264 0.5709 0.6666 0.082 Uiso 1 1 calc R U . . .
H12N H 1.0740 0.6157 0.6251 0.082 Uiso 1 1 calc R U . . .
H12P H 1.0328 0.6415 0.6923 0.082 Uiso 1 1 calc R U . . .
C13 C 0.6280(9) 0.2472(7) 0.4179(7) 0.034(3) Uani 1 1 d . . . . .
C14 C 0.5738(9) 0.2717(6) 0.3667(7) 0.034(3) Uani 1 1 d . . . . .
C15 C 0.8452(9) 0.1735(8) 0.5513(8) 0.041(3) Uani 1 1 d . . . . .
H15A H 0.8527 0.2146 0.5705 0.049 Uiso 1 1 calc R U . . .
H15B H 0.8918 0.1574 0.5210 0.049 Uiso 1 1 calc R U . . .
C16 C 0.8516(9) 0.1203(7) 0.6039(8) 0.040(3) Uani 1 1 d . . . . .
C17 C 0.7864(8) 0.1469(7) 0.6567(8) 0.038(3) Uani 1 1 d . . . . .
H17A H 0.7989 0.1152 0.6943 0.045 Uiso 1 1 calc R U . . .
H17B H 0.7924 0.1909 0.6702 0.045 Uiso 1 1 calc R U . . .
C18 C 0.6574(9) 0.1262(7) 0.6750(7) 0.035(3) Uani 1 1 d . . . . .
H18 H 0.6866 0.1009 0.7105 0.043 Uiso 1 1 calc R U . . .
C19 C 0.5713(8) 0.1266(7) 0.6698(6) 0.030(3) Uani 1 1 d . . . . .
C20 C 0.5162(9) 0.1657(7) 0.6237(6) 0.031(3) Uani 1 1 d . . . . .
C21 C 0.4343(9) 0.1588(7) 0.6219(7) 0.034(3) Uani 1 1 d . . . . .
C22 C 0.4071(9) 0.1181(7) 0.6649(7) 0.035(3) Uani 1 1 d . . . . .
H22 H 0.3515 0.1151 0.6633 0.042 Uiso 1 1 calc R U . . .
C23 C 0.4624(10) 0.0801(7) 0.7121(7) 0.040(3) Uani 1 1 d . . . . .
H23 H 0.4443 0.0518 0.7426 0.047 Uiso 1 1 calc R U . . .
C24 C 0.5417(9) 0.0851(7) 0.7130(7) 0.035(3) Uani 1 1 d . . . . .
H24 H 0.5787 0.0592 0.7443 0.042 Uiso 1 1 calc R U . . .
C30 C 0.4796(9) 0.3453(7) 0.1241(6) 0.032(3) Uani 1 1 d . . . . .
C31 C 0.5639(9) 0.3479(7) 0.1197(7) 0.033(3) Uani 1 1 d . . . . .
C32 C 0.5920(10) 0.3911(7) 0.1552(6) 0.037(3) Uani 1 1 d . . . . .
H32 H 0.6484 0.3920 0.1520 0.044 Uiso 1 1 calc R U . . .
C34 C 0.5377(10) 0.4344(8) 0.1963(7) 0.042(4) Uani 1 1 d . . . . .
H34 H 0.5575 0.4639 0.2218 0.051 Uiso 1 1 calc R U . . .
C35 C 0.4566(10) 0.4342(7) 0.1999(7) 0.038(3) Uani 1 1 d . . . . .
H35 H 0.4198 0.4648 0.2269 0.046 Uiso 1 1 calc R U . . .
C36 C 0.4256(9) 0.3889(7) 0.1639(6) 0.032(3) Uani 1 1 d . . . . .
C37 C 0.3382(8) 0.3922(7) 0.1717(7) 0.034(3) Uani 1 1 d . . . . .
H37 H 0.3097 0.4195 0.2051 0.041 Uiso 1 1 calc R U . . .
C38 C 0.3683(9) 0.2599(7) -0.0688(7) 0.037(3) Uani 1 1 d . . . . .
C39 C 0.2833(9) 0.2896(7) -0.0857(7) 0.038(3) Uani 1 1 d . . . . .
C40 C 0.2192(10) 0.3165(7) -0.0381(7) 0.040(3) Uani 1 1 d . . . . .
H40 H 0.1639 0.3297 -0.0535 0.048 Uiso 1 1 calc R U . . .
C41 C 0.4222(9) 0.2289(7) -0.1175(7) 0.035(3) Uani 1 1 d . . . . .
C42 C 0.5538(9) 0.3333(7) -0.1095(6) 0.035(3) Uani 1 1 d . . . . .
C43 C 0.6261(8) 0.2784(7) -0.1142(7) 0.031(3) Uani 1 1 d . . . . .
C44 C 0.5303(11) 0.3780(8) -0.1604(8) 0.046(4) Uani 1 1 d . . . . .
H44 H 0.4812 0.4139 -0.1571 0.055 Uiso 1 1 calc R U . . .
C45 C 0.5768(10) 0.3720(8) -0.2171(8) 0.045(4) Uani 1 1 d . . . . .
H45 H 0.5605 0.4037 -0.2519 0.054 Uiso 1 1 calc R U . . .
C46 C 0.3521(10) -0.3180(8) 0.2210(7) 0.042(4) Uani 1 1 d . . . . .
H46 H 0.3210 -0.3128 0.2598 0.051 Uiso 1 1 calc R U . . .
C47 C 0.3246(10) -0.2711(7) 0.1706(6) 0.036(3) Uani 1 1 d . . . . .
C48 C 0.6607(9) 0.1434(8) 0.1437(7) 0.040(3) Uani 1 1 d . . . . .
C49 C 0.7131(9) 0.1402(7) 0.0899(7) 0.034(3) Uani 1 1 d . . . . .
C50 C 0.7984(9) 0.1116(7) 0.1020(7) 0.037(3) Uani 1 1 d . . . . .
C51 C 0.1377(10) -0.1059(8) -0.0537(8) 0.045(4) Uani 1 1 d . . . . .
H51 H 0.0825 -0.0882 -0.0688 0.054 Uiso 1 1 calc R U . . .
C52 C 0.3599(10) 0.0463(7) 0.1427(6) 0.035(3) Uani 1 1 d . . . . .
C53 C 0.1135(10) 0.0726(7) 0.1188(7) 0.038(3) Uani 1 1 d . . . . .
C55 C 0.3107(9) 0.0853(7) 0.0267(7) 0.037(3) Uani 1 1 d . . . . .
Tb1 Tb 0.44945(4) 0.27050(3) 0.50172(3) 0.02871(15) Uani 1 1 d . . . . .
Tb2 Tb 0.54323(4) 0.22928(3) 0.01527(3) 0.02900(15) Uani 1 1 d . . . . .
N1 N 0.7453(8) 0.5818(6) 0.5957(6) 0.038(3) Uani 1 1 d . . . . .
N2 N 0.8645(7) 0.6299(5) 0.5234(6) 0.034(3) Uani 1 1 d . . . . .
N3 N 0.7940(7) 0.6957(6) 0.6454(5) 0.031(2) Uani 1 1 d . . . . .
N4 N 0.7677(7) 0.1921(6) 0.5148(5) 0.033(3) Uani 1 1 d . . . . .
N5 N 0.6994(7) 0.1555(6) 0.6381(6) 0.034(3) Uani 1 1 d . . . . .
N6 N 0.4276(7) 0.0220(6) 0.1581(5) 0.034(3) Uani 1 1 d . . . . .
N7 N 0.2608(7) -0.0649(6) 0.0687(6) 0.034(3) Uani 1 1 d . . . . .
N8 N 0.3561(8) 0.0838(7) -0.0159(6) 0.047(3) Uani 1 1 d . . . . .
N9 N 0.0492(8) 0.0605(7) 0.1216(7) 0.047(3) Uani 1 1 d . . . . .
Ni1 Ni 0.75244(11) 0.67138(8) 0.56302(8) 0.0292(4) Uani 1 1 d . . . . .
Ni2 Ni 0.65612(11) 0.21192(9) 0.55853(8) 0.0300(4) Uani 1 1 d . . . . .
Ni3 Ni 0.33730(11) 0.30310(9) 0.06632(9) 0.0319(4) Uani 1 1 d . . . . .
Ni4 Ni 0.25592(10) -0.15697(9) 0.04915(8) 0.0294(4) Uani 1 1 d . . . . .
O1 O 0.4862(6) 0.1594(5) 0.4494(5) 0.037(2) Uani 1 1 d . . . . .
O2 O 0.3519(6) 0.2536(4) 0.4298(4) 0.032(2) Uani 1 1 d . . . . .
O3 O 0.3082(6) 0.3310(5) 0.5187(4) 0.034(2) Uani 1 1 d . . . . .
O4 O 0.3859(6) 0.1965(5) 0.5732(5) 0.037(2) Uani 1 1 d . . . . .
O5 O 0.5384(6) 0.2063(5) 0.5795(5) 0.034(2) Uani 1 1 d . . . . .
O6 O 0.5945(6) 0.2460(4) 0.4778(4) 0.031(2) Uani 1 1 d . . . . .
O7 O 0.4910(6) 0.2940(5) 0.3857(4) 0.033(2) Uani 1 1 d . . . . .
O8 O 0.4611(6) 0.3786(6) 0.4934(5) 0.051(3) Uani 1 1 d . . . . .
O9 O 0.4123(6) 0.3285(5) 0.6094(5) 0.035(2) Uani 1 1 d . . . . .
O10 O 0.4554(6) 0.3014(5) 0.0854(4) 0.031(2) Uani 1 1 d . . . . .
O11 O 0.6111(6) 0.3038(5) 0.0754(4) 0.034(2) Uani 1 1 d . . . . .
O12 O 0.3981(5) 0.2605(5) -0.0106(4) 0.032(2) Uani 1 1 d . . . . .
O13 O 0.5135(6) 0.3363(5) -0.0515(5) 0.036(2) Uani 1 1 d . . . . .
O14 O 0.6452(6) 0.2358(5) -0.0627(4) 0.034(2) Uani 1 1 d . . . . .
O15 O 0.6807(6) 0.1630(5) 0.0345(4) 0.031(2) Uani 1 1 d . . . . .
O16 O 0.5025(6) 0.1992(5) -0.0957(5) 0.033(2) Uani 1 1 d . . . . .
O17 O 0.5767(6) 0.1764(5) 0.1287(4) 0.035(2) Uani 1 1 d . . . . .
W1 W 0.76321(3) 0.41880(3) 0.61296(3) 0.02889(14) Uani 1 1 d . . . . .
W2 W 0.23374(3) 0.09271(3) 0.11239(3) 0.02901(14) Uani 1 1 d . . . . .
H1OA H 0.5904 0.4377 0.4298 0.050 Uiso 1 1 d . U . . .
H2OB H 0.5261 0.4083 0.4358 0.050 Uiso 1 1 d . U . . .
H1OC H 0.4665 0.9796 0.8857 0.050 Uiso 1 1 d . U . . .
H2OD H 0.4015 1.0077 0.9256 0.050 Uiso 1 1 d . U . . .
H1OE H 0.5095 0.0889 0.0362 0.050 Uiso 1 1 d . U . . .
H2OF H 0.4924 0.1336 -0.0154 0.050 Uiso 1 1 d . U . . .
H1OG H 0.4317 0.4136 0.5124 0.050 Uiso 1 1 d . U . . .
H2OH H 0.5111 0.3730 0.5061 0.050 Uiso 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
C56 N10 1.149(19) . ?
C56 W2 2.173(15) . ?
C57 N7 1.183(17) . ?
C57 W2 2.135(14) . ?
C58 N12 1.271(18) . ?
C58 C47 1.45(2) . ?
C59 O3 1.306(16) . ?
C59 C60 1.416(19) . ?
C59 C96 1.42(2) . ?
C60 C93 1.36(2) . ?
C60 O9 1.384(16) . ?
C70 N14 1.142(17) . ?
C70 W1 2.177(14) . ?
C71 N25 1.138(18) . ?
C71 W1 2.172(15) . ?
C72 N20 1.182(18) . ?
C72 W1 2.140(14) . ?
C73 N19 1.168(18) . ?
C73 W1 2.144(16) . ?
C74 N23 1.138(18) . ?
C74 W1 2.179(14) . ?
C75 N4 1.300(19) . ?
C75 C76 1.45(2) . ?
C76 C13 1.40(2) . ?
C76 C108 1.42(2) . ?
C77 O7 1.453(16) . ?
C78 O4 1.457(16) . ?
C79 N22 1.143(19) . ?
C79 W1 2.173(16) . ?
C80 N24 1.14(2) . ?
C80 W2 2.165(17) . ?
C81 O17 1.429(16) . ?
C82 N13 1.475(18) . ?
C82 C83 1.51(2) . ?
C83 C100 1.52(2) . ?
C83 C99 1.53(2) . ?
C83 C84 1.54(2) . ?
C84 N12 1.452(18) . ?
C85 N16 1.479(17) . ?
C85 C86 1.52(2) . ?
C86 C106 1.51(2) . ?
C86 C105 1.53(2) . ?
C86 C87 1.53(2) . ?
C87 N15 1.493(17) . ?
C88 C41 1.38(2) . ?
C88 C89 1.39(2) . ?
C89 C90 1.34(2) . ?
C90 C39 1.40(2) . ?
C91 C108 1.33(2) . ?
C91 C92 1.40(2) . ?
C92 C14 1.36(2) . ?
C93 C94 1.38(2) . ?
C94 C95 1.38(2) . ?
C95 C96 1.44(2) . ?
C96 C97 1.436(19) 2_666 ?
C97 N2 1.292(17) . ?
C97 C96 1.435(19) 2_666 ?
C101 O16 1.425(17) . ?
C102 C16 1.52(2) . ?
C103 C16 1.51(2) . ?
C104 O1 1.459(18) . ?
C107 O13 1.451(17) . ?
C110 C48 1.37(2) . ?
C110 C111 1.38(2) . ?
C111 C112 1.37(2) . ?
C112 C50 1.40(2) . ?
C113 N26 1.12(3) . ?
C113 C114 1.43(3) . ?
C115 N30 1.10(3) . ?
C115 C116 1.50(3) . ?
C117 N32 1.12(3) . ?
C117 C118 1.46(4) . ?
C119 N34 1.12(3) . ?
C119 C120 1.41(3) . ?
C121 N31 1.11(2) . ?
C121 C122 1.45(3) . ?
C123 N27 1.13(3) . ?
C123 C124 1.37(3) . ?
C125 N28 1.13(3) . ?
C125 C126 1.40(3) . ?
C127 N29 1.10(3) . ?
C127 C128 1.46(3) . ?
C129 N33 1.124(18) . ?
C129 W1 2.181(14) . ?
C130 O9 1.456(15) . ?
C131 C139 1.45(3) . ?
C132 O11 1.441(16) . ?
C135 N35 1.13(3) . ?
C135 C136 1.46(3) . ?
C137 N11 1.161(18) . ?
C137 W2 2.159(15) . ?
C139 N38 1.07(3) . ?
C141 N18 1.218(18) . ?
C141 W2 2.066(15) . ?
C142 N1 1.224(19) . ?
C142 W1 2.078(16) . ?
N12 Ni4 2.014(11) . ?
N13 C51 1.318(19) . ?
N13 Ni4 2.006(12) . ?
N14 Ni2 1.988(12) . ?
N15 C40 1.270(18) . ?
N15 Ni3 2.009(12) . ?
N16 C37 1.274(18) . ?
N16 Ni3 1.994(12) . ?
N18 Ni3 2.008(12) . ?
O18 Tb2 2.268(13) . ?
C1 O2 1.347(15) . ?
C1 C6 1.402(18) . ?
C1 C2 1.415(19) . ?
C2 C3 1.370(19) . ?
C2 O1 1.403(16) . ?
C3 C4 1.39(2) . ?
C4 C5 1.38(2) . ?
C5 C6 1.407(19) . ?
C6 C7 1.433(19) . ?
C7 N3 1.291(17) 2_666 ?
C8 N3 1.454(18) . ?
C8 C9 1.53(2) . ?
C9 C11 1.52(2) . ?
C9 C10 1.53(2) . ?
C9 C12 1.53(2) . ?
C10 N2 1.487(18) . ?
C13 O6 1.365(16) . ?
C13 C14 1.40(2) . ?
C14 O7 1.394(17) . ?
C15 N4 1.466(18) . ?
C15 C16 1.51(2) . ?
C16 C17 1.55(2) . ?
C17 N5 1.475(16) . ?
C18 N5 1.280(18) . ?
C18 C19 1.444(19) . ?
C19 C24 1.397(19) . ?
C19 C20 1.412(18) . ?
C20 O5 1.339(16) . ?
C20 C21 1.416(19) . ?
C21 C22 1.364(19) . ?
C21 O4 1.384(16) . ?
C22 C23 1.42(2) . ?
C23 C24 1.36(2) . ?
C30 O10 1.376(15) . ?
C30 C36 1.383(18) . ?
C30 C31 1.428(19) . ?
C31 C32 1.360(19) . ?
C31 O11 1.402(16) . ?
C32 C34 1.40(2) . ?
C34 C35 1.36(2) . ?
C35 C36 1.424(19) . ?
C36 C37 1.453(19) . ?
C38 O12 1.324(17) . ?
C38 C41 1.40(2) . ?
C38 C39 1.432(19) . ?
C39 C40 1.46(2) . ?
C41 O16 1.392(16) . ?
C42 C44 1.37(2) . ?
C42 O13 1.374(16) . ?
C42 C43 1.42(2) . ?
C43 O14 1.350(16) . ?
C43 C47 1.418(19) 2_655 ?
C44 C45 1.40(2) . ?
C45 C46 1.40(2) 2_655 ?
C46 C45 1.40(2) 2_655 ?
C46 C47 1.40(2) . ?
C47 C43 1.418(19) 2_655 ?
C48 C49 1.41(2) . ?
C48 O17 1.419(17) . ?
C49 O15 1.303(16) . ?
C49 C50 1.411(19) . ?
C50 C51 1.44(2) 2_655 ?
C51 C50 1.44(2) 2_655 ?
C52 N6 1.154(18) . ?
C52 W2 2.161(16) . ?
C53 N9 1.169(19) . ?
C53 W2 2.163(16) . ?
C55 N8 1.158(19) . ?
C55 W2 2.177(16) . ?
Tb1 O8 2.289(13) . ?
Tb1 O5 2.335(10) . ?
Tb1 O2 2.337(9) . ?
Tb1 O3 2.383(9) . ?
Tb1 O6 2.392(9) . ?
Tb1 O1 2.495(9) . ?
Tb1 O4 2.521(10) . ?
Tb1 O9 2.576(9) . ?
Tb1 O7 2.578(9) . ?
Tb2 O10 2.332(9) . ?
Tb2 O15 2.367(9) . ?
Tb2 O14 2.369(9) . ?
Tb2 O12 2.402(9) . ?
Tb2 O13 2.502(9) . ?
Tb2 O11 2.521(9) . ?
Tb2 O16 2.571(9) . ?
Tb2 O17 2.576(9) . ?
N1 Ni1 1.980(12) . ?
N2 Ni1 2.018(11) . ?
N3 C7 1.291(17) 2_666 ?
N3 Ni1 1.997(11) . ?
N4 Ni2 2.015(11) . ?
N5 Ni2 2.018(11) . ?
N7 Ni4 1.981(12) . ?
Ni1 O2 2.004(9) 2_666 ?
Ni1 O3 2.007(9) 2_666 ?
Ni2 O6 1.994(9) . ?
Ni2 O5 2.045(9) . ?
Ni3 O12 1.991(9) . ?
Ni3 O10 2.013(9) . ?
Ni4 O14 1.996(9) 2_655 ?
Ni4 O15 2.021(9) 2_655 ?
O2 Ni1 2.004(9) 2_666 ?
O3 Ni1 2.007(9) 2_666 ?
O14 Ni4 1.996(9) 2_655 ?
O15 Ni4 2.021(9) 2_655 ?

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
N10 C56 W2 178.3(14) . . ?
N7 C57 W2 179.5(14) . . ?
N12 C58 C47 127.9(12) . . ?
O3 C59 C60 119.3(13) . . ?
O3 C59 C96 122.9(13) . . ?
C60 C59 C96 117.7(12) . . ?
C93 C60 O9 124.7(12) . . ?
C93 C60 C59 123.1(13) . . ?
O9 C60 C59 112.2(11) . . ?
N14 C70 W1 177.0(13) . . ?
N25 C71 W1 178.5(12) . . ?
N20 C72 W1 177.9(13) . . ?
N19 C73 W1 178.7(12) . . ?
N23 C74 W1 175.3(13) . . ?
N4 C75 C76 128.1(14) . . ?
C13 C76 C108 117.5(14) . . ?
C13 C76 C75 125.4(14) . . ?
C108 C76 C75 117.1(14) . . ?
N22 C79 W1 176.9(15) . . ?
N24 C80 W2 179.3(16) . . ?
N13 C82 C83 115.4(13) . . ?
C82 C83 C100 111.3(14) . . ?
C82 C83 C99 106.4(15) . . ?
C100 C83 C99 109.4(14) . . ?
C82 C83 C84 111.4(12) . . ?
C100 C83 C84 111.2(15) . . ?
C99 C83 C84 106.9(14) . . ?
N12 C84 C83 111.8(12) . . ?
N16 C85 C86 115.8(13) . . ?
C106 C86 C85 110.1(14) . . ?
C106 C86 C105 109.5(13) . . ?
C85 C86 C105 108.0(14) . . ?
C106 C86 C87 111.0(15) . . ?
C85 C86 C87 112.0(13) . . ?
C105 C86 C87 106.1(12) . . ?
N15 C87 C86 113.8(12) . . ?
C41 C88 C89 119.4(14) . . ?
C90 C89 C88 119.1(15) . . ?
C89 C90 C39 124.2(15) . . ?
C108 C91 C92 119.9(14) . . ?
C14 C92 C91 119.5(15) . . ?
C60 C93 C94 118.5(14) . . ?
C95 C94 C93 122.6(14) . . ?
C94 C95 C96 118.8(15) . . ?
C59 C96 C95 119.3(13) . . ?
C59 C96 C97 125.7(13) . 2_666 ?
C95 C96 C97 114.9(14) . 2_666 ?
N2 C97 C96 128.1(13) . 2_666 ?
C91 C108 C76 122.4(16) . . ?
C48 C110 C111 119.5(16) . . ?
C112 C111 C110 119.4(15) . . ?
C111 C112 C50 121.3(15) . . ?
N26 C113 C114 177(3) . . ?
N30 C115 C116 176(2) . . ?
N32 C117 C118 177(3) . . ?
N34 C119 C120 176(3) . . ?
N31 C121 C122 177(2) . . ?
N27 C123 C124 178(3) . . ?
N28 C125 C126 179(3) . . ?
N29 C127 C128 176(3) . . ?
N33 C129 W1 176.4(14) . . ?
N35 C135 C136 178(3) . . ?
N11 C137 W2 178.2(13) . . ?
N38 C139 C131 174(3) . . ?
N18 C141 W2 173.5(13) . . ?
N1 C142 W1 174.9(13) . . ?
C58 N12 C84 115.7(12) . . ?
C58 N12 Ni4 126.2(9) . . ?
C84 N12 Ni4 118.1(9) . . ?
C51 N13 C82 114.8(13) . . ?
C51 N13 Ni4 120.7(11) . . ?
C82 N13 Ni4 123.4(10) . . ?
C70 N14 Ni2 160.7(11) . . ?
C40 N15 C87 113.9(13) . . ?
C40 N15 Ni3 124.2(10) . . ?
C87 N15 Ni3 121.5(10) . . ?
C37 N16 C85 117.3(12) . . ?
C37 N16 Ni3 125.5(9) . . ?
C85 N16 Ni3 117.1(9) . . ?
C141 N18 Ni3 154.4(11) . . ?
O2 C1 C6 124.2(12) . . ?
O2 C1 C2 117.5(11) . . ?
C6 C1 C2 118.3(12) . . ?
C3 C2 O1 126.1(12) . . ?
C3 C2 C1 121.7(13) . . ?
O1 C2 C1 112.2(11) . . ?
C2 C3 C4 120.1(14) . . ?
C5 C4 C3 119.5(13) . . ?
C4 C5 C6 121.5(14) . . ?
C1 C6 C5 118.9(13) . . ?
C1 C6 C7 123.3(12) . . ?
C5 C6 C7 117.7(12) . . ?
N3 C7 C6 127.8(12) 2_666 . ?
N3 C8 C9 114.3(12) . . ?
C11 C9 C10 112.4(13) . . ?
C11 C9 C8 109.8(12) . . ?
C10 C9 C8 110.7(12) . . ?
C11 C9 C12 110.8(13) . . ?
C10 C9 C12 105.4(13) . . ?
C8 C9 C12 107.6(13) . . ?
N2 C10 C9 117.2(12) . . ?
O6 C13 C76 123.2(13) . . ?
O6 C13 C14 118.0(12) . . ?
C76 C13 C14 118.9(13) . . ?
C92 C14 O7 125.1(14) . . ?
C92 C14 C13 121.7(14) . . ?
O7 C14 C13 113.2(12) . . ?
N4 C15 C16 116.2(12) . . ?
C103 C16 C15 109.2(13) . . ?
C103 C16 C102 109.0(13) . . ?
C15 C16 C102 113.2(14) . . ?
C103 C16 C17 106.2(13) . . ?
C15 C16 C17 110.0(12) . . ?
C102 C16 C17 109.0(13) . . ?
N5 C17 C16 115.2(12) . . ?
N5 C18 C19 128.3(13) . . ?
C24 C19 C20 118.6(12) . . ?
C24 C19 C18 117.3(12) . . ?
C20 C19 C18 124.1(12) . . ?
O5 C20 C19 123.4(12) . . ?
O5 C20 C21 118.3(12) . . ?
C19 C20 C21 118.2(12) . . ?
C22 C21 O4 124.0(13) . . ?
C22 C21 C20 121.8(13) . . ?
O4 C21 C20 114.2(12) . . ?
C21 C22 C23 119.6(13) . . ?
C24 C23 C22 118.9(13) . . ?
C23 C24 C19 122.8(13) . . ?
O10 C30 C36 123.4(13) . . ?
O10 C30 C31 117.6(11) . . ?
C36 C30 C31 118.8(12) . . ?
C32 C31 O11 125.4(13) . . ?
C32 C31 C30 121.2(13) . . ?
O11 C31 C30 113.4(11) . . ?
C31 C32 C34 119.9(14) . . ?
C35 C34 C32 120.0(13) . . ?
C34 C35 C36 121.3(14) . . ?
C30 C36 C35 118.8(13) . . ?
C30 C36 C37 124.3(13) . . ?
C35 C36 C37 116.9(12) . . ?
N16 C37 C36 127.7(13) . . ?
O12 C38 C41 119.0(13) . . ?
O12 C38 C39 123.8(13) . . ?
C41 C38 C39 117.2(13) . . ?
C90 C39 C38 117.3(13) . . ?
C90 C39 C40 120.1(14) . . ?
C38 C39 C40 122.4(13) . . ?
N15 C40 C39 128.9(14) . . ?
C88 C41 O16 124.5(13) . . ?
C88 C41 C38 122.6(14) . . ?
O16 C41 C38 112.8(12) . . ?
C44 C42 O13 125.7(14) . . ?
C44 C42 C43 119.8(14) . . ?
O13 C42 C43 114.5(12) . . ?
O14 C43 C47 123.0(12) . 2_655 ?
O14 C43 C42 116.9(12) . . ?
C47 C43 C42 120.2(13) 2_655 . ?
C42 C44 C45 121.7(15) . . ?
C46 C45 C44 117.9(15) 2_655 . ?
C45 C46 C47 123.0(15) 2_655 . ?
C46 C47 C43 117.3(14) . 2_655 ?
C46 C47 C58 119.2(14) . . ?
C43 C47 C58 123.4(13) 2_655 . ?
C110 C48 C49 123.8(14) . . ?
C110 C48 O17 124.1(14) . . ?
C49 C48 O17 112.0(12) . . ?
O15 C49 C48 119.1(13) . . ?
O15 C49 C50 125.6(13) . . ?
C48 C49 C50 115.3(13) . . ?
C112 C50 C49 120.7(14) . . ?
C112 C50 C51 115.5(13) . 2_655 ?
C49 C50 C51 123.7(13) . 2_655 ?
N13 C51 C50 129.9(14) . 2_655 ?
N6 C52 W2 179.0(13) . . ?
N9 C53 W2 178.7(13) . . ?
N8 C55 W2 174.1(13) . . ?
O8 Tb1 O5 111.6(4) . . ?
O8 Tb1 O2 111.5(4) . . ?
O5 Tb1 O2 136.9(3) . . ?
O8 Tb1 O3 80.2(3) . . ?
O5 Tb1 O3 125.5(3) . . ?
O2 Tb1 O3 63.0(3) . . ?
O8 Tb1 O6 81.3(3) . . ?
O5 Tb1 O6 64.2(3) . . ?
O2 Tb1 O6 123.0(3) . . ?
O3 Tb1 O6 161.5(3) . . ?
O8 Tb1 O1 144.1(3) . . ?
O5 Tb1 O1 80.8(3) . . ?
O2 Tb1 O1 64.1(3) . . ?
O3 Tb1 O1 121.1(3) . . ?
O6 Tb1 O1 74.1(3) . . ?
O8 Tb1 O4 140.4(3) . . ?
O5 Tb1 O4 65.1(3) . . ?
O2 Tb1 O4 81.7(3) . . ?
O3 Tb1 O4 73.1(3) . . ?
O6 Tb1 O4 123.8(3) . . ?
O1 Tb1 O4 75.5(3) . . ?
O8 Tb1 O9 69.9(3) . . ?
O5 Tb1 O9 72.1(3) . . ?
O2 Tb1 O9 124.3(3) . . ?
O3 Tb1 O9 62.6(3) . . ?
O6 Tb1 O9 112.5(3) . . ?
O1 Tb1 O9 144.1(3) . . ?
O4 Tb1 O9 72.0(3) . . ?
O8 Tb1 O7 71.6(3) . . ?
O5 Tb1 O7 125.4(3) . . ?
O2 Tb1 O7 69.5(3) . . ?
O3 Tb1 O7 109.0(3) . . ?
O6 Tb1 O7 62.7(3) . . ?
O1 Tb1 O7 74.0(3) . . ?
O4 Tb1 O7 144.8(3) . . ?
O9 Tb1 O7 141.4(3) . . ?
O18 Tb2 O10 108.7(4) . . ?
O18 Tb2 O15 83.0(3) . . ?
O10 Tb2 O15 127.6(3) . . ?
O18 Tb2 O14 113.7(4) . . ?
O10 Tb2 O14 137.5(3) . . ?
O15 Tb2 O14 62.6(3) . . ?
O18 Tb2 O12 78.6(3) . . ?
O10 Tb2 O12 63.8(3) . . ?
O15 Tb2 O12 161.1(3) . . ?
O14 Tb2 O12 121.4(3) . . ?
O18 Tb2 O13 141.5(3) . . ?
O10 Tb2 O13 80.6(3) . . ?
O15 Tb2 O13 121.6(3) . . ?
O14 Tb2 O13 64.4(3) . . ?
O12 Tb2 O13 72.4(3) . . ?
O18 Tb2 O11 142.3(3) . . ?
O10 Tb2 O11 65.3(3) . . ?
O15 Tb2 O11 74.9(3) . . ?
O14 Tb2 O11 82.6(3) . . ?
O12 Tb2 O11 123.1(3) . . ?
O13 Tb2 O11 75.9(3) . . ?
O18 Tb2 O16 70.3(3) . . ?
O10 Tb2 O16 125.4(3) . . ?
O15 Tb2 O16 106.7(3) . . ?
O14 Tb2 O16 68.7(3) . . ?
O12 Tb2 O16 62.7(3) . . ?
O13 Tb2 O16 74.1(3) . . ?
O11 Tb2 O16 145.2(3) . . ?
O18 Tb2 O17 70.4(3) . . ?
O10 Tb2 O17 73.4(3) . . ?
O15 Tb2 O17 62.8(3) . . ?
O14 Tb2 O17 124.0(3) . . ?
O12 Tb2 O17 114.2(3) . . ?
O13 Tb2 O17 145.2(3) . . ?
O11 Tb2 O17 72.4(3) . . ?
O16 Tb2 O17 140.3(3) . . ?
C142 N1 Ni1 164.6(12) . . ?
C97 N2 C10 115.1(12) . . ?
C97 N2 Ni1 122.8(10) . . ?
C10 N2 Ni1 121.6(9) . . ?
C7 N3 C8 117.8(12) 2_666 . ?
C7 N3 Ni1 126.1(9) 2_666 . ?
C8 N3 Ni1 116.1(9) . . ?
C75 N4 C15 114.7(12) . . ?
C75 N4 Ni2 123.3(10) . . ?
C15 N4 Ni2 121.6(9) . . ?
C18 N5 C17 115.8(12) . . ?
C18 N5 Ni2 125.6(10) . . ?
C17 N5 Ni2 118.6(9) . . ?
C57 N7 Ni4 169.6(11) . . ?
N1 Ni1 N3 94.4(5) . . ?
N1 Ni1 O2 115.6(4) . 2_666 ?
N3 Ni1 O2 90.9(4) . 2_666 ?
N1 Ni1 O3 94.9(5) . 2_666 ?
N3 Ni1 O3 166.2(4) . 2_666 ?
O2 Ni1 O3 75.9(4) 2_666 2_666 ?
N1 Ni1 N2 90.9(5) . . ?
N3 Ni1 N2 97.0(5) . . ?
O2 Ni1 N2 151.8(4) 2_666 . ?
O3 Ni1 N2 93.0(4) 2_666 . ?
N14 Ni2 O6 97.9(4) . . ?
N14 Ni2 N4 90.2(5) . . ?
O6 Ni2 N4 93.3(4) . . ?
N14 Ni2 N5 98.1(5) . . ?
O6 Ni2 N5 162.2(4) . . ?
N4 Ni2 N5 94.4(5) . . ?
N14 Ni2 O5 109.6(4) . . ?
O6 Ni2 O5 76.9(4) . . ?
N4 Ni2 O5 158.8(4) . . ?
N5 Ni2 O5 90.5(4) . . ?
O12 Ni3 N16 164.5(4) . . ?
O12 Ni3 N18 97.4(5) . . ?
N16 Ni3 N18 96.2(5) . . ?
O12 Ni3 N15 92.2(4) . . ?
N16 Ni3 N15 94.9(5) . . ?
N18 Ni3 N15 91.3(5) . . ?
O12 Ni3 O10 77.4(4) . . ?
N16 Ni3 O10 91.5(4) . . ?
N18 Ni3 O10 107.0(4) . . ?
N15 Ni3 O10 159.9(4) . . ?
N7 Ni4 O14 120.6(4) . 2_655 ?
N7 Ni4 N13 91.8(5) . . ?
O14 Ni4 N13 146.6(4) 2_655 . ?
N7 Ni4 N12 94.4(5) . . ?
O14 Ni4 N12 90.7(4) 2_655 . ?
N13 Ni4 N12 94.8(5) . . ?
N7 Ni4 O15 96.3(4) . 2_655 ?
O14 Ni4 O15 75.5(4) 2_655 2_655 ?
N13 Ni4 O15 94.5(4) . 2_655 ?
N12 Ni4 O15 165.6(4) . 2_655 ?
C2 O1 C104 113.3(11) . . ?
C2 O1 Tb1 118.2(7) . . ?
C104 O1 Tb1 128.5(9) . . ?
C1 O2 Ni1 127.3(8) . 2_666 ?
C1 O2 Tb1 123.1(8) . . ?
Ni1 O2 Tb1 108.8(4) 2_666 . ?
C59 O3 Ni1 127.2(9) . 2_666 ?
C59 O3 Tb1 125.8(9) . . ?
Ni1 O3 Tb1 106.9(4) 2_666 . ?
C21 O4 C78 115.4(11) . . ?
C21 O4 Tb1 117.9(8) . . ?
C78 O4 Tb1 126.5(8) . . ?
C20 O5 Ni2 127.0(9) . . ?
C20 O5 Tb1 124.4(8) . . ?
Ni2 O5 Tb1 108.0(4) . . ?
C13 O6 Ni2 126.6(9) . . ?
C13 O6 Tb1 125.4(8) . . ?
Ni2 O6 Tb1 107.6(4) . . ?
C14 O7 C77 114.2(11) . . ?
C14 O7 Tb1 119.7(8) . . ?
C77 O7 Tb1 125.9(8) . . ?
C60 O9 C130 114.6(10) . . ?
C60 O9 Tb1 119.3(7) . . ?
C130 O9 Tb1 125.9(8) . . ?
C30 O10 Ni3 125.4(8) . . ?
C30 O10 Tb2 124.6(8) . . ?
Ni3 O10 Tb2 108.8(4) . . ?
C31 O11 C132 114.4(10) . . ?
C31 O11 Tb2 118.9(8) . . ?
C132 O11 Tb2 126.7(8) . . ?
C38 O12 Ni3 127.6(9) . . ?
C38 O12 Tb2 124.5(8) . . ?
Ni3 O12 Tb2 106.9(4) . . ?
C42 O13 C107 116.6(11) . . ?
C42 O13 Tb2 116.4(8) . . ?
C107 O13 Tb2 126.6(8) . . ?
C43 O14 Ni4 128.6(8) . 2_655 ?
C43 O14 Tb2 120.9(8) . . ?
Ni4 O14 Tb2 108.8(4) 2_655 . ?
C49 O15 Ni4 125.1(9) . 2_655 ?
C49 O15 Tb2 126.5(8) . . ?
Ni4 O15 Tb2 108.0(4) 2_655 . ?
C41 O16 C101 115.8(11) . . ?
C41 O16 Tb2 118.5(8) . . ?
C101 O16 Tb2 125.0(8) . . ?
C48 O17 C81 115.8(11) . . ?
C48 O17 Tb2 118.2(8) . . ?
C81 O17 Tb2 125.6(8) . . ?
C142 W1 C72 70.8(6) . . ?
C142 W1 C73 79.9(6) . . ?
C72 W1 C73 143.1(5) . . ?
C142 W1 C71 140.2(6) . . ?
C72 W1 C71 79.1(5) . . ?
C73 W1 C71 113.1(5) . . ?
C142 W1 C79 113.8(6) . . ?
C72 W1 C79 72.9(6) . . ?
C73 W1 C79 141.7(5) . . ?
C71 W1 C79 79.9(5) . . ?
C142 W1 C70 145.1(6) . . ?
C72 W1 C70 141.2(5) . . ?
C73 W1 C70 74.0(5) . . ?
C71 W1 C70 72.8(5) . . ?
C79 W1 C70 76.3(5) . . ?
C142 W1 C74 72.3(6) . . ?
C72 W1 C74 113.6(5) . . ?
C73 W1 C74 76.6(5) . . ?
C71 W1 C74 145.7(5) . . ?
C79 W1 C74 74.5(6) . . ?
C70 W1 C74 79.3(5) . . ?
C142 W1 C129 75.5(6) . . ?
C72 W1 C129 76.7(6) . . ?
C73 W1 C129 74.5(5) . . ?
C71 W1 C129 72.7(5) . . ?
C79 W1 C129 142.2(6) . . ?
C70 W1 C129 117.9(5) . . ?
C74 W1 C129 139.8(5) . . ?
C141 W2 C57 145.6(6) . . ?
C141 W2 C137 69.1(6) . . ?
C57 W2 C137 144.7(5) . . ?
C141 W2 C52 77.5(6) . . ?
C57 W2 C52 78.2(5) . . ?
C137 W2 C52 116.6(5) . . ?
C141 W2 C53 139.1(6) . . ?
C57 W2 C53 73.5(5) . . ?
C137 W2 C53 75.5(5) . . ?
C52 W2 C53 138.6(5) . . ?
C141 W2 C80 80.0(6) . . ?
C57 W2 C80 106.6(6) . . ?
C137 W2 C80 80.9(6) . . ?
C52 W2 C80 143.3(5) . . ?
C53 W2 C80 74.8(5) . . ?
C141 W2 C56 115.1(6) . . ?
C57 W2 C56 79.3(6) . . ?
C137 W2 C56 76.1(6) . . ?
C52 W2 C56 71.8(5) . . ?
C53 W2 C56 73.7(5) . . ?
C80 W2 C56 144.7(5) . . ?
C141 W2 C55 74.3(6) . . ?
C57 W2 C55 75.8(5) . . ?
C137 W2 C55 137.7(5) . . ?
C52 W2 C55 73.6(5) . . ?
C53 W2 C55 125.7(5) . . ?
C80 W2 C55 72.6(5) . . ?
C56 W2 C55 140.7(5) . . ?

_refine_diff_density_max         5.561
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.238

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1048762'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-25 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            'C120 H134 N34 Ni4 O20 W2 Y2'
_chemical_formula_weight         3152.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   16.7100(10)
_cell_length_b                   20.6630(10)
_cell_length_c                   20.8520(10)
_cell_angle_alpha                87.7970(10)
_cell_angle_beta                 89.1850(10)
_cell_angle_gamma                74.1580(10)
_cell_volume                     6921.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    177677
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             3180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.088
_shelx_estimated_absorpt_T_min   0.638
_shelx_estimated_absorpt_T_max   0.708
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6379
_exptl_absorpt_correction_T_max  0.7082
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55372
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.411
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             28125
_reflns_number_gt                22847
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0121P)²+21.0123P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         28125
_refine_ls_number_parameters     1665
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.000
_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
C1 C 0.4357(3) 0.1540(2) 0.3814(2) 0.0230(9) Uani 1 1 d . . . . .
C2 C 0.5189(3) 0.1564(2) 0.3774(2) 0.0223(9) Uani 1 1 d . . . . .
C3 C 0.5730(3) 0.1120(2) 0.3370(2) 0.0248(10) Uani 1 1 d . . . . .
C4 C 0.5424(3) 0.0672(2) 0.3009(2) 0.0302(11) Uani 1 1 d . . . . .
H4 H 0.5790 0.0370 0.2734 0.036 Uiso 1 1 calc R U . . .
C5 C 0.4606(3) 0.0670(2) 0.3053(2) 0.0324(11) Uani 1 1 d . . . . .
H5 H 0.4409 0.0369 0.2807 0.039 Uiso 1 1 calc R U . . .
C6 C 0.4060(3) 0.1110(2) 0.3457(2) 0.0278(10) Uani 1 1 d . . . . .
H6 H 0.3492 0.1111 0.3486 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6605(3) 0.1079(2) 0.3279(2) 0.0283(10) Uani 1 1 d . . . . .
H7 H 0.6886 0.0801 0.2948 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7909(3) 0.1295(2) 0.3392(2) 0.0330(11) Uani 1 1 d . . . . .
H8A H 0.7964 0.1733 0.3219 0.040 Uiso 1 1 calc R U . . .
H8B H 0.8034 0.0976 0.3038 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8552(3) 0.1039(2) 0.3919(3) 0.0344(12) Uani 1 1 d . . . . .
C10 C 0.8471(3) 0.0386(3) 0.4235(3) 0.0469(14) Uani 1 1 d . . . . .
H10A H 0.7920 0.0461 0.4436 0.070 Uiso 1 1 calc R U . . .
H10B H 0.8901 0.0230 0.4563 0.070 Uiso 1 1 calc R U . . .
H10C H 0.8537 0.0044 0.3910 0.070 Uiso 1 1 calc R U . . .
C11 C 0.9416(3) 0.0922(3) 0.3594(3) 0.0439(14) Uani 1 1 d . . . . .
H11A H 0.9482 0.0576 0.3274 0.066 Uiso 1 1 calc R U . . .
H11B H 0.9852 0.0772 0.3920 0.066 Uiso 1 1 calc R U . . .
H11C H 0.9462 0.1342 0.3384 0.066 Uiso 1 1 calc R U . . .
C12 C 0.8504(3) 0.1576(2) 0.4413(2) 0.0313(11) Uani 1 1 d . . . . .
H12A H 0.8975 0.1412 0.4714 0.038 Uiso 1 1 calc R U . . .
H12B H 0.8576 0.1986 0.4187 0.038 Uiso 1 1 calc R U . . .
C13 C 0.7809(3) 0.1843(2) 0.5383(2) 0.0330(11) Uani 1 1 d . . . . .
H13 H 0.8363 0.1715 0.5541 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7157(3) 0.2113(2) 0.5850(2) 0.0308(11) Uani 1 1 d . . . . .
C15 C 0.6315(3) 0.2406(2) 0.5686(2) 0.0236(9) Uani 1 1 d . . . . .
C16 C 0.6016(3) 0.2723(2) 0.6794(2) 0.0346(12) Uani 1 1 d . . . . .
H16 H 0.5625 0.2933 0.7110 0.042 Uiso 1 1 calc R U . . .
C17 C 0.6841(3) 0.2421(3) 0.6956(3) 0.0435(14) Uani 1 1 d . . . . .
H17 H 0.7018 0.2416 0.7388 0.052 Uiso 1 1 calc R U . . .
C18 C 0.7400(3) 0.2132(3) 0.6493(3) 0.0444(14) Uani 1 1 d . . . . .
H18 H 0.7966 0.1939 0.6608 0.053 Uiso 1 1 calc R U . . .
C19 C 0.4478(3) 0.3545(2) 0.6326(2) 0.0354(12) Uani 1 1 d . . . . .
H19D H 0.4246 0.3352 0.6697 0.053 Uiso 1 1 calc R U . . .
H19E H 0.4024 0.3827 0.6064 0.053 Uiso 1 1 calc R U . . .
H19F H 0.4829 0.3819 0.6475 0.053 Uiso 1 1 calc R U . . .
C20 C 0.5487(3) 0.1019(2) 0.5383(2) 0.0385(13) Uani 1 1 d . . . . .
H20A H 0.5966 0.0969 0.5664 0.058 Uiso 1 1 calc R U . . .
H20B H 0.5668 0.1022 0.4934 0.058 Uiso 1 1 calc R U . . .
H20C H 0.5246 0.0642 0.5466 0.058 Uiso 1 1 calc R U . . .
C21 C 0.3030(3) 0.1951(3) 0.4332(2) 0.0340(11) Uani 1 1 d . . . . .
H21A H 0.2721 0.2108 0.3934 0.051 Uiso 1 1 calc R U . . .
H21B H 0.2769 0.2238 0.4682 0.051 Uiso 1 1 calc R U . . .
H21C H 0.3026 0.1485 0.4436 0.051 Uiso 1 1 calc R U . . .
C22 C 0.7116(3) 0.3255(2) 0.3878(2) 0.0252(10) Uani 1 1 d . . . . .
C23 C 0.6395(3) 0.4536(2) 0.3563(2) 0.0233(10) Uani 1 1 d . . . . .
C24 C 0.8401(3) 0.3432(2) 0.4619(2) 0.0292(10) Uani 1 1 d . . . . .
C25 C 0.7708(3) 0.4575(2) 0.2948(2) 0.0283(10) Uani 1 1 d . . . . .
C26 C 0.8402(3) 0.3288(2) 0.3280(2) 0.0247(10) Uani 1 1 d . . . . .
C27 C 0.7492(3) 0.5079(2) 0.4161(2) 0.0257(10) Uani 1 1 d . . . . .
C28 C 0.8703(3) 0.6331(2) 0.3460(2) 0.0310(11) Uani 1 1 d . . . . .
H28A H 0.8849 0.6477 0.3027 0.037 Uiso 1 1 calc R U . . .
H28B H 0.8687 0.5857 0.3441 0.037 Uiso 1 1 calc R U . . .
C29 C 0.9380(3) 0.6376(3) 0.3939(2) 0.0336(11) Uani 1 1 d . . . . .
C30 C 1.0216(3) 0.6035(3) 0.3628(3) 0.0496(15) Uani 1 1 d . . . . .
H30A H 1.0666 0.6015 0.3931 0.074 Uiso 1 1 calc R U . . .
H30B H 1.0294 0.6295 0.3241 0.074 Uiso 1 1 calc R U . . .
H30C H 1.0224 0.5578 0.3514 0.074 Uiso 1 1 calc R U . . .
C31 C 0.9328(3) 0.7109(3) 0.4065(3) 0.0451(14) Uani 1 1 d . . . . .
H31A H 0.8818 0.7309 0.4306 0.068 Uiso 1 1 calc R U . . .
H31B H 0.9322 0.7359 0.3656 0.068 Uiso 1 1 calc R U . . .
H31C H 0.9812 0.7130 0.4316 0.068 Uiso 1 1 calc R U . . .
C32 C 0.9324(3) 0.5976(2) 0.4555(2) 0.0326(11) Uani 1 1 d . . . . .
H32A H 0.9394 0.5501 0.4447 0.039 Uiso 1 1 calc R U . . .
H32B H 0.9795 0.5987 0.4833 0.039 Uiso 1 1 calc R U . . .
C33 C 0.8614(3) 0.6047(2) 0.5536(2) 0.0317(11) Uani 1 1 d . . . . .
H33 H 0.9167 0.5853 0.5682 0.038 Uiso 1 1 calc R U . . .
C34 C 0.7975(3) 0.6122(2) 0.6020(2) 0.0277(10) Uani 1 1 d . . . . .
C35 C 0.8253(3) 0.5896(3) 0.6647(2) 0.0426(13) Uani 1 1 d . . . . .
H35 H 0.8832 0.5716 0.6724 0.051 Uiso 1 1 calc R U . . .
C36 C 0.7707(3) 0.5932(3) 0.7142(3) 0.0475(15) Uani 1 1 d . . . . .
H36 H 0.7903 0.5764 0.7558 0.057 Uiso 1 1 calc R U . . .
C37 C 0.6859(3) 0.6216(3) 0.7042(2) 0.0384(12) Uani 1 1 d . . . . .
H37 H 0.6478 0.6245 0.7389 0.046 Uiso 1 1 calc R U . . .
C38 C 0.6575(3) 0.6451(2) 0.6443(2) 0.0257(10) Uani 1 1 d . . . . .
C39 C 0.7122(3) 0.6399(2) 0.5914(2) 0.0234(9) Uani 1 1 d . . . . .
C40 C 0.6731(3) 0.7716(2) 0.3305(2) 0.0232(9) Uani 1 1 d . . . . .
C41 C 0.7515(3) 0.7216(2) 0.3232(2) 0.0281(10) Uani 1 1 d . . . . .
H41 H 0.7798 0.7234 0.2836 0.034 Uiso 1 1 calc R U . . .
C42 C 0.6471(3) 0.8191(2) 0.2795(2) 0.0327(11) Uani 1 1 d . . . . .
H42 H 0.6791 0.8150 0.2411 0.039 Uiso 1 1 calc R U . . .
C43 C 0.5757(3) 0.8714(2) 0.2845(2) 0.0336(11) Uani 1 1 d . . . . .
H43 H 0.5586 0.9027 0.2494 0.040 Uiso 1 1 calc R U . . .
C44 C 0.5288(3) 0.8786(2) 0.3407(2) 0.0312(11) Uani 1 1 d . . . . .
H44 H 0.4799 0.9148 0.3444 0.037 Uiso 1 1 calc R U . . .
C45 C 0.5537(3) 0.8330(2) 0.3906(2) 0.0238(9) Uani 1 1 d . . . . .
C46 C 0.6247(3) 0.7781(2) 0.3867(2) 0.0217(9) Uani 1 1 d . . . . .
C47 C 0.6280(3) 0.2935(2) 1.1143(2) 0.0214(9) Uani 1 1 d . . . . .
C48 C 0.5546(3) 0.3460(2) 1.1056(2) 0.0230(9) Uani 1 1 d . . . . .
C49 C 0.5305(3) 0.3973(2) 1.1478(2) 0.0282(10) Uani 1 1 d . . . . .
H49 H 0.4811 0.4326 1.1405 0.034 Uiso 1 1 calc R U . . .
C50 C 0.5794(3) 0.3971(2) 1.2012(2) 0.0322(11) Uani 1 1 d . . . . .
H50 H 0.5632 0.4321 1.2308 0.039 Uiso 1 1 calc R U . . .
C51 C 0.4469(3) 0.4002(2) 1.0308(3) 0.0422(14) Uani 1 1 d . . . . .
H51A H 0.4017 0.4082 1.0625 0.063 Uiso 1 1 calc R U . . .
H51B H 0.4253 0.3936 0.9888 0.063 Uiso 1 1 calc R U . . .
H51C H 0.4699 0.4390 1.0279 0.063 Uiso 1 1 calc R U . . .
C52 C 0.5651(3) 0.1649(2) 1.1627(2) 0.0318(11) Uani 1 1 d . . . . .
H52A H 0.5697 0.1928 1.1987 0.048 Uiso 1 1 calc R U . . .
H52B H 0.6202 0.1464 1.1437 0.048 Uiso 1 1 calc R U . . .
H52C H 0.5427 0.1279 1.1782 0.048 Uiso 1 1 calc R U . . .
C53 C 0.4270(3) 0.2271(2) 1.1331(2) 0.0255(10) Uani 1 1 d . . . . .
C54 C 0.3729(3) 0.2519(2) 1.0811(2) 0.0233(9) Uani 1 1 d . . . . .
C55 C 0.2235(3) 0.2981(2) 1.0462(2) 0.0322(11) Uani 1 1 d . . . . .
H55 H 0.1677 0.3079 1.0613 0.039 Uiso 1 1 calc R U . . .
C56 C 0.2874(3) 0.2743(2) 1.0939(2) 0.0293(10) Uani 1 1 d . . . . .
C57 C 0.2597(3) 0.2713(3) 1.1581(2) 0.0404(13) Uani 1 1 d . . . . .
H57 H 0.2019 0.2867 1.1672 0.049 Uiso 1 1 calc R U . . .
C58 C 0.3141(3) 0.2469(3) 1.2073(2) 0.0392(12) Uani 1 1 d . . . . .
H58 H 0.2939 0.2454 1.2500 0.047 Uiso 1 1 calc R U . . .
C59 C 0.3994(3) 0.2240(2) 1.1949(2) 0.0321(11) Uani 1 1 d . . . . .
H59 H 0.4375 0.2067 1.2287 0.039 Uiso 1 1 calc R U . . .
C60 C 0.1552(3) 0.3249(2) 0.9482(2) 0.0299(11) Uani 1 1 d . . . . .
H60A H 0.1078 0.3413 0.9778 0.036 Uiso 1 1 calc R U . . .
H60B H 0.1487 0.2835 0.9292 0.036 Uiso 1 1 calc R U . . .
C61 C 0.1616(3) 0.4429(3) 0.9201(3) 0.0490(15) Uani 1 1 d . . . . .
H61A H 0.1189 0.4601 0.9525 0.073 Uiso 1 1 calc R U . . .
H61B H 0.1564 0.4764 0.8847 0.073 Uiso 1 1 calc R U . . .
H61C H 0.2168 0.4341 0.9394 0.073 Uiso 1 1 calc R U . . .
C62 C 0.0645(3) 0.3923(3) 0.8631(3) 0.0428(13) Uani 1 1 d . . . . .
H62A H 0.0573 0.3507 0.8461 0.064 Uiso 1 1 calc R U . . .
H62B H 0.0604 0.4260 0.8280 0.064 Uiso 1 1 calc R U . . .
H62C H 0.0212 0.4096 0.8951 0.064 Uiso 1 1 calc R U . . .
C63 C 0.2149(3) 0.3514(2) 0.8423(2) 0.0295(11) Uani 1 1 d . . . . .
H63A H 0.2092 0.3074 0.8290 0.035 Uiso 1 1 calc R U . . .
H63B H 0.2025 0.3829 0.8045 0.035 Uiso 1 1 calc R U . . .
C64 C 0.1503(3) 0.3778(2) 0.8946(2) 0.0312(11) Uani 1 1 d . . . . .
C65 C 0.3436(3) 0.3725(2) 0.8250(2) 0.0252(10) Uani 1 1 d . . . . .
H65 H 0.3145 0.3980 0.7895 0.030 Uiso 1 1 calc R U . . .
C66 C 0.4301(3) 0.3720(2) 0.8307(2) 0.0230(9) Uani 1 1 d . . . . .
C67 C 0.4846(3) 0.3332(2) 0.8773(2) 0.0209(9) Uani 1 1 d . . . . .
C68 C 0.5663(3) 0.3398(2) 0.8787(2) 0.0230(9) Uani 1 1 d . . . . .
C69 C 0.5936(3) 0.3813(2) 0.8359(2) 0.0283(10) Uani 1 1 d . . . . .
H69 H 0.6492 0.3844 0.8378 0.034 Uiso 1 1 calc R U . . .
C70 C 0.5389(3) 0.4190(2) 0.7895(2) 0.0297(11) Uani 1 1 d . . . . .
H70 H 0.5573 0.4477 0.7596 0.036 Uiso 1 1 calc R U . . .
C71 C 0.4591(3) 0.4144(2) 0.7875(2) 0.0277(10) Uani 1 1 d . . . . .
H71 H 0.4222 0.4405 0.7561 0.033 Uiso 1 1 calc R U . . .
C72 C 0.8101(3) 0.1165(2) 0.9171(2) 0.0277(10) Uani 1 1 d . . . . .
C73 C 0.8381(3) 0.0902(3) 0.8568(2) 0.0394(13) Uani 1 1 d . . . . .
H73 H 0.8961 0.0720 0.8499 0.047 Uiso 1 1 calc R U . . .
C74 C 0.7842(3) 0.0902(3) 0.8080(2) 0.0467(15) Uani 1 1 d . . . . .
H74 H 0.8049 0.0722 0.7679 0.056 Uiso 1 1 calc R U . . .
C75 C 0.6980(3) 0.1171(3) 0.8174(2) 0.0385(12) Uani 1 1 d . . . . .
H75 H 0.6601 0.1168 0.7840 0.046 Uiso 1 1 calc R U . . .
C76 C 0.1716(3) 0.1702(2) 0.8316(2) 0.0234(9) Uani 1 1 d . . . . .
C77 C 0.3010(3) 0.1568(2) 0.9032(2) 0.0233(9) Uani 1 1 d . . . . .
C78 C 0.1143(3) 0.0673(2) 0.8819(2) 0.0272(10) Uani 1 1 d . . . . .
C79 C 0.2486(3) -0.0235(3) 0.8964(2) 0.0267(10) Uani 1 1 d . . . . .
C80 C 0.2298(3) 0.0501(2) 0.7896(2) 0.0261(10) Uani 1 1 d . . . . .
C81 C 0.3640(3) 0.0392(2) 0.8556(2) 0.0232(9) Uani 1 1 d . . . . .
C82 C 0.1274(3) -0.1112(2) 1.0346(2) 0.0273(10) Uani 1 1 d . . . . .
H82 H 0.0719 -0.0903 1.0475 0.033 Uiso 1 1 calc R U . . .
C83 C 0.0600(3) -0.1091(2) 0.9368(2) 0.0281(10) Uani 1 1 d . . . . .
H83A H 0.0546 -0.0625 0.9203 0.034 Uiso 1 1 calc R U . . .
H83B H 0.0116 -0.1077 0.9651 0.034 Uiso 1 1 calc R U . . .
C84 C 0.0551(3) -0.1523(2) 0.8799(2) 0.0269(10) Uani 1 1 d . . . . .
C084 C 0.6958(3) 0.3128(3) 0.9355(2) 0.0329(11) Uani 1 1 d . . . . .
H08A H 0.7299 0.2967 0.8977 0.049 Uiso 1 1 calc R U . . .
H08B H 0.7226 0.2879 0.9739 0.049 Uiso 1 1 calc R U . . .
H08C H 0.6901 0.3609 0.9397 0.049 Uiso 1 1 calc R U . . .
C85 C -0.0270(3) -0.1167(3) 0.8451(3) 0.0421(13) Uani 1 1 d . . . . .
H85A H -0.0328 -0.1419 0.8073 0.063 Uiso 1 1 calc R U . . .
H85B H -0.0264 -0.0709 0.8315 0.063 Uiso 1 1 calc R U . . .
H85C H -0.0740 -0.1147 0.8743 0.063 Uiso 1 1 calc R U . . .
C86 C 0.0555(3) -0.2237(3) 0.9013(3) 0.0391(12) Uani 1 1 d . . . . .
H86A H 0.1057 -0.2443 0.9264 0.059 Uiso 1 1 calc R U . . .
H86B H 0.0548 -0.2503 0.8635 0.059 Uiso 1 1 calc R U . . .
H86C H 0.0061 -0.2223 0.9277 0.059 Uiso 1 1 calc R U . . .
C87 C 0.1256(3) -0.1533(2) 0.8319(2) 0.0293(11) Uani 1 1 d . . . . .
H87A H 0.1121 -0.1702 0.7907 0.035 Uiso 1 1 calc R U . . .
H87B H 0.1294 -0.1067 0.8237 0.035 Uiso 1 1 calc R U . . .
C88 C 0.2440(3) -0.2447(2) 0.8189(2) 0.0255(10) Uani 1 1 d . . . . .
H88 H 0.2169 -0.2490 0.7802 0.031 Uiso 1 1 calc R U . . .
C89 C 0.3229(3) -0.2939(2) 0.8317(2) 0.0221(9) Uani 1 1 d . . . . .
C90 C 0.3486(3) -0.3462(2) 0.7887(2) 0.0301(11) Uani 1 1 d . . . . .
H90 H 0.3158 -0.3466 0.7520 0.036 Uiso 1 1 calc R U . . .
C92 C 0.3031(3) 0.0418(2) 0.9751(2) 0.0246(10) Uani 1 1 d . . . . .
C95 C 0.5775(3) 0.2712(2) 0.6167(2) 0.0242(10) Uani 1 1 d . . . . .
C96 C 0.1649(3) 0.1388(2) 0.9627(2) 0.0282(10) Uani 1 1 d . . . . .
C98 C 0.8870(3) 0.4267(2) 0.3820(2) 0.0262(10) Uani 1 1 d . . . . .
C99 C 0.6879(3) 0.4148(2) 0.4721(2) 0.0254(10) Uani 1 1 d . . . . .
C100 C 0.0900(4) 0.7072(3) 0.0726(3) 0.0501(15) Uani 1 1 d . . . . .
C101 C 0.0472(4) 0.7597(3) 0.1130(4) 0.0651(19) Uani 1 1 d . . . . .
H10D H 0.0018 0.7909 0.0890 0.098 Uiso 1 1 calc R U . . .
H10E H 0.0860 0.7840 0.1277 0.098 Uiso 1 1 calc R U . . .
H10F H 0.0243 0.7403 0.1502 0.098 Uiso 1 1 calc R U . . .
C103 C 0.7234(3) 0.1434(2) 0.9272(2) 0.0217(9) Uani 1 1 d . . . . .
C104 C 0.6695(3) 0.1437(2) 0.8755(2) 0.0263(10) Uani 1 1 d . . . . .
C105 C 0.5277(3) 0.1617(3) 0.8450(2) 0.0369(12) Uani 1 1 d . . . . .
H10W H 0.5338 0.1850 0.8042 0.055 Uiso 1 1 calc R U . . .
H10X H 0.4711 0.1796 0.8616 0.055 Uiso 1 1 calc R U . . .
H10Y H 0.5382 0.1134 0.8384 0.055 Uiso 1 1 calc R U . . .
C110 C 0.7829(4) 0.8772(3) 0.7682(4) 0.0581(17) Uani 1 1 d . . . . .
C111 C 0.7415(4) 0.9069(4) 0.8260(4) 0.078(2) Uani 1 1 d . . . . .
H11D H 0.7430 0.9540 0.8271 0.117 Uiso 1 1 calc R U . . .
H11E H 0.7700 0.8819 0.8638 0.117 Uiso 1 1 calc R U . . .
H11F H 0.6835 0.9050 0.8261 0.117 Uiso 1 1 calc R U . . .
C120 C 0.2791(4) 0.5616(3) 0.9406(3) 0.0520(15) Uani 1 1 d . . . . .
C121 C 0.2103(4) 0.5997(3) 0.9019(3) 0.0507(15) Uani 1 1 d . . . . .
H12D H 0.2125 0.6465 0.8971 0.076 Uiso 1 1 calc R U . . .
H12E H 0.1579 0.5982 0.9227 0.076 Uiso 1 1 calc R U . . .
H12F H 0.2138 0.5803 0.8594 0.076 Uiso 1 1 calc R U . . .
C122 C 0.4856(3) 0.3291(2) 0.3232(2) 0.0319(11) Uani 1 1 d . . . . .
H12G H 0.4778 0.3052 0.2851 0.048 Uiso 1 1 calc R U . . .
H12H H 0.5416 0.3092 0.3403 0.048 Uiso 1 1 calc R U . . .
H12I H 0.4788 0.3767 0.3115 0.048 Uiso 1 1 calc R U . . .
C130 C 0.9073(4) 0.8012(4) 0.5665(4) 0.0627(19) Uani 1 1 d . . . . .
C131 C 0.9459(4) 0.7478(3) 0.6112(4) 0.073(2) Uani 1 1 d . . . . .
H13A H 0.9029 0.7334 0.6357 0.110 Uiso 1 1 calc R U . . .
H13B H 0.9809 0.7637 0.6407 0.110 Uiso 1 1 calc R U . . .
H13C H 0.9803 0.7097 0.5879 0.110 Uiso 1 1 calc R U . . .
C140 C 0.7395(5) 0.5036(3) 0.8626(4) 0.0622(18) Uani 1 1 d . . . . .
C141 C 0.8147(6) 0.4941(6) 0.8981(5) 0.132(4) Uani 1 1 d . . . . .
H14A H 0.8593 0.4991 0.8689 0.198 Uiso 1 1 calc R U . . .
H14B H 0.8300 0.4489 0.9185 0.198 Uiso 1 1 calc R U . . .
H14C H 0.8062 0.5278 0.9311 0.198 Uiso 1 1 calc R U . . .
C150 C 0.7348(4) 0.0149(3) 0.6520(3) 0.0463(14) Uani 1 1 d . . . . .
C151 C 0.8067(5) -0.0076(4) 0.6107(4) 0.081(2) Uani 1 1 d . . . . .
H15A H 0.8380 0.0263 0.6086 0.122 Uiso 1 1 calc R U . . .
H15B H 0.7884 -0.0139 0.5675 0.122 Uiso 1 1 calc R U . . .
H15C H 0.8424 -0.0503 0.6280 0.122 Uiso 1 1 calc R U . . .
C160 C 0.9771(4) 0.1125(4) 0.6744(4) 0.072(2) Uani 1 1 d . . . . .
C161 C 1.0134(5) 0.1425(4) 0.7217(4) 0.089(3) Uani 1 1 d . . . . .
H16A H 1.0688 0.1444 0.7074 0.134 Uiso 1 1 calc R U . . .
H16B H 1.0180 0.1157 0.7620 0.134 Uiso 1 1 calc R U . . .
H16C H 0.9784 0.1882 0.7285 0.134 Uiso 1 1 calc R U . . .
C180 C 0.2068(5) 0.6345(5) 0.2750(4) 0.090(3) Uani 1 1 d . . . . .
C181 C 0.2503(5) 0.6002(5) 0.3310(5) 0.113(4) Uani 1 1 d . . . . .
H18A H 0.3073 0.6045 0.3305 0.170 Uiso 1 1 calc R U . . .
H18B H 0.2517 0.5525 0.3309 0.170 Uiso 1 1 calc R U . . .
H18C H 0.2215 0.6203 0.3697 0.170 Uiso 1 1 calc R U . . .
C190 C 1.0195(4) 0.3974(4) 0.1589(4) 0.0648(19) Uani 1 1 d . . . . .
C191 C 0.9866(5) 0.3847(5) 0.2204(4) 0.104(3) Uani 1 1 d . . . . .
H19A H 0.9381 0.3675 0.2147 0.156 Uiso 1 1 calc R U . . .
H19B H 0.9700 0.4267 0.2437 0.156 Uiso 1 1 calc R U . . .
H19C H 1.0293 0.3513 0.2449 0.156 Uiso 1 1 calc R U . . .
C200 C 0.6973(5) 0.9397(3) 0.4458(4) 0.0609(18) Uani 1 1 d . . . . .
C201 C 0.7522(5) 0.8954(3) 0.4039(3) 0.067(2) Uani 1 1 d . . . . .
H20D H 0.8097 0.8955 0.4126 0.100 Uiso 1 1 calc R U . . .
H20E H 0.7384 0.9105 0.3592 0.100 Uiso 1 1 calc R U . . .
H20F H 0.7465 0.8497 0.4109 0.100 Uiso 1 1 calc R U . . .
N1 N 0.7039(2) 0.13789(18) 0.36009(18) 0.0266(8) Uani 1 1 d . . . . .
N2 N 0.7724(2) 0.17587(18) 0.47882(19) 0.0275(9) Uani 1 1 d . . . . .
N3 N 0.6820(2) 0.28062(18) 0.39238(18) 0.0240(8) Uani 1 1 d . . . . .
N4 N 0.5718(2) 0.47835(18) 0.34075(17) 0.0240(8) Uani 1 1 d . . . . .
N5 N 0.8780(3) 0.3095(2) 0.5010(2) 0.0458(12) Uani 1 1 d . . . . .
N6 N 0.7745(3) 0.4844(2) 0.2457(2) 0.0407(11) Uani 1 1 d . . . . .
N7 N 0.8772(2) 0.2866(2) 0.2965(2) 0.0328(9) Uani 1 1 d . . . . .
N8 N 0.7393(2) 0.56362(19) 0.43121(18) 0.0256(8) Uani 1 1 d . . . . .
N10 N 0.8542(2) 0.62069(18) 0.49311(18) 0.0254(8) Uani 1 1 d . . . . .
N11 N 0.7878(2) 0.67499(18) 0.36393(17) 0.0248(8) Uani 1 1 d . . . . .
N12 N 0.2330(2) 0.30752(18) 0.98575(18) 0.0259(8) Uani 1 1 d . . . . .
N13 N 0.3015(2) 0.34295(18) 0.86173(18) 0.0252(8) Uani 1 1 d . . . . .
N14 N 0.3305(2) 0.20011(17) 0.91210(17) 0.0226(8) Uani 1 1 d . . . . .
N15 N 0.3401(3) 0.0170(2) 1.0199(2) 0.0361(10) Uani 1 1 d . . . . .
N16 N 0.4317(2) 0.01656(19) 0.84017(18) 0.0277(9) Uani 1 1 d . . . . .
N17 N 0.1380(2) 0.21730(19) 0.80148(19) 0.0304(9) Uani 1 1 d . . . . .
N18 N 0.0493(3) 0.0583(2) 0.8781(2) 0.0379(10) Uani 1 1 d . . . . .
N19 N 0.2237(3) 0.0322(2) 0.7392(2) 0.0403(11) Uani 1 1 d . . . . .
N20 N 0.1364(2) -0.13090(17) 0.97627(18) 0.0229(8) Uani 1 1 d . . . . .
N21 N 0.2067(2) -0.19571(18) 0.85442(17) 0.0232(8) Uani 1 1 d . . . . .
N22 N 0.1235(4) 0.6650(3) 0.0403(3) 0.0780(18) Uani 1 1 d . . . . .
N23 N 0.8146(4) 0.8534(3) 0.7227(3) 0.0781(18) Uani 1 1 d . . . . .
N24 N 0.3336(4) 0.5323(3) 0.9718(4) 0.090(2) Uani 1 1 d . . . . .
N25 N 0.8757(5) 0.8429(4) 0.5315(4) 0.096(2) Uani 1 1 d . . . . .
N26 N 0.6787(3) 0.0322(3) 0.6843(3) 0.0585(14) Uani 1 1 d . . . . .
N27 N 0.6806(4) 0.5118(3) 0.8337(3) 0.0807(19) Uani 1 1 d . . . . .
N28 N 0.1287(3) 0.1705(2) 1.0029(2) 0.0435(11) Uani 1 1 d . . . . .
N30 N 0.9477(5) 0.0902(4) 0.6357(5) 0.120(3) Uani 1 1 d . . . . .
N31 N 0.1731(5) 0.6635(5) 0.2321(4) 0.131(3) Uani 1 1 d . . . . .
N33 N 1.0448(5) 0.4065(4) 0.1107(4) 0.110(3) Uani 1 1 d . . . . .
N34 N 0.6554(5) 0.9731(3) 0.4812(4) 0.116(3) Uani 1 1 d . . . . .
N35 N 0.6431(3) 0.4163(2) 0.51524(19) 0.0333(9) Uani 1 1 d . . . . .
N36 N 0.9504(2) 0.4383(2) 0.3784(2) 0.0378(10) Uani 1 1 d . . . . .
N050 N 0.2557(2) -0.08136(18) 0.90421(18) 0.0256(8) Uani 1 1 d . . . . .
O2 O 0.60077(17) 0.24103(14) 0.51004(14) 0.0230(6) Uani 1 1 d . . . . .
O3 O 0.54266(17) 0.19949(14) 0.41442(14) 0.0230(6) Uani 1 1 d . . . . .
O4 O 0.42475(18) 0.32345(15) 0.37134(14) 0.0255(7) Uani 1 1 d . . . . .
O5 O 0.38778(18) 0.19823(14) 0.42495(14) 0.0249(7) Uani 1 1 d . . . . .
O6 O 0.49708(18) 0.30106(14) 0.59476(14) 0.0245(7) Uani 1 1 d . . . . .
O7 O 0.48696(18) 0.16449(14) 0.55066(14) 0.0254(7) Uani 1 1 d . . . . .
O8 O 0.64382(17) 0.73510(14) 0.43798(13) 0.0210(6) Uani 1 1 d . . . . .
O9 O 0.67936(17) 0.66237(14) 0.53406(13) 0.0211(6) Uani 1 1 d . . . . .
O10 O 0.48777(19) 0.37279(15) 0.47738(15) 0.0314(7) Uani 1 1 d . . . . .
O13 O 0.64699(17) 0.24604(14) 1.07024(13) 0.0207(6) Uani 1 1 d . . . . .
O14 O 0.51181(18) 0.34039(14) 1.05037(14) 0.0265(7) Uani 1 1 d . . . . .
O15 O 0.51008(18) 0.20549(15) 1.11489(14) 0.0248(7) Uani 1 1 d . . . . .
O16 O 0.40665(18) 0.25248(14) 1.02254(14) 0.0234(7) Uani 1 1 d . . . . .
O17 O 0.46246(17) 0.29271(14) 0.92110(13) 0.0211(6) Uani 1 1 d . . . . .
O18 O 0.58638(18) 0.17214(15) 0.89043(14) 0.0255(7) Uani 1 1 d . . . . .
O19 O 0.69005(17) 0.16895(14) 0.98175(13) 0.0212(6) Uani 1 1 d . . . . .
O20 O 0.54015(19) 0.12088(15) 1.00739(15) 0.0310(7) Uani 1 1 d . . . . .
O23 O 0.61440(18) 0.30229(15) 0.92826(14) 0.0253(7) Uani 1 1 d . . . . .
O21 O 0.41842(19) 0.47635(15) 0.39939(16) 0.0316(7) Uani 1 1 d . . . . .
O22 O 0.5571(2) 0.92101(16) 0.90994(16) 0.0331(8) Uani 1 1 d . . . . .
Ni1 Ni 0.74292(3) 0.65636(3) 0.45107(3) 0.02011(12) Uani 1 1 d . . . . .
Ni2 Ni 0.66207(3) 0.19786(3) 0.43355(3) 0.02163(12) Uani 1 1 d . . . . .
Ni3 Ni 0.34471(3) 0.28678(3) 0.94148(3) 0.02021(12) Uani 1 1 d . . . . .
Ni06 Ni 0.24834(3) -0.17125(3) 0.93711(3) 0.01939(12) Uani 1 1 d . . . . .
Y1 Y 0.45698(2) 0.27089(2) 0.48469(2) 0.01877(9) Uani 1 1 d . . . . .
Y2 Y 0.55063(2) 0.22956(2) 0.99842(2) 0.01868(9) Uani 1 1 d . . . . .
W1 W 0.76604(2) 0.40735(2) 0.38718(2) 0.01895(4) Uani 1 1 d . . . . .
W2 W 0.23712(2) 0.08078(2) 0.88681(2) 0.01887(4) Uani 1 1 d . . . . .
H1O H 0.4629 0.4861 0.3827 0.023 Uiso 1 1 d . U . . .
H3O H 0.5820 0.9504 0.9220 0.023 Uiso 1 1 d . U . . .
H20 H 0.4057 0.5190 0.4160 0.023 Uiso 1 1 d . U . . .
H40 H 0.5354 0.9572 0.8788 0.023 Uiso 1 1 d . U . . .
H1OA H 0.4714 0.3878 0.4394 0.050 Uiso 1 1 d . U . . .
H2OB H 0.5338 0.3828 0.4830 0.050 Uiso 1 1 d . U . . .
H1OC H 0.5635 0.0820 0.9927 0.050 Uiso 1 1 d . U . . .
H2OD H 0.5204 0.1137 1.0444 0.050 Uiso 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
C1 C6 1.376(6) . ?
C1 O5 1.394(5) . ?
C1 C2 1.406(6) . ?
C2 O3 1.343(5) . ?
C2 C3 1.397(6) . ?
C3 C4 1.416(6) . ?
C3 C7 1.451(6) . ?
C4 C5 1.369(7) . ?
C5 C6 1.397(6) . ?
C7 N1 1.285(6) . ?
C8 N1 1.478(6) . ?
C8 C9 1.523(7) . ?
C9 C10 1.518(7) . ?
C9 C12 1.528(7) . ?
C9 C11 1.548(6) . ?
C12 N2 1.477(6) . ?
C13 N2 1.276(6) . ?
C13 C14 1.457(7) . ?
C14 C18 1.412(7) . ?
C14 C15 1.413(6) . ?
C15 O2 1.330(5) . ?
C15 C95 1.391(6) . ?
C16 C95 1.376(6) . ?
C16 C17 1.391(7) . ?
C17 C18 1.370(7) . ?
C19 O6 1.439(5) . ?
C20 O7 1.447(5) . ?
C21 O5 1.443(5) . ?
C22 N3 1.164(6) . ?
C22 W1 2.128(5) . ?
C23 N4 1.154(5) . ?
C23 W1 2.165(5) . ?
C24 N5 1.132(6) . ?
C24 W1 2.171(5) . ?
C25 N6 1.155(6) . ?
C25 W1 2.164(5) . ?
C26 N7 1.145(6) . ?
C26 W1 2.169(5) . ?
C27 N8 1.172(6) . ?
C27 W1 2.129(5) . ?
C28 N11 1.466(5) . ?
C28 C29 1.544(7) . ?
C29 C32 1.516(7) . ?
C29 C31 1.527(7) . ?
C29 C30 1.530(7) . ?
C32 N10 1.486(5) . ?
C33 N10 1.290(6) . ?
C33 C34 1.440(7) . ?
C34 C39 1.402(6) . ?
C34 C35 1.413(7) . ?
C35 C36 1.360(7) . ?
C36 C37 1.393(7) . ?
C37 C38 1.365(6) . ?
C38 O4 1.388(5) 2_666 ?
C38 C39 1.411(6) . ?
C39 O9 1.335(5) . ?
C40 C46 1.402(6) . ?
C40 C42 1.408(6) . ?
C40 C41 1.441(6) . ?
C41 N11 1.284(6) . ?
C42 C43 1.379(7) . ?
C43 C44 1.392(7) . ?
C44 C45 1.365(6) . ?
C45 O7 1.388(5) 2_666 ?
C45 C46 1.405(6) . ?
C46 O8 1.348(5) . ?
C47 O13 1.341(5) . ?
C47 C89 1.405(6) 2_657 ?
C47 C48 1.406(6) . ?
C48 C49 1.375(6) . ?
C48 O14 1.389(5) . ?
C49 C50 1.390(6) . ?
C50 C90 1.376(7) 2_657 ?
C51 O14 1.453(5) . ?
C52 O15 1.444(5) . ?
C53 C59 1.366(6) . ?
C53 O15 1.390(5) . ?
C53 C54 1.410(6) . ?
C54 O16 1.338(5) . ?
C54 C56 1.403(6) . ?
C55 N12 1.282(6) . ?
C55 C56 1.442(7) . ?
C56 C57 1.413(7) . ?
C57 C58 1.369(7) . ?
C58 C59 1.398(7) . ?
C60 N12 1.478(6) . ?
C60 C64 1.519(7) . ?
C61 C64 1.525(7) . ?
C62 C64 1.534(6) . ?
C63 N13 1.471(5) . ?
C63 C64 1.530(7) . ?
C65 N13 1.280(6) . ?
C65 C66 1.449(6) . ?
C66 C71 1.404(6) . ?
C66 C67 1.408(6) . ?
C67 O17 1.332(5) . ?
C67 C68 1.409(6) . ?
C68 C69 1.372(6) . ?
C68 O23 1.391(5) . ?
C69 C70 1.399(6) . ?
C70 C71 1.364(6) . ?
C72 C73 1.412(6) . ?
C72 C103 1.418(6) . ?
C72 C82 1.441(6) 2_657 ?
C73 C74 1.368(7) . ?
C74 C75 1.409(7) . ?
C75 C104 1.374(6) . ?
C76 N17 1.149(6) . ?
C76 W2 2.170(5) . ?
C77 N14 1.156(5) . ?
C77 W2 2.166(5) . ?
C78 N18 1.156(6) . ?
C78 W2 2.149(5) . ?
C79 N050 1.174(6) . ?
C79 W2 2.113(5) . ?
C80 N19 1.142(6) . ?
C80 W2 2.162(5) . ?
C81 N16 1.146(5) . ?
C81 W2 2.161(5) . ?
C82 N20 1.291(6) . ?
C82 C72 1.441(6) 2_657 ?
C83 N20 1.482(5) . ?
C83 C84 1.529(6) . ?
C84 C86 1.523(7) . ?
C84 C87 1.531(6) . ?
C84 C85 1.545(6) . ?
C084 O23 1.446(5) . ?
C87 N21 1.471(5) . ?
C88 N21 1.290(6) . ?
C88 C89 1.448(6) . ?
C89 C90 1.402(6) . ?
C89 C47 1.405(6) 2_657 ?
C90 C50 1.376(6) 2_657 ?
C92 N15 1.150(6) . ?
C92 W2 2.171(5) . ?
C95 O6 1.393(5) . ?
C96 N28 1.143(6) . ?
C96 W2 2.168(5) . ?
C98 N36 1.149(6) . ?
C98 W1 2.165(5) . ?
C99 N35 1.158(6) . ?
C99 W1 2.170(5) . ?
C100 N22 1.138(8) . ?
C100 C101 1.424(9) . ?
C103 O19 1.323(5) . ?
C103 C104 1.415(6) . ?
C104 O18 1.388(5) . ?
C105 O18 1.436(5) . ?
C110 N23 1.142(8) . ?
C110 C111 1.452(9) . ?
C120 N24 1.142(8) . ?
C120 C121 1.442(9) . ?
C122 O4 1.443(5) . ?
C130 N25 1.124(9) . ?
C130 C131 1.433(10) . ?
C140 N27 1.131(9) . ?
C140 C141 1.430(11) . ?
C150 N26 1.131(7) . ?
C150 C151 1.449(9) . ?
C160 N30 1.126(9) . ?
C160 C161 1.411(10) . ?
C180 N31 1.125(10) . ?
C180 C181 1.440(11) . ?
C190 N33 1.114(9) . ?
C190 C191 1.430(10) . ?
C200 N34 1.129(9) . ?
C200 C201 1.423(9) . ?
N1 Ni2 2.003(4) . ?
N2 Ni2 2.013(4) . ?
N3 Ni2 1.990(4) . ?
N8 Ni1 1.993(4) . ?
N10 Ni1 2.004(4) . ?
N11 Ni1 2.019(4) . ?
N12 Ni3 2.017(4) . ?
N13 Ni3 2.015(4) . ?
N14 Ni3 1.990(4) . ?
N20 Ni06 2.005(3) . ?
N21 Ni06 2.002(4) . ?
N050 Ni06 1.990(4) . ?
O2 Ni2 1.988(3) . ?
O2 Y1 2.374(3) . ?
O3 Ni2 2.031(3) . ?
O3 Y1 2.308(3) . ?
O4 C38 1.388(5) 2_666 ?
O4 Y1 2.564(3) . ?
O5 Y1 2.505(3) . ?
O6 Y1 2.547(3) . ?
O7 C45 1.388(5) 2_666 ?
O7 Y1 2.482(3) . ?
O8 Ni1 1.993(3) . ?
O8 Y1 2.340(3) 2_666 ?
O9 Ni1 2.008(3) . ?
O9 Y1 2.348(3) 2_666 ?
O10 Y1 2.299(3) . ?
O13 Ni06 2.001(3) 2_657 ?
O13 Y2 2.315(3) . ?
O14 Y2 2.490(3) . ?
O15 Y2 2.579(3) . ?
O16 Ni3 1.997(3) . ?
O16 Y2 2.372(3) . ?
O17 Ni3 2.042(3) . ?
O17 Y2 2.308(3) . ?
O18 Y2 2.572(3) . ?
O19 Ni06 2.002(3) 2_657 ?
O19 Y2 2.353(3) . ?
O20 Y2 2.300(3) . ?
O23 Y2 2.489(3) . ?
Ni2 Y1 3.5151(7) . ?
Ni3 Y2 3.5262(7) . ?
Ni06 O13 2.001(3) 2_657 ?
Ni06 O19 2.002(3) 2_657 ?
Ni06 Y2 3.5125(7) 2_657 ?
Y1 O8 2.340(3) 2_666 ?
Y1 O9 2.348(3) 2_666 ?
Y2 Ni06 3.5125(7) 2_657 ?

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
C6 C1 O5 124.1(4) . . ?
C6 C1 C2 122.1(4) . . ?
O5 C1 C2 113.8(4) . . ?
O3 C2 C3 123.7(4) . . ?
O3 C2 C1 118.0(4) . . ?
C3 C2 C1 118.3(4) . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 C7 124.9(4) . . ?
C4 C3 C7 115.7(4) . . ?
C5 C4 C3 120.7(4) . . ?
C4 C5 C6 120.4(4) . . ?
C1 C6 C5 119.1(4) . . ?
N1 C7 C3 126.8(4) . . ?
N1 C8 C9 114.5(4) . . ?
C10 C9 C8 111.7(4) . . ?
C10 C9 C12 111.4(4) . . ?
C8 C9 C12 111.1(4) . . ?
C10 C9 C11 109.8(4) . . ?
C8 C9 C11 106.6(4) . . ?
C12 C9 C11 106.1(4) . . ?
N2 C12 C9 115.0(4) . . ?
N2 C13 C14 127.6(4) . . ?
C18 C14 C15 118.5(4) . . ?
C18 C14 C13 117.5(4) . . ?
C15 C14 C13 123.7(4) . . ?
O2 C15 C95 118.0(4) . . ?
O2 C15 C14 124.2(4) . . ?
C95 C15 C14 117.8(4) . . ?
C95 C16 C17 118.7(5) . . ?
C18 C17 C16 120.0(5) . . ?
C17 C18 C14 121.7(5) . . ?
N3 C22 W1 175.6(4) . . ?
N4 C23 W1 179.0(4) . . ?
N5 C24 W1 179.2(5) . . ?
N6 C25 W1 179.0(4) . . ?
N7 C26 W1 177.9(4) . . ?
N8 C27 W1 179.0(4) . . ?
N11 C28 C29 112.1(4) . . ?
C32 C29 C31 111.8(4) . . ?
C32 C29 C30 106.7(4) . . ?
C31 C29 C30 110.1(4) . . ?
C32 C29 C28 111.0(4) . . ?
C31 C29 C28 110.7(4) . . ?
C30 C29 C28 106.4(4) . . ?
N10 C32 C29 116.1(4) . . ?
N10 C33 C34 129.1(4) . . ?
C39 C34 C35 119.0(4) . . ?
C39 C34 C33 125.3(4) . . ?
C35 C34 C33 115.7(4) . . ?
C36 C35 C34 121.1(5) . . ?
C35 C36 C37 120.1(5) . . ?
C38 C37 C36 119.9(5) . . ?
C37 C38 O4 125.4(4) . 2_666 ?
C37 C38 C39 121.4(4) . . ?
O4 C38 C39 113.2(4) 2_666 . ?
O9 C39 C34 123.8(4) . . ?
O9 C39 C38 117.8(4) . . ?
C34 C39 C38 118.4(4) . . ?
C46 C40 C42 118.8(4) . . ?
C46 C40 C41 123.8(4) . . ?
C42 C40 C41 117.3(4) . . ?
N11 C41 C40 127.7(4) . . ?
C43 C42 C40 120.9(4) . . ?
C42 C43 C44 120.2(4) . . ?
C45 C44 C43 119.3(4) . . ?
C44 C45 O7 124.7(4) . 2_666 ?
C44 C45 C46 122.1(4) . . ?
O7 C45 C46 113.3(4) 2_666 . ?
O8 C46 C40 123.5(4) . . ?
O8 C46 C45 117.9(4) . . ?
C40 C46 C45 118.6(4) . . ?
O13 C47 C89 123.9(4) . 2_657 ?
O13 C47 C48 117.8(4) . . ?
C89 C47 C48 118.3(4) 2_657 . ?
C49 C48 O14 125.0(4) . . ?
C49 C48 C47 122.0(4) . . ?
O14 C48 C47 113.0(4) . . ?
C48 C49 C50 119.2(4) . . ?
C90 C50 C49 120.2(4) 2_657 . ?
C59 C53 O15 124.0(4) . . ?
C59 C53 C54 122.8(4) . . ?
O15 C53 C54 113.2(4) . . ?
O16 C54 C56 124.2(4) . . ?
O16 C54 C53 117.8(4) . . ?
C56 C54 C53 117.9(4) . . ?
N12 C55 C56 127.8(4) . . ?
C54 C56 C57 118.7(4) . . ?
C54 C56 C55 125.1(4) . . ?
C57 C56 C55 116.2(4) . . ?
C58 C57 C56 121.7(5) . . ?
C57 C58 C59 120.0(5) . . ?
C53 C59 C58 118.9(5) . . ?
N12 C60 C64 115.1(4) . . ?
N13 C63 C64 114.4(4) . . ?
C60 C64 C61 111.5(4) . . ?
C60 C64 C63 110.9(4) . . ?
C61 C64 C63 110.2(4) . . ?
C60 C64 C62 108.2(4) . . ?
C61 C64 C62 109.1(4) . . ?
C63 C64 C62 106.8(4) . . ?
N13 C65 C66 128.2(4) . . ?
C71 C66 C67 119.4(4) . . ?
C71 C66 C65 116.7(4) . . ?
C67 C66 C65 124.0(4) . . ?
O17 C67 C66 123.7(4) . . ?
O17 C67 C68 118.5(4) . . ?
C66 C67 C68 117.7(4) . . ?
C69 C68 O23 124.1(4) . . ?
C69 C68 C67 122.1(4) . . ?
O23 C68 C67 113.7(4) . . ?
C68 C69 C70 119.5(4) . . ?
C71 C70 C69 119.8(4) . . ?
C70 C71 C66 121.6(4) . . ?
C73 C72 C103 118.8(4) . . ?
C73 C72 C82 116.7(4) . 2_657 ?
C103 C72 C82 124.5(4) . 2_657 ?
C74 C73 C72 121.9(5) . . ?
C73 C74 C75 119.8(5) . . ?
C104 C75 C74 119.2(5) . . ?
N17 C76 W2 178.7(4) . . ?
N14 C77 W2 176.0(4) . . ?
N18 C78 W2 177.9(4) . . ?
N050 C79 W2 177.4(4) . . ?
N19 C80 W2 177.0(4) . . ?
N16 C81 W2 178.6(4) . . ?
N20 C82 C72 129.0(4) . 2_657 ?
N20 C83 C84 116.5(4) . . ?
C86 C84 C83 111.9(4) . . ?
C86 C84 C87 110.6(4) . . ?
C83 C84 C87 111.1(4) . . ?
C86 C84 C85 110.3(4) . . ?
C83 C84 C85 106.0(4) . . ?
C87 C84 C85 106.7(4) . . ?
N21 C87 C84 112.9(4) . . ?
N21 C88 C89 127.0(4) . . ?
C90 C89 C47 119.1(4) . 2_657 ?
C90 C89 C88 117.2(4) . . ?
C47 C89 C88 123.7(4) 2_657 . ?
C50 C90 C89 121.2(4) 2_657 . ?
N15 C92 W2 175.3(4) . . ?
C16 C95 C15 123.3(4) . . ?
C16 C95 O6 123.7(4) . . ?
C15 C95 O6 113.0(4) . . ?
N28 C96 W2 177.8(4) . . ?
N36 C98 W1 178.5(4) . . ?
N35 C99 W1 175.4(4) . . ?
N22 C100 C101 179.4(8) . . ?
O19 C103 C104 118.0(4) . . ?
O19 C103 C72 124.1(4) . . ?
C104 C103 C72 117.9(4) . . ?
C75 C104 O18 124.7(4) . . ?
C75 C104 C103 122.3(4) . . ?
O18 C104 C103 112.9(4) . . ?
N23 C110 C111 179.0(8) . . ?
N24 C120 C121 179.0(8) . . ?
N25 C130 C131 178.7(9) . . ?
N27 C140 C141 178.6(8) . . ?
N26 C150 C151 179.7(8) . . ?
N30 C160 C161 178.0(9) . . ?
N31 C180 C181 177.4(12) . . ?
N33 C190 C191 179.0(10) . . ?
N34 C200 C201 177.1(8) . . ?
C7 N1 C8 116.9(4) . . ?
C7 N1 Ni2 125.5(3) . . ?
C8 N1 Ni2 117.6(3) . . ?
C13 N2 C12 115.3(4) . . ?
C13 N2 Ni2 124.2(3) . . ?
C12 N2 Ni2 119.9(3) . . ?
C22 N3 Ni2 155.2(3) . . ?
C27 N8 Ni1 169.8(3) . . ?
C33 N10 C32 114.6(4) . . ?
C33 N10 Ni1 122.0(3) . . ?
C32 N10 Ni1 122.3(3) . . ?
C41 N11 C28 116.6(4) . . ?
C41 N11 Ni1 125.9(3) . . ?
C28 N11 Ni1 117.4(3) . . ?
C55 N12 C60 114.9(4) . . ?
C55 N12 Ni3 123.7(3) . . ?
C60 N12 Ni3 120.8(3) . . ?
C65 N13 C63 115.6(4) . . ?
C65 N13 Ni3 125.5(3) . . ?
C63 N13 Ni3 119.0(3) . . ?
C77 N14 Ni3 160.8(3) . . ?
C82 N20 C83 114.7(4) . . ?
C82 N20 Ni06 122.4(3) . . ?
C83 N20 Ni06 121.8(3) . . ?
C88 N21 C87 116.9(4) . . ?
C88 N21 Ni06 126.5(3) . . ?
C87 N21 Ni06 116.7(3) . . ?
C79 N050 Ni06 164.9(4) . . ?
C15 O2 Ni2 126.6(3) . . ?
C15 O2 Y1 125.0(3) . . ?
Ni2 O2 Y1 107.05(12) . . ?
C2 O3 Ni2 125.6(3) . . ?
C2 O3 Y1 125.0(3) . . ?
Ni2 O3 Y1 108.03(12) . . ?
C38 O4 C122 115.7(3) 2_666 . ?
C38 O4 Y1 118.4(2) 2_666 . ?
C122 O4 Y1 125.6(3) . . ?
C1 O5 C21 115.8(3) . . ?
C1 O5 Y1 117.9(2) . . ?
C21 O5 Y1 126.2(3) . . ?
C95 O6 C19 115.8(3) . . ?
C95 O6 Y1 118.4(2) . . ?
C19 O6 Y1 125.1(3) . . ?
C45 O7 C20 115.7(3) 2_666 . ?
C45 O7 Y1 116.6(2) 2_666 . ?
C20 O7 Y1 127.4(3) . . ?
C46 O8 Ni1 128.5(3) . . ?
C46 O8 Y1 120.9(2) . 2_666 ?
Ni1 O8 Y1 109.11(12) . 2_666 ?
C39 O9 Ni1 125.4(3) . . ?
C39 O9 Y1 125.8(3) . 2_666 ?
Ni1 O9 Y1 108.25(12) . 2_666 ?
C47 O13 Ni06 127.8(3) . 2_657 ?
C47 O13 Y2 122.8(2) . . ?
Ni06 O13 Y2 108.72(12) 2_657 . ?
C48 O14 C51 115.4(3) . . ?
C48 O14 Y2 117.2(2) . . ?
C51 O14 Y2 127.4(3) . . ?
C53 O15 C52 115.1(3) . . ?
C53 O15 Y2 118.9(2) . . ?
C52 O15 Y2 125.7(2) . . ?
C54 O16 Ni3 125.8(3) . . ?
C54 O16 Y2 126.2(3) . . ?
Ni3 O16 Y2 107.31(12) . . ?
C67 O17 Ni3 127.0(3) . . ?
C67 O17 Y2 124.2(2) . . ?
Ni3 O17 Y2 108.14(12) . . ?
C104 O18 C105 115.4(3) . . ?
C104 O18 Y2 118.5(2) . . ?
C105 O18 Y2 126.0(3) . . ?
C103 O19 Ni06 126.0(3) . 2_657 ?
C103 O19 Y2 126.5(2) . . ?
Ni06 O19 Y2 107.27(12) 2_657 . ?
C68 O23 C084 115.5(3) . . ?
C68 O23 Y2 117.8(2) . . ?
C084 O23 Y2 126.7(2) . . ?
O8 Ni1 N8 121.26(13) . . ?
O8 Ni1 N10 146.31(13) . . ?
N8 Ni1 N10 91.26(15) . . ?
O8 Ni1 O9 75.07(11) . . ?
N8 Ni1 O9 96.62(14) . . ?
N10 Ni1 O9 94.05(13) . . ?
O8 Ni1 N11 90.54(13) . . ?
N8 Ni1 N11 94.34(15) . . ?
N10 Ni1 N11 95.85(15) . . ?
O9 Ni1 N11 165.04(13) . . ?
O2 Ni2 N3 97.06(13) . . ?
O2 Ni2 N1 164.48(14) . . ?
N3 Ni2 N1 96.25(15) . . ?
O2 Ni2 N2 92.56(14) . . ?
N3 Ni2 N2 91.38(15) . . ?
N1 Ni2 N2 95.04(16) . . ?
O2 Ni2 O3 77.24(12) . . ?
N3 Ni2 O3 107.22(13) . . ?
N1 Ni2 O3 91.22(14) . . ?
N2 Ni2 O3 159.61(14) . . ?
O2 Ni2 Y1 40.21(8) . . ?
N3 Ni2 Y1 97.15(10) . . ?
N1 Ni2 Y1 129.78(11) . . ?
N2 Ni2 Y1 132.63(11) . . ?
O3 Ni2 Y1 38.63(8) . . ?
N14 Ni3 O16 98.49(13) . . ?
N14 Ni3 N13 97.33(15) . . ?
O16 Ni3 N13 162.29(13) . . ?
N14 Ni3 N12 90.94(15) . . ?
O16 Ni3 N12 93.17(14) . . ?
N13 Ni3 N12 94.49(15) . . ?
N14 Ni3 O17 109.92(13) . . ?
O16 Ni3 O17 76.59(11) . . ?
N13 Ni3 O17 90.56(13) . . ?
N12 Ni3 O17 157.74(14) . . ?
N14 Ni3 Y2 99.18(10) . . ?
O16 Ni3 Y2 39.96(8) . . ?
N13 Ni3 Y2 128.98(11) . . ?
N12 Ni3 Y2 132.89(11) . . ?
O17 Ni3 Y2 38.47(8) . . ?
N050 Ni06 O13 115.31(13) . 2_657 ?
N050 Ni06 N21 94.58(15) . . ?
O13 Ni06 N21 90.80(13) 2_657 . ?
N050 Ni06 O19 94.46(14) . 2_657 ?
O13 Ni06 O19 75.62(11) 2_657 2_657 ?
N21 Ni06 O19 165.96(13) . 2_657 ?
N050 Ni06 N20 91.53(14) . . ?
O13 Ni06 N20 151.53(13) 2_657 . ?
N21 Ni06 N20 96.59(15) . . ?
O19 Ni06 N20 93.88(13) 2_657 . ?
N050 Ni06 Y2 98.11(10) . 2_657 ?
O13 Ni06 Y2 38.62(8) 2_657 2_657 ?
N21 Ni06 Y2 127.95(11) . 2_657 ?
O19 Ni06 Y2 39.76(8) 2_657 2_657 ?
N20 Ni06 Y2 133.00(11) . 2_657 ?
O10 Y1 O3 108.17(11) . . ?
O10 Y1 O8 114.28(11) . 2_666 ?
O3 Y1 O8 137.45(10) . 2_666 ?
O10 Y1 O9 83.22(10) . 2_666 ?
O3 Y1 O9 127.28(10) . 2_666 ?
O8 Y1 O9 62.66(10) 2_666 2_666 ?
O10 Y1 O2 77.35(10) . . ?
O3 Y1 O2 64.80(10) . . ?
O8 Y1 O2 121.65(10) 2_666 . ?
O9 Y1 O2 159.97(10) 2_666 . ?
O10 Y1 O7 141.53(11) . . ?
O3 Y1 O7 80.48(10) . . ?
O8 Y1 O7 64.77(9) 2_666 . ?
O9 Y1 O7 122.09(10) 2_666 . ?
O2 Y1 O7 72.88(10) . . ?
O10 Y1 O5 142.02(10) . . ?
O3 Y1 O5 65.28(9) . . ?
O8 Y1 O5 82.45(10) 2_666 . ?
O9 Y1 O5 74.69(10) 2_666 . ?
O2 Y1 O5 124.32(10) . . ?
O7 Y1 O5 76.13(10) . . ?
O10 Y1 O6 70.26(10) . . ?
O3 Y1 O6 126.32(10) . . ?
O8 Y1 O6 68.61(10) 2_666 . ?
O9 Y1 O6 106.18(9) 2_666 . ?
O2 Y1 O6 62.66(9) . . ?
O7 Y1 O6 74.65(10) . . ?
O5 Y1 O6 145.42(10) . . ?
O10 Y1 O4 70.18(10) . . ?
O3 Y1 O4 72.63(10) . . ?
O8 Y1 O4 124.48(9) 2_666 . ?
O9 Y1 O4 63.26(9) 2_666 . ?
O2 Y1 O4 113.40(10) . . ?
O7 Y1 O4 144.89(10) . . ?
O5 Y1 O4 72.35(10) . . ?
O6 Y1 O4 139.99(10) . . ?
O10 Y1 Ni2 87.06(8) . . ?
O3 Y1 Ni2 33.34(7) . . ?
O8 Y1 Ni2 144.70(7) 2_666 . ?
O9 Y1 Ni2 151.61(7) 2_666 . ?
O2 Y1 Ni2 32.74(7) . . ?
O7 Y1 Ni2 80.94(7) . . ?
O5 Y1 Ni2 97.87(7) . . ?
O6 Y1 Ni2 95.39(6) . . ?
O4 Y1 Ni2 88.35(7) . . ?
O20 Y2 O17 111.95(11) . . ?
O20 Y2 O13 110.86(11) . . ?
O17 Y2 O13 137.19(10) . . ?
O20 Y2 O19 79.36(10) . . ?
O17 Y2 O19 125.57(10) . . ?
O13 Y2 O19 63.43(10) . . ?
O20 Y2 O16 80.97(10) . . ?
O17 Y2 O16 64.65(10) . . ?
O13 Y2 O16 122.88(10) . . ?
O19 Y2 O16 160.22(10) . . ?
O20 Y2 O23 140.49(11) . . ?
O17 Y2 O23 65.70(9) . . ?
O13 Y2 O23 81.49(10) . . ?
O19 Y2 O23 73.15(10) . . ?
O16 Y2 O23 124.89(10) . . ?
O20 Y2 O14 143.78(11) . . ?
O17 Y2 O14 80.49(10) . . ?
O13 Y2 O14 64.72(9) . . ?
O19 Y2 O14 122.20(10) . . ?
O16 Y2 O14 74.04(10) . . ?
O23 Y2 O14 75.71(10) . . ?
O20 Y2 O18 70.01(10) . . ?
O17 Y2 O18 71.48(10) . . ?
O13 Y2 O18 125.02(9) . . ?
O19 Y2 O18 62.99(9) . . ?
O16 Y2 O18 111.72(10) . . ?
O23 Y2 O18 72.38(10) . . ?
O14 Y2 O18 143.96(10) . . ?
O20 Y2 O15 71.23(10) . . ?
O17 Y2 O15 125.90(10) . . ?
O13 Y2 O15 68.99(10) . . ?
O19 Y2 O15 108.36(9) . . ?
O16 Y2 O15 62.74(9) . . ?
O23 Y2 O15 144.51(10) . . ?
O14 Y2 O15 74.12(10) . . ?
O18 Y2 O15 141.22(10) . . ?
O20 Y2 Ni06 88.24(8) . 2_657 ?
O17 Y2 Ni06 149.29(7) . 2_657 ?
O13 Y2 Ni06 32.66(7) . 2_657 ?
O19 Y2 Ni06 32.97(7) . 2_657 ?
O16 Y2 Ni06 144.36(7) . 2_657 ?
O23 Y2 Ni06 83.92(7) . 2_657 ?
O14 Y2 Ni06 96.97(7) . 2_657 ?
O18 Y2 Ni06 95.90(7) . 2_657 ?
O15 Y2 Ni06 81.62(7) . 2_657 ?
O20 Y2 Ni3 90.83(8) . . ?
O17 Y2 Ni3 33.39(7) . . ?
O13 Y2 Ni3 145.96(7) . . ?
O19 Y2 Ni3 149.36(7) . . ?
O16 Y2 Ni3 32.73(7) . . ?
O23 Y2 Ni3 98.53(7) . . ?
O14 Y2 Ni3 82.17(7) . . ?
O18 Y2 Ni3 86.37(7) . . ?
O15 Y2 Ni3 95.46(7) . . ?
Ni06 Y2 Ni3 177.084(18) 2_657 . ?
C22 W1 C27 144.42(16) . . ?
C22 W1 C25 115.67(17) . . ?
C27 W1 C25 79.83(17) . . ?
C22 W1 C23 76.34(15) . . ?
C27 W1 C23 79.09(15) . . ?
C25 W1 C23 72.03(16) . . ?
C22 W1 C98 140.19(16) . . ?
C27 W1 C98 73.21(16) . . ?
C25 W1 C98 74.20(17) . . ?
C23 W1 C98 139.33(16) . . ?
C22 W1 C26 70.65(16) . . ?
C27 W1 C26 144.46(16) . . ?
C25 W1 C26 75.85(17) . . ?
C23 W1 C26 116.47(16) . . ?
C98 W1 C26 75.46(16) . . ?
C22 W1 C99 72.65(16) . . ?
C27 W1 C99 75.87(16) . . ?
C25 W1 C99 140.55(16) . . ?
C23 W1 C99 73.18(16) . . ?
C98 W1 C99 125.80(17) . . ?
C26 W1 C99 137.79(16) . . ?
C22 W1 C24 80.36(16) . . ?
C27 W1 C24 105.83(17) . . ?
C25 W1 C24 144.54(17) . . ?
C23 W1 C24 143.25(16) . . ?
C98 W1 C24 74.21(17) . . ?
C26 W1 C24 81.00(17) . . ?
C99 W1 C24 72.94(17) . . ?
C79 W2 C78 72.30(16) . . ?
C79 W2 C81 78.83(16) . . ?
C78 W2 C81 142.80(16) . . ?
C79 W2 C80 75.64(16) . . ?
C78 W2 C80 76.49(17) . . ?
C81 W2 C80 73.98(16) . . ?
C79 W2 C77 143.36(16) . . ?
C78 W2 C77 141.56(16) . . ?
C81 W2 C77 73.86(15) . . ?
C80 W2 C77 118.27(16) . . ?
C79 W2 C96 113.78(17) . . ?
C78 W2 C96 73.37(17) . . ?
C81 W2 C96 141.52(17) . . ?
C80 W2 C96 143.15(17) . . ?
C77 W2 C96 76.49(16) . . ?
C79 W2 C76 141.33(16) . . ?
C78 W2 C76 78.38(16) . . ?
C81 W2 C76 113.46(16) . . ?
C80 W2 C76 73.40(16) . . ?
C77 W2 C76 73.39(16) . . ?
C96 W2 C76 80.14(17) . . ?
C79 W2 C92 71.23(16) . . ?
C78 W2 C92 114.44(17) . . ?
C81 W2 C92 76.33(16) . . ?
C80 W2 C92 138.91(16) . . ?
C77 W2 C92 78.86(16) . . ?
C96 W2 C92 74.32(17) . . ?
C76 W2 C92 145.87(16) . . ?

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
C6 C1 C2 O3 -179.4(4) . . . . ?
O5 C1 C2 O3 -0.2(5) . . . . ?
C6 C1 C2 C3 -1.7(6) . . . . ?
O5 C1 C2 C3 177.5(4) . . . . ?
O3 C2 C3 C4 178.5(4) . . . . ?
C1 C2 C3 C4 1.0(6) . . . . ?
O3 C2 C3 C7 -2.0(7) . . . . ?
C1 C2 C3 C7 -179.5(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C7 C3 C4 C5 -179.5(4) . . . . ?
C3 C4 C5 C6 -0.3(7) . . . . ?
O5 C1 C6 C5 -177.7(4) . . . . ?
C2 C1 C6 C5 1.5(7) . . . . ?
C4 C5 C6 C1 -0.5(7) . . . . ?
C2 C3 C7 N1 8.4(7) . . . . ?
C4 C3 C7 N1 -172.1(4) . . . . ?
N1 C8 C9 C10 55.0(5) . . . . ?
N1 C8 C9 C12 -70.1(5) . . . . ?
N1 C8 C9 C11 174.8(4) . . . . ?
C10 C9 C12 N2 -59.8(5) . . . . ?
C8 C9 C12 N2 65.4(5) . . . . ?
C11 C9 C12 N2 -179.2(4) . . . . ?
N2 C13 C14 C18 177.3(5) . . . . ?
N2 C13 C14 C15 -8.3(8) . . . . ?
C18 C14 C15 O2 -178.9(4) . . . . ?
C13 C14 C15 O2 6.7(7) . . . . ?
C18 C14 C15 C95 1.6(7) . . . . ?
C13 C14 C15 C95 -172.9(4) . . . . ?
C95 C16 C17 C18 1.2(8) . . . . ?
C16 C17 C18 C14 -1.8(9) . . . . ?
C15 C14 C18 C17 0.4(8) . . . . ?
C13 C14 C18 C17 175.1(5) . . . . ?
N11 C28 C29 C32 75.3(5) . . . . ?
N11 C28 C29 C31 -49.5(5) . . . . ?
N11 C28 C29 C30 -169.0(4) . . . . ?
C31 C29 C32 N10 61.4(5) . . . . ?
C30 C29 C32 N10 -178.2(4) . . . . ?
C28 C29 C32 N10 -62.7(5) . . . . ?
N10 C33 C34 C39 -0.5(8) . . . . ?
N10 C33 C34 C35 179.9(5) . . . . ?
C39 C34 C35 C36 1.2(8) . . . . ?
C33 C34 C35 C36 -179.1(5) . . . . ?
C34 C35 C36 C37 -2.1(9) . . . . ?
C35 C36 C37 C38 0.7(9) . . . . ?
C36 C37 C38 O4 -177.4(5) . . . 2_666 ?
C36 C37 C38 C39 1.7(8) . . . . ?
C35 C34 C39 O9 -179.7(4) . . . . ?
C33 C34 C39 O9 0.7(7) . . . . ?
C35 C34 C39 C38 1.1(7) . . . . ?
C33 C34 C39 C38 -178.6(4) . . . . ?
C37 C38 C39 O9 178.2(4) . . . . ?
O4 C38 C39 O9 -2.6(6) 2_666 . . . ?
C37 C38 C39 C34 -2.6(7) . . . . ?
O4 C38 C39 C34 176.7(4) 2_666 . . . ?
C46 C40 C41 N11 2.6(7) . . . . ?
C42 C40 C41 N11 178.2(4) . . . . ?
C46 C40 C42 C43 0.5(7) . . . . ?
C41 C40 C42 C43 -175.3(4) . . . . ?
C40 C42 C43 C44 0.8(7) . . . . ?
C42 C43 C44 C45 -0.5(7) . . . . ?
C43 C44 C45 O7 178.7(4) . . . 2_666 ?
C43 C44 C45 C46 -1.1(7) . . . . ?
C42 C40 C46 O8 179.5(4) . . . . ?
C41 C40 C46 O8 -4.9(7) . . . . ?
C42 C40 C46 C45 -2.1(6) . . . . ?
C41 C40 C46 C45 173.5(4) . . . . ?
C44 C45 C46 O8 -179.0(4) . . . . ?
O7 C45 C46 O8 1.1(6) 2_666 . . . ?
C44 C45 C46 C40 2.4(7) . . . . ?
O7 C45 C46 C40 -177.4(4) 2_666 . . . ?
O13 C47 C48 C49 -179.1(4) . . . . ?
C89 C47 C48 C49 0.5(6) 2_657 . . . ?
O13 C47 C48 O14 -0.2(6) . . . . ?
C89 C47 C48 O14 179.5(4) 2_657 . . . ?
O14 C48 C49 C50 -179.7(4) . . . . ?
C47 C48 C49 C50 -0.8(7) . . . . ?
C48 C49 C50 C90 0.5(7) . . . 2_657 ?
C59 C53 C54 O16 -179.9(4) . . . . ?
O15 C53 C54 O16 -0.8(6) . . . . ?
C59 C53 C54 C56 0.1(7) . . . . ?
O15 C53 C54 C56 179.2(4) . . . . ?
O16 C54 C56 C57 -179.7(4) . . . . ?
C53 C54 C56 C57 0.3(7) . . . . ?
O16 C54 C56 C55 3.1(7) . . . . ?
C53 C54 C56 C55 -176.9(4) . . . . ?
N12 C55 C56 C54 -5.5(8) . . . . ?
N12 C55 C56 C57 177.2(5) . . . . ?
C54 C56 C57 C58 -0.4(8) . . . . ?
C55 C56 C57 C58 177.1(5) . . . . ?
C56 C57 C58 C59 0.0(8) . . . . ?
O15 C53 C59 C58 -179.5(4) . . . . ?
C54 C53 C59 C58 -0.5(7) . . . . ?
C57 C58 C59 C53 0.4(8) . . . . ?
N12 C60 C64 C61 -57.1(5) . . . . ?
N12 C60 C64 C63 66.1(5) . . . . ?
N12 C60 C64 C62 -177.1(4) . . . . ?
N13 C63 C64 C60 -69.9(5) . . . . ?
N13 C63 C64 C61 54.1(5) . . . . ?
N13 C63 C64 C62 172.4(4) . . . . ?
N13 C65 C66 C71 -173.7(4) . . . . ?
N13 C65 C66 C67 4.9(7) . . . . ?
C71 C66 C67 O17 178.5(4) . . . . ?
C65 C66 C67 O17 0.0(7) . . . . ?
C71 C66 C67 C68 1.0(6) . . . . ?
C65 C66 C67 C68 -177.6(4) . . . . ?
O17 C67 C68 C69 -178.9(4) . . . . ?
C66 C67 C68 C69 -1.2(6) . . . . ?
O17 C67 C68 O23 -0.9(6) . . . . ?
C66 C67 C68 O23 176.8(4) . . . . ?
O23 C68 C69 C70 -177.3(4) . . . . ?
C67 C68 C69 C70 0.6(7) . . . . ?
C68 C69 C70 C71 0.3(7) . . . . ?
C69 C70 C71 C66 -0.6(7) . . . . ?
C67 C66 C71 C70 -0.1(7) . . . . ?
C65 C66 C71 C70 178.5(4) . . . . ?
C103 C72 C73 C74 0.3(8) . . . . ?
C82 C72 C73 C74 177.6(5) 2_657 . . . ?
C72 C73 C74 C75 0.0(9) . . . . ?
C73 C74 C75 C104 0.7(9) . . . . ?
N20 C83 C84 C86 62.9(5) . . . . ?
N20 C83 C84 C87 -61.2(5) . . . . ?
N20 C83 C84 C85 -176.8(4) . . . . ?
C86 C84 C87 N21 -50.2(5) . . . . ?
C83 C84 C87 N21 74.6(5) . . . . ?
C85 C84 C87 N21 -170.3(4) . . . . ?
N21 C88 C89 C90 175.0(4) . . . . ?
N21 C88 C89 C47 -1.9(7) . . . 2_657 ?
C47 C89 C90 C50 0.4(7) 2_657 . . 2_657 ?
C88 C89 C90 C50 -176.7(4) . . . 2_657 ?
C17 C16 C95 C15 0.8(7) . . . . ?
C17 C16 C95 O6 -178.5(4) . . . . ?
O2 C15 C95 C16 178.2(4) . . . . ?
C14 C15 C95 C16 -2.2(7) . . . . ?
O2 C15 C95 O6 -2.4(6) . . . . ?
C14 C15 C95 O6 177.2(4) . . . . ?
C73 C72 C103 O19 179.6(4) . . . . ?
C82 C72 C103 O19 2.5(7) 2_657 . . . ?
C73 C72 C103 C104 -1.3(7) . . . . ?
C82 C72 C103 C104 -178.4(4) 2_657 . . . ?
C74 C75 C104 O18 179.3(5) . . . . ?
C74 C75 C104 C103 -1.8(8) . . . . ?
O19 C103 C104 C75 -178.7(4) . . . . ?
C72 C103 C104 C75 2.1(7) . . . . ?
O19 C103 C104 O18 0.3(6) . . . . ?
C72 C103 C104 O18 -178.9(4) . . . . ?
C3 C7 N1 C8 -176.0(4) . . . . ?
C3 C7 N1 Ni2 1.3(7) . . . . ?
C9 C8 N1 C7 -125.9(5) . . . . ?
C9 C8 N1 Ni2 56.5(5) . . . . ?
C14 C13 N2 C12 170.8(5) . . . . ?
C14 C13 N2 Ni2 -0.7(7) . . . . ?
C9 C12 N2 C13 139.2(4) . . . . ?
C9 C12 N2 Ni2 -49.0(5) . . . . ?
C34 C33 N10 C32 -172.3(5) . . . . ?
C34 C33 N10 Ni1 -4.3(7) . . . . ?
C29 C32 N10 C33 -155.1(4) . . . . ?
C29 C32 N10 Ni1 37.0(5) . . . . ?
C40 C41 N11 C28 -176.3(4) . . . . ?
C40 C41 N11 Ni1 1.7(7) . . . . ?
C29 C28 N11 C41 119.8(5) . . . . ?
C29 C28 N11 Ni1 -58.3(5) . . . . ?
C56 C55 N12 C60 173.4(4) . . . . ?
C56 C55 N12 Ni3 2.6(7) . . . . ?
C64 C60 N12 C55 140.9(4) . . . . ?
C64 C60 N12 Ni3 -48.1(5) . . . . ?
C66 C65 N13 C63 -178.3(4) . . . . ?
C66 C65 N13 Ni3 1.2(7) . . . . ?
C64 C63 N13 C65 -126.4(4) . . . . ?
C64 C63 N13 Ni3 54.1(5) . . . . ?
C72 C82 N20 C83 -172.0(4) 2_657 . . . ?
C72 C82 N20 Ni06 -3.7(7) 2_657 . . . ?
C84 C83 N20 C82 -155.4(4) . . . . ?
C84 C83 N20 Ni06 36.3(5) . . . . ?
C89 C88 N21 C87 -178.5(4) . . . . ?
C89 C88 N21 Ni06 1.9(7) . . . . ?
C84 C87 N21 C88 121.2(4) . . . . ?
C84 C87 N21 Ni06 -59.1(5) . . . . ?
C95 C15 O2 Ni2 -177.1(3) . . . . ?
C14 C15 O2 Ni2 3.3(6) . . . . ?
C95 C15 O2 Y1 -12.5(5) . . . . ?
C14 C15 O2 Y1 167.9(3) . . . . ?
C3 C2 O3 Ni2 -12.7(6) . . . . ?
C1 C2 O3 Ni2 164.9(3) . . . . ?
C3 C2 O3 Y1 -177.6(3) . . . . ?
C1 C2 O3 Y1 -0.1(5) . . . . ?
C6 C1 O5 C21 2.3(6) . . . . ?
C2 C1 O5 C21 -176.9(4) . . . . ?
C6 C1 O5 Y1 179.5(3) . . . . ?
C2 C1 O5 Y1 0.3(4) . . . . ?
C16 C95 O6 C19 23.1(6) . . . . ?
C15 C95 O6 C19 -156.3(4) . . . . ?
C16 C95 O6 Y1 -166.2(4) . . . . ?
C15 C95 O6 Y1 14.4(5) . . . . ?
C40 C46 O8 Ni1 2.9(6) . . . . ?
C45 C46 O8 Ni1 -175.6(3) . . . . ?
C40 C46 O8 Y1 -161.3(3) . . . 2_666 ?
C45 C46 O8 Y1 20.3(5) . . . 2_666 ?
C34 C39 O9 Ni1 4.0(6) . . . . ?
C38 C39 O9 Ni1 -176.7(3) . . . . ?
C34 C39 O9 Y1 -166.4(3) . . . 2_666 ?
C38 C39 O9 Y1 12.8(5) . . . 2_666 ?
C89 C47 O13 Ni06 -7.2(6) 2_657 . . 2_657 ?
C48 C47 O13 Ni06 172.5(3) . . . 2_657 ?
C89 C47 O13 Y2 162.8(3) 2_657 . . . ?
C48 C47 O13 Y2 -17.5(5) . . . . ?
C49 C48 O14 C51 12.5(6) . . . . ?
C47 C48 O14 C51 -166.4(4) . . . . ?
C49 C48 O14 Y2 -165.5(3) . . . . ?
C47 C48 O14 Y2 15.6(5) . . . . ?
C59 C53 O15 C52 13.8(6) . . . . ?
C54 C53 O15 C52 -165.3(4) . . . . ?
C59 C53 O15 Y2 -172.3(3) . . . . ?
C54 C53 O15 Y2 8.6(5) . . . . ?
C56 C54 O16 Ni3 1.5(6) . . . . ?
C53 C54 O16 Ni3 -178.5(3) . . . . ?
C56 C54 O16 Y2 171.2(3) . . . . ?
C53 C54 O16 Y2 -8.8(5) . . . . ?
C66 C67 O17 Ni3 -10.0(6) . . . . ?
C68 C67 O17 Ni3 167.5(3) . . . . ?
C66 C67 O17 Y2 -179.3(3) . . . . ?
C68 C67 O17 Y2 -1.8(5) . . . . ?
C75 C104 O18 C105 11.0(6) . . . . ?
C103 C104 O18 C105 -167.9(4) . . . . ?
C75 C104 O18 Y2 -173.6(4) . . . . ?
C103 C104 O18 Y2 7.5(5) . . . . ?
C104 C103 O19 Ni06 177.3(3) . . . 2_657 ?
C72 C103 O19 Ni06 -3.5(6) . . . 2_657 ?
C104 C103 O19 Y2 -9.4(5) . . . . ?
C72 C103 O19 Y2 169.7(3) . . . . ?
C69 C68 O23 C084 4.0(6) . . . . ?
C67 C68 O23 C084 -174.0(4) . . . . ?
C69 C68 O23 Y2 -179.2(3) . . . . ?
C67 C68 O23 Y2 2.8(5) . . . . ?

_refine_diff_density_max         1.894
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.101

