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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_8
_database_code_depnum_ccdc_archive 'CCDC 1551796'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C48 H40 N18 Ni2 O11 Tb, C H F3 O3 S, 0.5(H2 O), C4 H8 O'
_chemical_formula_sum            'C53 H50 F3 N18 Ni2 O15.50 S Tb'
_chemical_formula_weight         1552.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.001(5)
_cell_length_b                   28.854(5)
_cell_length_c                   18.858(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.021(5)
_cell_angle_gamma                90
_cell_volume                     5876(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.391
_diffrn_reflns_Laue_measured_fraction_max 0.689
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16124
_diffrn_reflns_point_group_measured_fraction_full 0.391
_diffrn_reflns_point_group_measured_fraction_max 0.689
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.689
_diffrn_reflns_theta_min         2.824
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.391
_diffrn_measured_fraction_theta_max 0.689
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2999
_reflns_number_total             4159
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          2.039
_refine_ls_shift/su_mean         0.036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0837P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1289
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O12(0.5) H12A(0.5) H12B(0.5)
3.a Free rotating group:
 O12(H12A,H12B)
3.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
3.c Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39),
 C40(H40), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48)
3.e Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.48259(6) 0.27576(2) 0.36228(3) 0.0182(3) Uani 1 1 d . . . . .
Ni1 Ni 0.44056(14) 0.35751(5) 0.66926(8) 0.0181(5) Uani 1 1 d . . . . .
Ni2 Ni 0.51706(14) 0.11900(5) 0.68289(8) 0.0167(5) Uani 1 1 d . . . . .
O1 O 0.4649(7) 0.3135(3) 0.4630(4) 0.027(2) Uiso 1 1 d . . . . .
O2 O 0.5491(8) 0.1511(3) 0.4710(5) 0.045(3) Uiso 1 1 d . . . . .
O3 O 0.7527(7) 0.3420(3) 0.8329(4) 0.022(2) Uiso 1 1 d . . . . .
O4 O 0.3342(7) 0.3218(3) 0.3050(4) 0.024(2) Uiso 1 1 d . . . . .
O5 O 0.1176(8) 0.3104(3) 0.7288(4) 0.038(3) Uiso 1 1 d . . . . .
O6 O 0.1798(7) 0.1428(3) 0.7448(4) 0.023(2) Uiso 1 1 d . . . . .
O7 O 0.6333(7) 0.3345(3) 0.3772(4) 0.036(2) Uiso 1 1 d . . . . .
H7A H 0.6983 0.3262 0.4086 0.054 Uiso 1 1 d GR . . . .
H7B H 0.6561 0.3400 0.3364 0.054 Uiso 1 1 d GR . . . .
O8 O 0.5664(7) 0.2780(3) 0.2557(4) 0.032(2) Uiso 1 1 d . . . . .
H8A H 0.5840 0.2502 0.2438 0.049 Uiso 1 1 d GR . . . .
H8B H 0.5134 0.2898 0.2205 0.049 Uiso 1 1 d GR . . . .
O9 O 0.4485(8) 0.2038(3) 0.3029(4) 0.032(2) Uiso 1 1 d . . . . .
H9A H 0.5181 0.1907 0.3013 0.047 Uiso 1 1 d GR . . . .
H9B H 0.4068 0.1861 0.3261 0.047 Uiso 1 1 d GR . . . .
O10 O 0.3323(7) 0.2328(3) 0.4103(4) 0.029(2) Uiso 1 1 d . . . . .
H10A H 0.3091 0.2485 0.4436 0.044 Uiso 1 1 d GR . . . .
H10B H 0.2701 0.2275 0.3768 0.044 Uiso 1 1 d GR . . . .
O11 O 0.6369(7) 0.2304(3) 0.4344(4) 0.027(2) Uiso 1 1 d . . . . .
H11A H 0.6781 0.2466 0.4704 0.041 Uiso 1 1 d GR . . . .
H11B H 0.6034 0.2067 0.4524 0.041 Uiso 1 1 d GR . . . .
N1 N 0.3451(8) 0.3934(3) 0.5768(5) 0.020(3) Uiso 1 1 d . . . . .
N2 N 0.2347(10) 0.4304(4) 0.4415(6) 0.044(3) Uiso 1 1 d . . . . .
N3 N 0.4997(8) 0.3213(3) 0.5869(5) 0.017(3) Uiso 1 1 d . . . . .
N4 N 0.5597(8) 0.1551(3) 0.5958(5) 0.016(3) Uiso 1 1 d . . . . .
N5 N 0.3489(12) 0.0284(5) 0.4665(7) 0.065(4) Uiso 1 1 d . . . . .
N6 N 0.4434(8) 0.0746(4) 0.5941(5) 0.020(3) Uiso 1 1 d . . . . .
N7 N 0.3490(8) 0.3972(3) 0.7372(5) 0.018(3) Uiso 1 1 d . . . . .
N8 N 0.2084(11) 0.4401(4) 0.8269(6) 0.046(3) Uiso 1 1 d . . . . .
N9 N 0.2903(8) 0.3158(3) 0.6753(5) 0.017(3) Uiso 1 1 d . . . . .
N10 N 0.3436(8) 0.1479(3) 0.6847(5) 0.012(3) Uiso 1 1 d . . . . .
N11 N 0.3234(10) 0.0190(4) 0.8384(6) 0.043(3) Uiso 1 1 d . . . . .
N12 N 0.4530(9) 0.0762(3) 0.7590(5) 0.017(3) Uiso 1 1 d . . . . .
N13 N 0.5896(9) 0.4039(4) 0.6823(5) 0.024(3) Uiso 1 1 d . . . . .
N14 N 0.7986(10) 0.4605(4) 0.7166(6) 0.041(3) Uiso 1 1 d . . . . .
N15 N 0.5628(8) 0.3281(3) 0.7571(5) 0.015(3) Uiso 1 1 d . . . . .
N16 N 0.6276(8) 0.1616(3) 0.7614(5) 0.014(3) Uiso 1 1 d . . . . .
N17 N 0.9355(10) 0.0531(4) 0.7191(6) 0.036(3) Uiso 1 1 d . . . . .
N18 N 0.6904(8) 0.0852(4) 0.6957(5) 0.018(3) Uiso 1 1 d . . . . .
C1 C 0.2723(11) 0.4308(5) 0.5696(7) 0.027(4) Uiso 1 1 d . . . . .
H1 H 0.2573 0.4452 0.6112 0.032 Uiso 1 1 calc R . . . .
C2 C 0.2175(12) 0.4491(5) 0.5026(7) 0.033(4) Uiso 1 1 d . . . . .
H2 H 0.1675 0.4753 0.5010 0.040 Uiso 1 1 calc R . . . .
C3 C 0.3085(12) 0.3919(5) 0.4484(7) 0.039(4) Uiso 1 1 d . . . . .
H3 H 0.3215 0.3770 0.4067 0.047 Uiso 1 1 calc R . . . .
C4 C 0.3653(11) 0.3737(4) 0.5157(6) 0.018(3) Uiso 1 1 d . . . . .
C5 C 0.4475(11) 0.3327(4) 0.5219(7) 0.021(4) Uiso 1 1 d . . . . .
C6 C 0.5817(10) 0.2827(4) 0.5951(6) 0.013(3) Uiso 1 1 d . . . . .
C7 C 0.7089(11) 0.2897(4) 0.6139(6) 0.020(3) Uiso 1 1 d . . . . .
H7 H 0.7408 0.3196 0.6206 0.025 Uiso 1 1 calc R . . . .
C8 C 0.7871(12) 0.2521(4) 0.6227(6) 0.021(3) Uiso 1 1 d . . . . .
H8 H 0.8724 0.2566 0.6329 0.025 Uiso 1 1 calc R . . . .
C9 C 0.5362(11) 0.2384(4) 0.5876(6) 0.015(3) Uiso 1 1 d . . . . .
H9 H 0.4511 0.2339 0.5745 0.018 Uiso 1 1 calc R . . . .
C10 C 0.7388(11) 0.2069(4) 0.6163(6) 0.021(3) Uiso 1 1 d . . . . .
H10 H 0.7916 0.1815 0.6239 0.025 Uiso 1 1 calc R . . . .
C11 C 0.6118(10) 0.2006(4) 0.5988(6) 0.013(3) Uiso 1 1 d . . . . .
C12 C 0.5285(11) 0.1366(5) 0.5319(7) 0.029(4) Uiso 1 1 d . . . . .
C13 C 0.4593(11) 0.0913(4) 0.5316(6) 0.019(3) Uiso 1 1 d . . . . .
C14 C 0.4135(14) 0.0689(6) 0.4681(8) 0.055(5) Uiso 1 1 d . . . . .
H14 H 0.4269 0.0815 0.4249 0.066 Uiso 1 1 calc R . . . .
C15 C 0.3383(13) 0.0125(5) 0.5304(8) 0.046(4) Uiso 1 1 d . . . . .
H15 H 0.2968 -0.0154 0.5324 0.056 Uiso 1 1 calc R . . . .
C16 C 0.3837(10) 0.0341(4) 0.5935(6) 0.019(3) Uiso 1 1 d . . . . .
H16 H 0.3733 0.0208 0.6369 0.023 Uiso 1 1 calc R . . . .
C17 C 0.3796(12) 0.4401(5) 0.7665(6) 0.031(4) Uiso 1 1 d . . . . .
H17 H 0.4479 0.4559 0.7564 0.037 Uiso 1 1 calc R . . . .
C18 C 0.3071(12) 0.4595(5) 0.8116(7) 0.034(4) Uiso 1 1 d . . . . .
H18 H 0.3306 0.4882 0.8321 0.040 Uiso 1 1 calc R . . . .
C19 C 0.1786(14) 0.3981(5) 0.7967(7) 0.051(5) Uiso 1 1 d . . . . .
H19 H 0.1096 0.3829 0.8070 0.062 Uiso 1 1 calc R . . . .
C20 C 0.2468(12) 0.3766(4) 0.7508(6) 0.024(4) Uiso 1 1 d . . . . .
C21 C 0.2157(11) 0.3300(4) 0.7161(6) 0.020(3) Uiso 1 1 d . . . . .
C22 C 0.2638(10) 0.2716(4) 0.6424(6) 0.015(3) Uiso 1 1 d . . . . .
C23 C 0.1993(10) 0.2685(4) 0.5701(6) 0.019(3) Uiso 1 1 d . . . . .
H23 H 0.1707 0.2950 0.5442 0.022 Uiso 1 1 calc R . . . .
C24 C 0.1800(11) 0.2257(4) 0.5395(7) 0.023(3) Uiso 1 1 d . . . . .
H24 H 0.1339 0.2229 0.4930 0.027 Uiso 1 1 calc R . . . .
C25 C 0.3056(10) 0.2321(4) 0.6798(6) 0.014(3) Uiso 1 1 d . . . . .
H25 H 0.3447 0.2343 0.7280 0.016 Uiso 1 1 calc R . . . .
C26 C 0.2289(10) 0.1858(5) 0.5773(6) 0.021(4) Uiso 1 1 d . . . . .
H26 H 0.2190 0.1571 0.5545 0.025 Uiso 1 1 calc R . . . .
C27 C 0.2904(10) 0.1888(4) 0.6466(6) 0.013(3) Uiso 1 1 d . . . . .
C28 C 0.2819(11) 0.1292(4) 0.7290(6) 0.017(3) Uiso 1 1 d . . . . .
C29 C 0.3366(10) 0.0853(4) 0.7657(6) 0.014(3) Uiso 1 1 d . . . . .
C30 C 0.2720(13) 0.0567(5) 0.8031(7) 0.039(4) Uiso 1 1 d . . . . .
H30 H 0.1898 0.0636 0.8042 0.046 Uiso 1 1 calc R . . . .
C31 C 0.4421(12) 0.0125(5) 0.8346(7) 0.036(4) Uiso 1 1 d . . . . .
H31 H 0.4843 -0.0118 0.8609 0.043 Uiso 1 1 calc R . . . .
C32 C 0.5056(12) 0.0397(4) 0.7942(6) 0.022(3) Uiso 1 1 d . . . . .
H32 H 0.5869 0.0323 0.7917 0.027 Uiso 1 1 calc R . . . .
C33 C 0.6085(12) 0.4411(5) 0.6415(7) 0.031(4) Uiso 1 1 d . . . . .
H33 H 0.5500 0.4479 0.6003 0.037 Uiso 1 1 calc R . . . .
C34 C 0.7101(12) 0.4686(5) 0.6591(7) 0.036(4) Uiso 1 1 d . . . . .
H34 H 0.7180 0.4940 0.6299 0.043 Uiso 1 1 calc R . . . .
C35 C 0.7813(12) 0.4225(5) 0.7557(7) 0.030(4) Uiso 1 1 d . . . . .
H35 H 0.8416 0.4152 0.7958 0.036 Uiso 1 1 calc R . . . .
C36 C 0.6798(10) 0.3945(4) 0.7392(6) 0.015(3) Uiso 1 1 d . . . . .
C37 C 0.6631(11) 0.3514(4) 0.7799(6) 0.016(3) Uiso 1 1 d . . . . .
C38 C 0.5502(11) 0.2838(4) 0.7910(6) 0.017(3) Uiso 1 1 d . . . . .
C39 C 0.4748(10) 0.2783(4) 0.8414(6) 0.016(3) Uiso 1 1 d . . . . .
H39 H 0.4346 0.3038 0.8565 0.020 Uiso 1 1 calc R . . . .
C40 C 0.6068(10) 0.2456(4) 0.7675(6) 0.014(3) Uiso 1 1 d . . . . .
H40 H 0.6602 0.2491 0.7352 0.017 Uiso 1 1 calc R . . . .
C41 C 0.4598(11) 0.2348(4) 0.8691(6) 0.024(4) Uiso 1 1 d . . . . .
H41 H 0.4136 0.2314 0.9053 0.029 Uiso 1 1 calc R . . . .
C42 C 0.5118(10) 0.1965(4) 0.8442(6) 0.014(3) Uiso 1 1 d . . . . .
H42 H 0.4989 0.1672 0.8620 0.017 Uiso 1 1 calc R . . . .
C43 C 0.5831(10) 0.2019(4) 0.7928(6) 0.011(3) Uiso 1 1 d . . . . .
C44 C 0.7463(11) 0.1531(4) 0.7705(6) 0.020(3) Uiso 1 1 d . . . . .
C45 C 0.7808(10) 0.1093(4) 0.7370(6) 0.014(3) Uiso 1 1 d . . . . .
C46 C 0.9028(11) 0.0926(5) 0.7490(6) 0.025(4) Uiso 1 1 d . . . . .
H46 H 0.9641 0.1095 0.7789 0.031 Uiso 1 1 calc R . . . .
C47 C 0.8439(12) 0.0308(5) 0.6777(7) 0.036(4) Uiso 1 1 d . . . . .
H47 H 0.8614 0.0037 0.6548 0.043 Uiso 1 1 calc R . . . .
C48 C 0.7225(11) 0.0463(5) 0.6670(6) 0.024(4) Uiso 1 1 d . . . . .
H48 H 0.6611 0.0286 0.6386 0.029 Uiso 1 1 calc R . . . .
S1 S 1.3601(4) 0.09475(18) 0.9992(2) 0.0702(15) Uiso 1 1 d . . . . .
F1 F 1.4325(10) 0.1756(4) 1.0501(6) 0.108(4) Uiso 1 1 d . . . . .
F2 F 1.4056(9) 0.1243(4) 1.1298(5) 0.090(3) Uiso 1 1 d . . . . .
F3 F 1.5638(11) 0.1216(4) 1.0802(6) 0.115(4) Uiso 1 1 d . . . . .
O13 O 1.4198(11) 0.1074(5) 0.9381(7) 0.096(4) Uiso 1 1 d . . . . .
H13 H 1.3702 0.1040 0.9001 0.145 Uiso 1 1 calc GR . . . .
O14 O 1.3872(10) 0.0485(4) 1.0288(6) 0.072(3) Uiso 1 1 d . . . . .
O15 O 1.2316(10) 0.1086(4) 0.9947(6) 0.076(4) Uiso 1 1 d . . . . .
C49 C 1.4433(18) 0.1298(7) 1.0668(10) 0.079(6) Uiso 1 1 d . . . . .
O12 O 1.048(2) 0.0334(8) 0.9456(13) 0.067(7) Uiso 0.5 1 d . . P . .
H12A H 1.0668 0.0301 0.9912 0.100 Uiso 0.5 1 d G . P . .
H12B H 1.1142 0.0343 0.9284 0.100 Uiso 0.5 1 d G . P . .
O16 O 0.419(3) 0.4419(10) 1.0180(14) 0.249(11) Uiso 1 1 d . . . . .
C50 C 0.532(2) 0.4355(8) 0.9980(12) 0.121(8) Uiso 1 1 d . . . . .
H50A H 0.5966 0.4287 1.0391 0.145 Uiso 1 1 calc R . . . .
H50B H 0.5550 0.4620 0.9720 0.145 Uiso 1 1 calc R . . . .
C51 C 0.4980(19) 0.3923(7) 0.9477(10) 0.101(7) Uiso 1 1 d . . . . .
H51A H 0.4602 0.4019 0.8991 0.122 Uiso 1 1 calc R . . . .
H51B H 0.5714 0.3742 0.9454 0.122 Uiso 1 1 calc R . . . .
C52 C 0.4084(18) 0.3649(7) 0.9816(10) 0.094(7) Uiso 1 1 d . . . . .
H52A H 0.3302 0.3603 0.9485 0.113 Uiso 1 1 calc R . . . .
H52B H 0.4424 0.3351 0.9991 0.113 Uiso 1 1 calc R . . . .
C53 C 0.395(3) 0.3959(12) 1.0408(16) 0.192(13) Uiso 1 1 d . . . . .
H53A H 0.3126 0.3937 1.0512 0.230 Uiso 1 1 calc R . . . .
H53B H 0.4545 0.3877 1.0841 0.230 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.230(8) . ?
Tb1 O4 2.219(8) . ?
Tb1 O7 2.351(8) . ?
Tb1 O8 2.368(8) . ?
Tb1 O9 2.356(8) . ?
Tb1 O10 2.379(8) . ?
Tb1 O11 2.357(7) . ?
Ni1 N1 2.125(9) . ?
Ni1 N3 2.077(10) . ?
Ni1 N7 2.113(10) . ?
Ni1 N9 2.066(10) . ?
Ni1 N13 2.093(10) . ?
Ni1 N15 2.103(9) . ?
Ni2 N4 2.073(10) . ?
Ni2 N6 2.140(9) . ?
Ni2 N10 2.089(9) . ?
Ni2 N12 2.114(10) . ?
Ni2 N16 2.119(9) . ?
Ni2 N18 2.115(10) . ?
O1 C5 1.288(13) . ?
O2 C12 1.283(14) . ?
O3 C37 1.291(12) . ?
O4 C44 1.282(13) 4_565 ?
O5 C21 1.281(13) . ?
O6 C28 1.279(13) . ?
N1 C1 1.335(14) . ?
N1 C4 1.339(14) . ?
N2 C2 1.319(15) . ?
N2 C3 1.369(16) . ?
N3 C5 1.293(13) . ?
N3 C6 1.424(14) . ?
N4 C11 1.429(14) . ?
N4 C12 1.304(14) . ?
N5 C14 1.365(18) . ?
N5 C15 1.315(17) . ?
N6 C13 1.316(13) . ?
N6 C16 1.339(14) . ?
N7 C17 1.370(15) . ?
N7 C20 1.338(14) . ?
N8 C18 1.302(15) . ?
N8 C19 1.352(17) . ?
N9 C21 1.295(14) . ?
N9 C22 1.424(14) . ?
N10 C27 1.446(14) . ?
N10 C28 1.290(13) . ?
N11 C30 1.342(16) . ?
N11 C31 1.334(15) . ?
N12 C29 1.337(13) . ?
N12 C32 1.318(14) . ?
N13 C33 1.359(15) . ?
N13 C36 1.343(13) . ?
N14 C34 1.332(14) . ?
N14 C35 1.356(15) . ?
N15 C37 1.294(13) . ?
N15 C38 1.447(14) . ?
N16 C43 1.434(14) . ?
N16 C44 1.306(13) . ?
N17 C46 1.350(15) . ?
N17 C47 1.318(15) . ?
N18 C45 1.336(13) . ?
N18 C48 1.322(14) . ?
C1 C2 1.397(16) . ?
C3 C4 1.404(16) . ?
C4 C5 1.480(16) . ?
C6 C7 1.392(15) . ?
C6 C9 1.370(15) . ?
C7 C8 1.374(15) . ?
C8 C10 1.404(16) . ?
C9 C11 1.362(15) . ?
C10 C11 1.385(15) . ?
C12 C13 1.510(17) . ?
C13 C14 1.371(17) . ?
C15 C16 1.351(16) . ?
C17 C18 1.389(17) . ?
C19 C20 1.394(18) . ?
C20 C21 1.506(17) . ?
C22 C23 1.414(15) . ?
C22 C25 1.371(15) . ?
C23 C24 1.361(16) . ?
C24 C26 1.407(16) . ?
C25 C27 1.394(15) . ?
C26 C27 1.355(14) . ?
C28 C29 1.511(16) . ?
C29 C30 1.371(16) . ?
C31 C32 1.374(17) . ?
C33 C34 1.360(17) . ?
C35 C36 1.366(15) . ?
C36 C37 1.490(16) . ?
C38 C39 1.385(15) . ?
C38 C40 1.379(15) . ?
C39 C41 1.384(16) . ?
C40 C43 1.390(15) . ?
C41 C42 1.367(15) . ?
C42 C43 1.368(15) . ?
C44 O4 1.282(13) 4_666 ?
C44 C45 1.494(16) . ?
C45 C46 1.404(15) . ?
C47 C48 1.387(16) . ?
S1 O13 1.476(13) . ?
S1 O14 1.456(11) . ?
S1 O15 1.456(11) . ?
S1 C49 1.743(19) . ?
F1 C49 1.36(2) . ?
F2 C49 1.340(19) . ?
F3 C49 1.323(19) . ?
O16 C50 1.38(3) . ?
O16 C53 1.43(3) . ?
C50 C51 1.57(3) . ?
C51 C52 1.50(2) . ?
C52 C53 1.46(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O7 73.8(3) . . ?
O1 Tb1 O8 145.3(3) . . ?
O1 Tb1 O9 143.5(3) . . ?
O1 Tb1 O10 75.5(3) . . ?
O1 Tb1 O11 87.1(3) . . ?
O4 Tb1 O1 86.9(3) . . ?
O4 Tb1 O7 93.6(3) . . ?
O4 Tb1 O8 86.6(3) . . ?
O4 Tb1 O9 105.1(3) . . ?
O4 Tb1 O10 89.8(3) . . ?
O4 Tb1 O11 174.1(3) . . ?
O7 Tb1 O8 72.7(3) . . ?
O7 Tb1 O9 137.5(3) . . ?
O7 Tb1 O10 148.8(3) . . ?
O7 Tb1 O11 85.3(3) . . ?
O8 Tb1 O10 138.5(3) . . ?
O9 Tb1 O8 70.9(3) . . ?
O9 Tb1 O10 70.3(3) . . ?
O9 Tb1 O11 79.4(3) . . ?
O11 Tb1 O8 98.6(3) . . ?
O11 Tb1 O10 88.2(3) . . ?
N3 Ni1 N1 78.9(4) . . ?
N3 Ni1 N7 168.6(3) . . ?
N3 Ni1 N13 93.4(4) . . ?
N3 Ni1 N15 98.2(4) . . ?
N7 Ni1 N1 90.9(4) . . ?
N9 Ni1 N1 93.1(4) . . ?
N9 Ni1 N3 96.7(4) . . ?
N9 Ni1 N7 78.7(4) . . ?
N9 Ni1 N13 169.4(4) . . ?
N9 Ni1 N15 96.8(4) . . ?
N13 Ni1 N1 92.2(4) . . ?
N13 Ni1 N7 92.1(4) . . ?
N13 Ni1 N15 78.3(4) . . ?
N15 Ni1 N1 169.9(4) . . ?
N15 Ni1 N7 92.7(3) . . ?
N4 Ni2 N6 77.9(4) . . ?
N4 Ni2 N10 99.1(4) . . ?
N4 Ni2 N12 170.7(3) . . ?
N4 Ni2 N16 94.3(4) . . ?
N4 Ni2 N18 89.2(4) . . ?
N10 Ni2 N6 92.4(4) . . ?
N10 Ni2 N12 78.3(4) . . ?
N10 Ni2 N16 99.3(4) . . ?
N10 Ni2 N18 171.6(4) . . ?
N12 Ni2 N6 93.2(4) . . ?
N12 Ni2 N16 94.9(3) . . ?
N12 Ni2 N18 93.6(4) . . ?
N16 Ni2 N6 166.9(4) . . ?
N18 Ni2 N6 90.6(4) . . ?
N18 Ni2 N16 78.7(4) . . ?
C5 O1 Tb1 175.1(8) . . ?
C44 O4 Tb1 177.6(8) 4_565 . ?
C1 N1 Ni1 132.0(8) . . ?
C1 N1 C4 116.8(10) . . ?
C4 N1 Ni1 111.2(8) . . ?
C2 N2 C3 115.5(12) . . ?
C5 N3 Ni1 115.8(8) . . ?
C5 N3 C6 117.3(10) . . ?
C6 N3 Ni1 126.5(7) . . ?
C11 N4 Ni2 125.5(7) . . ?
C12 N4 Ni2 117.8(9) . . ?
C12 N4 C11 116.5(10) . . ?
C15 N5 C14 114.5(14) . . ?
C13 N6 Ni2 112.7(8) . . ?
C13 N6 C16 117.5(10) . . ?
C16 N6 Ni2 129.8(8) . . ?
C17 N7 Ni1 128.7(9) . . ?
C20 N7 Ni1 113.0(8) . . ?
C20 N7 C17 118.3(11) . . ?
C18 N8 C19 115.9(13) . . ?
C21 N9 Ni1 116.9(8) . . ?
C21 N9 C22 116.3(10) . . ?
C22 N9 Ni1 126.7(8) . . ?
C27 N10 Ni2 127.0(8) . . ?
C28 N10 Ni2 116.0(8) . . ?
C28 N10 C27 116.8(10) . . ?
C31 N11 C30 114.3(13) . . ?
C29 N12 Ni2 113.5(8) . . ?
C32 N12 Ni2 129.6(8) . . ?
C32 N12 C29 116.5(11) . . ?
C33 N13 Ni1 129.7(8) . . ?
C36 N13 Ni1 114.1(8) . . ?
C36 N13 C33 116.2(10) . . ?
C34 N14 C35 115.3(12) . . ?
C37 N15 Ni1 115.3(8) . . ?
C37 N15 C38 117.4(9) . . ?
C38 N15 Ni1 127.1(7) . . ?
C43 N16 Ni2 124.3(7) . . ?
C44 N16 Ni2 114.1(8) . . ?
C44 N16 C43 120.6(10) . . ?
C47 N17 C46 115.2(11) . . ?
C45 N18 Ni2 112.3(8) . . ?
C48 N18 Ni2 130.6(8) . . ?
C48 N18 C45 117.0(10) . . ?
N1 C1 C2 123.0(12) . . ?
N2 C2 C1 121.8(13) . . ?
N2 C3 C4 122.9(13) . . ?
N1 C4 C3 120.0(12) . . ?
N1 C4 C5 118.1(10) . . ?
C3 C4 C5 121.9(12) . . ?
O1 C5 N3 126.5(11) . . ?
O1 C5 C4 117.8(10) . . ?
N3 C5 C4 115.6(11) . . ?
C7 C6 N3 119.9(11) . . ?
C9 C6 N3 120.6(10) . . ?
C9 C6 C7 119.5(11) . . ?
C8 C7 C6 119.5(12) . . ?
C7 C8 C10 120.3(12) . . ?
C11 C9 C6 122.0(11) . . ?
C11 C10 C8 119.3(12) . . ?
C9 C11 N4 120.0(10) . . ?
C9 C11 C10 119.4(12) . . ?
C10 C11 N4 120.5(11) . . ?
O2 C12 N4 129.2(12) . . ?
O2 C12 C13 117.0(11) . . ?
N4 C12 C13 113.7(11) . . ?
N6 C13 C12 117.8(11) . . ?
N6 C13 C14 121.4(13) . . ?
C14 C13 C12 120.8(12) . . ?
N5 C14 C13 121.7(14) . . ?
N5 C15 C16 124.3(15) . . ?
N6 C16 C15 120.5(12) . . ?
N7 C17 C18 119.0(13) . . ?
N8 C18 C17 124.2(14) . . ?
N8 C19 C20 122.9(14) . . ?
N7 C20 C19 119.5(12) . . ?
N7 C20 C21 116.3(12) . . ?
C19 C20 C21 124.2(13) . . ?
O5 C21 N9 128.5(12) . . ?
O5 C21 C20 116.3(12) . . ?
N9 C21 C20 115.1(11) . . ?
C23 C22 N9 120.0(10) . . ?
C25 C22 N9 119.9(10) . . ?
C25 C22 C23 120.0(11) . . ?
C24 C23 C22 118.3(12) . . ?
C23 C24 C26 120.9(12) . . ?
C22 C25 C27 120.9(11) . . ?
C27 C26 C24 120.5(12) . . ?
C25 C27 N10 120.4(10) . . ?
C26 C27 N10 120.5(11) . . ?
C26 C27 C25 119.1(11) . . ?
O6 C28 N10 128.0(11) . . ?
O6 C28 C29 116.2(11) . . ?
N10 C28 C29 115.8(11) . . ?
N12 C29 C28 115.2(11) . . ?
N12 C29 C30 122.0(12) . . ?
C30 C29 C28 122.7(11) . . ?
N11 C30 C29 122.2(13) . . ?
N11 C31 C32 123.8(13) . . ?
N12 C32 C31 121.0(12) . . ?
N13 C33 C34 122.1(12) . . ?
N14 C34 C33 122.3(13) . . ?
N14 C35 C36 123.3(12) . . ?
N13 C36 C35 120.6(11) . . ?
N13 C36 C37 115.8(10) . . ?
C35 C36 C37 123.6(11) . . ?
O3 C37 N15 128.6(11) . . ?
O3 C37 C36 115.1(10) . . ?
N15 C37 C36 116.4(10) . . ?
C39 C38 N15 121.6(11) . . ?
C40 C38 N15 118.5(11) . . ?
C40 C38 C39 119.7(12) . . ?
C41 C39 C38 119.6(12) . . ?
C38 C40 C43 119.3(12) . . ?
C42 C41 C39 121.0(13) . . ?
C41 C42 C43 119.1(12) . . ?
C40 C43 N16 119.6(10) . . ?
C42 C43 N16 119.2(11) . . ?
C42 C43 C40 121.1(11) . . ?
O4 C44 N16 126.8(12) 4_666 . ?
O4 C44 C45 117.7(10) 4_666 . ?
N16 C44 C45 115.5(10) . . ?
N18 C45 C44 117.8(10) . . ?
N18 C45 C46 119.8(11) . . ?
C46 C45 C44 122.4(10) . . ?
N17 C46 C45 123.1(11) . . ?
N17 C47 C48 122.3(13) . . ?
N18 C48 C47 122.7(12) . . ?
O13 S1 C49 100.2(9) . . ?
O14 S1 O13 115.9(8) . . ?
O14 S1 O15 113.5(7) . . ?
O14 S1 C49 102.2(8) . . ?
O15 S1 O13 117.3(7) . . ?
O15 S1 C49 104.6(9) . . ?
F1 C49 S1 112.6(13) . . ?
F2 C49 S1 111.8(14) . . ?
F2 C49 F1 107.0(16) . . ?
F3 C49 S1 113.7(14) . . ?
F3 C49 F1 105.0(16) . . ?
F3 C49 F2 106.1(15) . . ?
C50 O16 C53 100(3) . . ?
O16 C50 C51 99(2) . . ?
C52 C51 C50 105.0(17) . . ?
C53 C52 C51 100(2) . . ?
O16 C53 C52 107(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dc170
_database_code_depnum_ccdc_archive 'CCDC 1551795'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H30 Gd N19 Ni2 O13, 3.5(O), C4 H8 O'
_chemical_formula_sum            'C52 H53 Gd N19 Ni2 O17.50'
_chemical_formula_weight         1498.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3895(7)
_cell_length_b                   24.9529(9)
_cell_length_c                   20.7809(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.632(5)
_cell_angle_gamma                90
_cell_volume                     6616.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10473
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6933
_cell_measurement_theta_min      2.9176
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.97791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_av_unetI/netI     0.2394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65369
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.768
_diffrn_reflns_theta_min         2.923
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8502
_reflns_number_total             20733
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.448
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         20733
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0648
_refine_ls_restrained_S_all      0.899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0790P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1843
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C56-C55 = C55-C54 = C54-C53
 1.4 with sigma of 0.02
 O15-C56 = O15-C53
 1.35 with sigma of 0.02
 C50-C49 = C51-C50 = C52-C51
 1.4 with sigma of 0.02
 N3-C20 \\sim N3A-C20A
 with sigma of 0.02
 N3-C17 \\sim N3A-C17A
 with sigma of 0.02
 O3A-C21 \\sim O3-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N14A) \\sim Ueq,
Uanis(N14) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17A)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N3A) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(O3)=Sof(N3A)=Sof(N14A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(C21A)=1-FVAR(1)
 Sof(O3A)=Sof(N3)=Sof(N14)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(C21)=FVAR(1)
 Sof(O19a)=1-FVAR(2)
 Sof(O19)=FVAR(2)
 Fixed Sof: O18(0.5) O20(0.5) O14(0.5) C49(0.5) H49a(0.5) H49b(0.5) C50(0.5)
 H50a(0.5) H50b(0.5) C51(0.5) H51a(0.5) H51b(0.5) C52(0.5) H52a(0.5) H52b(0.5)
 O15(0.5) C53(0.5) H53a(0.5) H53b(0.5) C54(0.5) H54a(0.5) H54b(0.5) C55(0.5)
 H55a(0.5) H55b(0.5) C56(0.5) H56a(0.5) H56b(0.5) O17(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b), C52(H52a,H52b), C53(H53a,
 H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C17A(H17A), C18(H18), C18A(H18A), C19(H19), C19A(H19A),
 C23(H23), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C43(H43), C46(H46),
 C47(H47), C48(H48)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.45641(3) 0.28675(2) 0.37729(2) 0.02326(10) Uani 1 1 d . . . . .
Ni1 Ni 0.68687(7) 0.10154(3) 0.68410(4) 0.0226(2) Uani 1 1 d . . . . .
Ni2 Ni 0.73144(7) 0.37585(3) 0.65318(4) 0.0227(2) Uani 1 1 d . . . . .
O1 O 1.0056(4) 0.1339(2) 0.7492(3) 0.0612(19) Uani 1 1 d . . . . .
O2 O 1.0384(4) 0.3214(2) 0.7272(3) 0.0457(15) Uani 1 1 d . . . . .
O3 O 0.4973(14) 0.1281(7) 0.4886(7) 0.051(5) Uani 0.50(2) 1 d D U P A 2
O3A O 0.5405(13) 0.1392(6) 0.4821(5) 0.035(4) Uani 0.50(2) 1 d D U P A 1
O4 O 0.5981(4) 0.30743(19) 0.4660(2) 0.0283(11) Uani 1 1 d . . . . .
O5 O 0.5303(4) 0.17344(18) 0.8055(2) 0.0290(11) Uani 1 1 d . . . . .
O6 O 0.5531(4) 0.34929(18) 0.7822(2) 0.0309(12) Uani 1 1 d . . . . .
O7 O 0.5898(4) 0.21693(19) 0.3909(2) 0.0345(12) Uani 1 1 d . . . . .
O8 O 0.3915(4) 0.2184(2) 0.4334(3) 0.0432(14) Uani 1 1 d . . . . .
O9 O 0.3998(4) 0.22682(19) 0.2802(3) 0.0380(13) Uani 1 1 d . . . . .
O10 O 0.2817(4) 0.3087(2) 0.3158(3) 0.0439(14) Uani 1 1 d . . . . .
O11 O 0.3802(4) 0.3376(2) 0.4563(3) 0.0382(13) Uani 1 1 d . . . . .
O12 O 0.4491(4) 0.38668(19) 0.3958(2) 0.0362(13) Uani 1 1 d . . . . .
O13 O 0.3902(6) 0.4238(2) 0.4725(3) 0.066(2) Uani 1 1 d . . . . .
N1 N 0.7908(5) 0.0539(2) 0.7575(3) 0.0270(13) Uani 1 1 d . . . . .
N2 N 0.8308(4) 0.1343(2) 0.6869(3) 0.0243(13) Uani 1 1 d . . . . .
N3 N 0.6934(19) 0.0480(9) 0.6092(10) 0.021(5) Uani 0.50(2) 1 d D U P A 1
N3A N 0.675(2) 0.0461(10) 0.6021(11) 0.028(7) Uani 0.50(2) 1 d D U P A 2
N4 N 0.5898(5) 0.1400(2) 0.5998(3) 0.0242(13) Uani 1 1 d . . . . .
N5 N 0.5526(5) 0.0660(2) 0.7005(3) 0.0249(13) Uani 1 1 d . . . . .
N6 N 0.6562(4) 0.1527(2) 0.7566(3) 0.0228(12) Uani 1 1 d . . . . .
N7 N 0.8484(5) 0.4219(2) 0.7186(3) 0.0297(14) Uani 1 1 d . . . . .
N8 N 0.8634(5) 0.3280(2) 0.6646(3) 0.0261(13) Uani 1 1 d . . . . .
N9 N 0.7552(5) 0.4094(2) 0.5652(3) 0.0276(14) Uani 1 1 d . . . . .
N10 N 0.6268(4) 0.3312(2) 0.5771(3) 0.0209(12) Uani 1 1 d . . . . .
N11 N 0.6078(4) 0.4278(2) 0.6533(3) 0.0223(12) Uani 1 1 d . . . . .
N12 N 0.6863(4) 0.3448(2) 0.7330(3) 0.0203(12) Uani 1 1 d . . . . .
N13 N 0.9481(6) 0.0015(3) 0.8550(4) 0.053(2) Uani 1 1 d . . . . .
N14 N 0.6922(15) -0.0083(7) 0.4900(8) 0.046(5) Uani 0.50(2) 1 d . U P A 1
N14A N 0.6351(19) -0.0214(8) 0.4928(9) 0.066(6) Uani 0.50(2) 1 d . U P A 2
N15 N 0.3621(5) 0.0371(3) 0.7191(3) 0.0381(16) Uani 1 1 d . . . . .
N16 N 1.0192(6) 0.4699(3) 0.8118(4) 0.055(2) Uani 1 1 d . . . . .
N17 N 0.7881(5) 0.4306(3) 0.4410(3) 0.0437(18) Uani 1 1 d . . . . .
N18 N 0.4155(5) 0.4732(2) 0.6497(3) 0.0388(16) Uani 1 1 d . . . . .
N19 N 0.4064(5) 0.3839(3) 0.4429(3) 0.0386(16) Uani 1 1 d . . . . .
C1 C 0.7710(6) 0.0119(3) 0.7896(4) 0.0330(18) Uani 1 1 d . . . . .
H1 H 0.7022 -0.0001 0.7793 0.040 Uiso 1 1 calc R . . . .
C2 C 0.8475(7) -0.0150(3) 0.8375(4) 0.046(2) Uani 1 1 d . . . . .
H2 H 0.8298 -0.0450 0.8582 0.055 Uiso 1 1 calc R . . . .
C3 C 0.9688(7) 0.0454(3) 0.8241(4) 0.046(2) Uani 1 1 d . . . . .
H3 H 1.0367 0.0589 0.8365 0.055 Uiso 1 1 calc R . . . .
C4 C 0.8920(6) 0.0706(3) 0.7746(4) 0.0298(17) Uani 1 1 d . . . . .
C5 C 0.9142(6) 0.1176(3) 0.7339(4) 0.0335(18) Uani 1 1 d . . . . .
C6 C 0.8447(5) 0.1791(3) 0.6470(3) 0.0241(15) Uani 1 1 d . . . . .
C7 C 0.8394(6) 0.1732(3) 0.5797(4) 0.0296(17) Uani 1 1 d . . . . .
H7 H 0.8318 0.1393 0.5604 0.036 Uiso 1 1 calc R . . . .
C8 C 0.8453(6) 0.2165(3) 0.5422(4) 0.0337(17) Uani 1 1 d . . . . .
H8 H 0.8413 0.2119 0.4970 0.040 Uiso 1 1 calc R . . . .
C9 C 0.8571(6) 0.2681(3) 0.5697(4) 0.0320(18) Uani 1 1 d . . . . .
H9 H 0.8611 0.2975 0.5431 0.038 Uiso 1 1 calc R . . . .
C10 C 0.8631(5) 0.2754(3) 0.6380(4) 0.0267(16) Uani 1 1 d . . . . .
C11 C 0.8596(5) 0.2311(3) 0.6760(4) 0.0255(16) Uani 1 1 d . . . . .
H11 H 0.8672 0.2352 0.7218 0.031 Uiso 1 1 calc R . . . .
C12 C 0.9510(6) 0.3442(3) 0.7084(4) 0.0335(18) Uani 1 1 d . . . . .
C13 C 0.9421(6) 0.3975(3) 0.7376(3) 0.0284(16) Uani 1 1 d . . . . .
C14 C 1.0270(7) 0.4230(3) 0.7849(4) 0.044(2) Uani 1 1 d . . . . .
H14 H 1.0917 0.4058 0.7977 0.053 Uiso 1 1 calc R . . . .
C15 C 0.9267(7) 0.4927(3) 0.7929(4) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.9183 0.5256 0.8117 0.056 Uiso 1 1 calc R . . . .
C16 C 0.8401(6) 0.4696(3) 0.7454(4) 0.0335(18) Uani 1 1 d . . . . .
H16 H 0.7763 0.4877 0.7326 0.040 Uiso 1 1 calc R . . . .
C17 C 0.745(2) 0.0017(11) 0.6120(17) 0.042(8) Uani 0.50(2) 1 d D U P A 1
H17 H 0.7834 -0.0131 0.6533 0.050 Uiso 0.50(2) 1 calc R . P A 1
C17A C 0.723(2) -0.0016(9) 0.6072(14) 0.024(6) Uani 0.50(2) 1 d D U P A 2
H17A H 0.7709 -0.0116 0.6481 0.029 Uiso 0.50(2) 1 calc R . P A 2
C18 C 0.7411(18) -0.0245(9) 0.5494(11) 0.047(6) Uani 0.50(2) 1 d . U P A 1
H18 H 0.7778 -0.0566 0.5527 0.056 Uiso 0.50(2) 1 calc R . P A 1
C18A C 0.7033(18) -0.0359(8) 0.5534(10) 0.041(5) Uani 0.50(2) 1 d . U P A 2
H18A H 0.7365 -0.0690 0.5582 0.050 Uiso 0.50(2) 1 calc R . P A 2
C19 C 0.6444(17) 0.0395(7) 0.4894(8) 0.038(5) Uani 0.50(2) 1 d . U P A 1
H19 H 0.6085 0.0545 0.4479 0.045 Uiso 0.50(2) 1 calc R . P A 1
C19A C 0.5900(19) 0.0287(8) 0.4904(10) 0.049(6) Uani 0.50(2) 1 d . U P A 2
H19A H 0.5431 0.0400 0.4498 0.058 Uiso 0.50(2) 1 calc R . P A 2
C20 C 0.6460(16) 0.0672(8) 0.5472(9) 0.027(5) Uani 0.50(2) 1 d D U P A 1
C20A C 0.6102(16) 0.0616(8) 0.5431(9) 0.026(4) Uani 0.50(2) 1 d D U P A 2
C21 C 0.5918(18) 0.1197(9) 0.5445(12) 0.032(5) Uani 0.50(2) 1 d D U P A 1
C21A C 0.5588(17) 0.1158(8) 0.5407(10) 0.022(4) Uani 0.50(2) 1 d . U P A 2
C22 C 0.5470(6) 0.1923(3) 0.5992(3) 0.0233(15) Uani 1 1 d . . . . .
C23 C 0.6013(5) 0.2358(3) 0.5845(3) 0.0217(14) Uani 1 1 d . . . . .
H23 H 0.6625 0.2302 0.5731 0.026 Uiso 1 1 calc R . . . .
C24 C 0.5644(5) 0.2878(3) 0.5868(3) 0.0194(13) Uani 1 1 d . . . . .
C25 C 0.4720(5) 0.2963(3) 0.6029(3) 0.0228(15) Uani 1 1 d . . . . .
H25 H 0.4468 0.3309 0.6042 0.027 Uiso 1 1 calc R . . . .
C26 C 0.4180(5) 0.2526(3) 0.6170(3) 0.0248(15) Uani 1 1 d . . . . .
H26 H 0.3565 0.2583 0.6281 0.030 Uiso 1 1 calc R . . . .
C27 C 0.4536(6) 0.2006(3) 0.6149(3) 0.0266(16) Uani 1 1 d . . . . .
H27 H 0.4160 0.1717 0.6238 0.032 Uiso 1 1 calc R . . . .
C28 C 0.6370(6) 0.3364(3) 0.5171(3) 0.0238(15) Uani 1 1 d . . . . .
C29 C 0.7075(5) 0.3807(3) 0.5094(3) 0.0234(15) Uani 1 1 d . . . . .
C30 C 0.7242(6) 0.3920(3) 0.4484(4) 0.0372(19) Uani 1 1 d . . . . .
H30 H 0.6891 0.3716 0.4108 0.045 Uiso 1 1 calc R . . . .
C31 C 0.8353(7) 0.4589(3) 0.4968(4) 0.053(2) Uani 1 1 d . . . . .
H31 H 0.8811 0.4862 0.4943 0.064 Uiso 1 1 calc R . . . .
C32 C 0.8181(6) 0.4487(3) 0.5582(4) 0.0377(19) Uani 1 1 d . . . . .
H32 H 0.8514 0.4699 0.5953 0.045 Uiso 1 1 calc R . . . .
C33 C 0.5008(6) 0.0216(3) 0.6723(4) 0.0296(17) Uani 1 1 d . . . . .
H33 H 0.5288 -0.0003 0.6459 0.036 Uiso 1 1 calc R . . . .
C34 C 0.4070(7) 0.0085(3) 0.6820(4) 0.0380(19) Uani 1 1 d . . . . .
H34 H 0.3730 -0.0223 0.6613 0.046 Uiso 1 1 calc R . . . .
C35 C 0.4157(6) 0.0812(3) 0.7466(4) 0.0346(18) Uani 1 1 d . . . . .
H35 H 0.3873 0.1032 0.7727 0.041 Uiso 1 1 calc R . . . .
C36 C 0.5096(5) 0.0955(3) 0.7383(3) 0.0225(15) Uani 1 1 d . . . . .
C37 C 0.5695(5) 0.1449(3) 0.7691(3) 0.0213(14) Uani 1 1 d . . . . .
C38 C 0.7096(5) 0.2011(3) 0.7809(3) 0.0228(15) Uani 1 1 d . . . . .
C39 C 0.8070(6) 0.2005(3) 0.8320(3) 0.0251(16) Uani 1 1 d . . . . .
H39 H 0.8359 0.1685 0.8521 0.030 Uiso 1 1 calc R . . . .
C40 C 0.8596(6) 0.2495(3) 0.8519(3) 0.0280(16) Uani 1 1 d . . . . .
H40 H 0.9223 0.2496 0.8870 0.034 Uiso 1 1 calc R . . . .
C41 C 0.8211(5) 0.2969(3) 0.8211(3) 0.0256(15) Uani 1 1 d . . . . .
H41 H 0.8578 0.3287 0.8344 0.031 Uiso 1 1 calc R . . . .
C42 C 0.7264(6) 0.2969(3) 0.7699(3) 0.0248(16) Uani 1 1 d . . . . .
C43 C 0.6699(5) 0.2494(2) 0.7515(3) 0.0180(13) Uani 1 1 d . . . . .
H43 H 0.6045 0.2502 0.7190 0.022 Uiso 1 1 calc R . . . .
C44 C 0.6004(6) 0.3646(3) 0.7407(3) 0.0240(15) Uani 1 1 d . . . . .
C45 C 0.5538(5) 0.4103(2) 0.6947(3) 0.0225(15) Uani 1 1 d . . . . .
C46 C 0.4586(6) 0.4323(3) 0.6913(4) 0.0322(17) Uani 1 1 d . . . . .
H46 H 0.4219 0.4185 0.7191 0.039 Uiso 1 1 calc R . . . .
C47 C 0.4730(6) 0.4909(3) 0.6124(4) 0.0341(18) Uani 1 1 d . . . . .
H47 H 0.4485 0.5201 0.5842 0.041 Uiso 1 1 calc R . . . .
C48 C 0.5679(6) 0.4681(3) 0.6129(3) 0.0298(17) Uani 1 1 d . . . . .
H48 H 0.6036 0.4815 0.5844 0.036 Uiso 1 1 calc R . . . .
O18 O 0.1840(9) 0.1876(4) 0.3899(6) 0.045(3) Uiso 0.5 1 d . . P . .
O19A O 0.0927(11) 0.2635(5) 0.2988(7) 0.052(5) Uiso 0.429(12) 1 d . . P B 2
O20 O 0.1897(15) 0.3998(7) 0.3345(10) 0.117(6) Uiso 0.5 1 d . . P . .
O14 O 0.1624(12) 0.3599(6) 0.5741(7) 0.073(4) Uiso 0.5 1 d . . P . .
C49 C 0.0617(16) 0.3602(9) 0.5482(9) 0.067(6) Uiso 0.5 1 d D . P . .
H49A H 0.0319 0.3944 0.5548 0.081 Uiso 0.5 1 calc R . P . .
H49B H 0.0291 0.3318 0.5666 0.081 Uiso 0.5 1 calc R . P . .
C50 C 0.0523(19) 0.3512(9) 0.4797(11) 0.099(8) Uiso 0.5 1 d D . P . .
H50A H -0.0175 0.3602 0.4511 0.119 Uiso 0.5 1 calc R . P . .
H50B H 0.0666 0.3140 0.4721 0.119 Uiso 0.5 1 calc R . P . .
C51 C 0.1295(13) 0.3860(7) 0.4661(8) 0.051(5) Uiso 0.5 1 d D . P . .
H51A H 0.1563 0.3724 0.4308 0.061 Uiso 0.5 1 calc R . P . .
H51B H 0.1049 0.4225 0.4562 0.061 Uiso 0.5 1 calc R . P . .
C52 C 0.1988(15) 0.3802(8) 0.5293(9) 0.064(6) Uiso 0.5 1 d D . P . .
H52A H 0.2563 0.3579 0.5259 0.076 Uiso 0.5 1 calc R . P . .
H52B H 0.2275 0.4152 0.5450 0.076 Uiso 0.5 1 calc R . P . .
O19 O 0.1189(9) 0.2844(4) 0.2053(6) 0.060(4) Uiso 0.571(12) 1 d . . P B 1
O15 O 0.0846(17) 0.1491(8) 0.4876(11) 0.143(8) Uiso 0.5 1 d D . P . .
C53 C 0.141(2) 0.1685(10) 0.5520(11) 0.103(9) Uiso 0.5 1 d D . P . .
H53A H 0.0982 0.1921 0.5699 0.124 Uiso 0.5 1 calc R . P . .
H53B H 0.2037 0.1875 0.5509 0.124 Uiso 0.5 1 calc R . P . .
C54 C 0.167(2) 0.1192(10) 0.5916(13) 0.107(9) Uiso 0.5 1 d D . P . .
H54A H 0.2344 0.1047 0.5919 0.128 Uiso 0.5 1 calc R . P . .
H54B H 0.1649 0.1238 0.6375 0.128 Uiso 0.5 1 calc R . P . .
C55 C 0.082(2) 0.0882(13) 0.5514(14) 0.153(13) Uiso 0.5 1 d D . P . .
H55A H 0.0331 0.0838 0.5775 0.184 Uiso 0.5 1 calc R . P . .
H55B H 0.1089 0.0529 0.5468 0.184 Uiso 0.5 1 calc R . P . .
C56 C 0.018(2) 0.1057(10) 0.4819(13) 0.106(9) Uiso 0.5 1 d D . P . .
H56A H 0.0199 0.0807 0.4466 0.127 Uiso 0.5 1 calc R . P . .
H56B H -0.0535 0.1156 0.4785 0.127 Uiso 0.5 1 calc R . P . .
O16 O 0.4397(5) 0.0969(3) 0.3565(3) 0.069(2) Uiso 1 1 d . . . . .
O17 O 0.2488(8) 0.1486(4) 0.2423(5) 0.042(3) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O4 2.269(5) . ?
Gd1 O5 2.255(4) 4_565 ?
Gd1 O7 2.449(5) . ?
Gd1 O8 2.375(5) . ?
Gd1 O9 2.441(5) . ?
Gd1 O10 2.365(5) . ?
Gd1 O11 2.522(5) . ?
Gd1 O12 2.529(5) . ?
Gd1 N19 2.956(6) . ?
Ni1 N1 2.095(6) . ?
Ni1 N2 2.078(6) . ?
Ni1 N3 2.07(2) . ?
Ni1 N3A 2.16(3) . ?
Ni1 N4 2.074(6) . ?
Ni1 N5 2.121(6) . ?
Ni1 N6 2.108(5) . ?
Ni2 N7 2.081(6) . ?
Ni2 N8 2.087(6) . ?
Ni2 N9 2.120(6) . ?
Ni2 N10 2.088(5) . ?
Ni2 N11 2.103(5) . ?
Ni2 N12 2.080(5) . ?
O1 C5 1.237(9) . ?
O2 C12 1.252(9) . ?
O3 C21A 1.19(2) . ?
O3A C21 1.36(2) . ?
O4 C28 1.258(8) . ?
O5 Gd1 2.254(4) 4_566 ?
O5 C37 1.264(7) . ?
O6 C44 1.272(8) . ?
O11 N19 1.263(7) . ?
O12 N19 1.277(8) . ?
O13 N19 1.225(8) . ?
N1 C1 1.312(8) . ?
N1 C4 1.358(9) . ?
N2 C5 1.309(9) . ?
N2 C6 1.436(8) . ?
N3 C17 1.341(14) . ?
N3 C20 1.341(15) . ?
N3A C17A 1.345(14) . ?
N3A C20A 1.326(15) . ?
N4 C21 1.26(2) . ?
N4 C21A 1.32(2) . ?
N4 C22 1.423(8) . ?
N5 C33 1.344(8) . ?
N5 C36 1.329(8) . ?
N6 C37 1.280(8) . ?
N6 C38 1.415(8) . ?
N7 C13 1.343(9) . ?
N7 C16 1.334(8) . ?
N8 C10 1.423(8) . ?
N8 C12 1.312(9) . ?
N9 C29 1.350(8) . ?
N9 C32 1.329(9) . ?
N10 C24 1.419(8) . ?
N10 C28 1.303(8) . ?
N11 C45 1.354(8) . ?
N11 C48 1.315(8) . ?
N12 C42 1.433(8) . ?
N12 C44 1.307(8) . ?
N13 C2 1.349(11) . ?
N13 C3 1.342(10) . ?
N14 C18 1.28(2) . ?
N14 C19 1.35(2) . ?
N14A C18A 1.36(3) . ?
N14A C19A 1.38(2) . ?
N15 C34 1.320(10) . ?
N15 C35 1.344(9) . ?
N16 C14 1.315(10) . ?
N16 C15 1.310(11) . ?
N17 C30 1.329(9) . ?
N17 C31 1.340(10) . ?
N18 C46 1.350(9) . ?
N18 C47 1.322(9) . ?
C1 C2 1.369(11) . ?
C3 C4 1.368(10) . ?
C4 C5 1.526(10) . ?
C6 C7 1.386(9) . ?
C6 C11 1.421(9) . ?
C7 C8 1.349(10) . ?
C8 C9 1.399(10) . ?
C9 C10 1.408(9) . ?
C10 C11 1.367(9) . ?
C12 C13 1.481(10) . ?
C13 C14 1.410(10) . ?
C15 C16 1.398(11) . ?
C17 C18 1.44(4) . ?
C17A C18A 1.37(3) . ?
C19 C20 1.38(2) . ?
C19A C20A 1.33(3) . ?
C20 C21 1.49(3) . ?
C20A C21A 1.51(3) . ?
C22 C23 1.392(9) . ?
C22 C27 1.399(9) . ?
C23 C24 1.395(9) . ?
C24 C25 1.392(9) . ?
C25 C26 1.389(9) . ?
C26 C27 1.388(9) . ?
C28 C29 1.492(9) . ?
C29 C30 1.381(9) . ?
C31 C32 1.386(10) . ?
C33 C34 1.372(10) . ?
C35 C36 1.368(10) . ?
C36 C37 1.502(9) . ?
C38 C39 1.411(9) . ?
C38 C43 1.383(8) . ?
C39 C40 1.409(9) . ?
C40 C41 1.370(9) . ?
C41 C42 1.386(10) . ?
C42 C43 1.396(9) . ?
C44 C45 1.497(9) . ?
C45 C46 1.370(10) . ?
C47 C48 1.388(10) . ?
O14 C49 1.29(2) . ?
O14 C52 1.28(2) . ?
C49 C50 1.408(17) . ?
C50 C51 1.441(16) . ?
C51 C52 1.368(16) . ?
O15 C53 1.408(17) . ?
O15 C56 1.384(17) . ?
C53 C54 1.461(17) . ?
C54 C55 1.424(18) . ?
C55 C56 1.502(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Gd1 O7 70.54(17) . . ?
O4 Gd1 O8 96.02(18) . . ?
O4 Gd1 O9 141.74(18) . . ?
O4 Gd1 O10 146.44(18) . . ?
O4 Gd1 O11 76.15(17) . . ?
O4 Gd1 O12 73.36(17) . . ?
O4 Gd1 N19 71.89(18) . . ?
O5 Gd1 O4 90.61(17) 4_565 . ?
O5 Gd1 O7 86.52(16) 4_565 . ?
O5 Gd1 O8 160.11(17) 4_565 . ?
O5 Gd1 O9 79.15(17) 4_565 . ?
O5 Gd1 O10 95.77(18) 4_565 . ?
O5 Gd1 O11 123.66(17) 4_565 . ?
O5 Gd1 O12 73.20(16) 4_565 . ?
O5 Gd1 N19 98.62(18) 4_565 . ?
O7 Gd1 O11 135.01(16) . . ?
O7 Gd1 O12 138.09(17) . . ?
O7 Gd1 N19 142.12(17) . . ?
O8 Gd1 O7 78.12(17) . . ?
O8 Gd1 O9 84.10(18) . . ?
O8 Gd1 O11 76.20(18) . . ?
O8 Gd1 O12 126.67(17) . . ?
O8 Gd1 N19 101.27(18) . . ?
O9 Gd1 O7 72.10(17) . . ?
O9 Gd1 O11 139.52(18) . . ?
O9 Gd1 O12 135.48(16) . . ?
O9 Gd1 N19 145.78(18) . . ?
O10 Gd1 O7 142.60(17) . . ?
O10 Gd1 O8 89.0(2) . . ?
O10 Gd1 O9 71.73(18) . . ?
O10 Gd1 O11 72.91(18) . . ?
O10 Gd1 O12 77.06(18) . . ?
O10 Gd1 N19 74.58(18) . . ?
O11 Gd1 O12 50.47(16) . . ?
O11 Gd1 N19 25.10(16) . . ?
O12 Gd1 N19 25.42(16) . . ?
N1 Ni1 N3A 94.9(5) . . ?
N1 Ni1 N5 93.2(2) . . ?
N1 Ni1 N6 93.1(2) . . ?
N2 Ni1 N1 78.3(2) . . ?
N2 Ni1 N3A 97.0(8) . . ?
N2 Ni1 N5 169.5(2) . . ?
N2 Ni1 N6 97.0(2) . . ?
N3 Ni1 N1 90.7(5) . . ?
N3 Ni1 N2 91.4(8) . . ?
N3 Ni1 N4 79.8(5) . . ?
N3 Ni1 N5 94.7(8) . . ?
N3 Ni1 N6 171.3(7) . . ?
N4 Ni1 N1 170.3(2) . . ?
N4 Ni1 N2 100.4(2) . . ?
N4 Ni1 N3A 75.6(5) . . ?
N4 Ni1 N5 89.1(2) . . ?
N4 Ni1 N6 96.6(2) . . ?
N5 Ni1 N3A 89.6(8) . . ?
N6 Ni1 N3A 165.0(7) . . ?
N6 Ni1 N5 77.3(2) . . ?
N7 Ni2 N8 78.4(2) . . ?
N7 Ni2 N9 93.7(2) . . ?
N7 Ni2 N10 171.3(2) . . ?
N7 Ni2 N11 95.5(2) . . ?
N8 Ni2 N9 88.9(2) . . ?
N8 Ni2 N10 97.6(2) . . ?
N8 Ni2 N11 173.1(2) . . ?
N10 Ni2 N9 78.5(2) . . ?
N10 Ni2 N11 89.0(2) . . ?
N11 Ni2 N9 94.6(2) . . ?
N12 Ni2 N7 91.6(2) . . ?
N12 Ni2 N8 97.9(2) . . ?
N12 Ni2 N9 172.1(2) . . ?
N12 Ni2 N10 96.6(2) . . ?
N12 Ni2 N11 79.1(2) . . ?
C28 O4 Gd1 147.8(5) . . ?
C37 O5 Gd1 171.7(4) . 4_566 ?
N19 O11 Gd1 97.0(4) . . ?
N19 O12 Gd1 96.3(4) . . ?
C1 N1 Ni1 129.1(5) . . ?
C1 N1 C4 116.8(6) . . ?
C4 N1 Ni1 114.0(4) . . ?
C5 N2 Ni1 118.0(5) . . ?
C5 N2 C6 116.6(6) . . ?
C6 N2 Ni1 124.8(4) . . ?
C17 N3 Ni1 131.5(19) . . ?
C20 N3 Ni1 112.0(15) . . ?
C20 N3 C17 116(2) . . ?
C17A N3A Ni1 125.8(17) . . ?
C20A N3A Ni1 114.6(16) . . ?
C20A N3A C17A 120(2) . . ?
C21 N4 Ni1 113.7(11) . . ?
C21 N4 C22 118.7(11) . . ?
C21A N4 Ni1 121.0(9) . . ?
C21A N4 C22 113.6(10) . . ?
C22 N4 Ni1 125.4(4) . . ?
C33 N5 Ni1 128.7(5) . . ?
C36 N5 Ni1 113.8(4) . . ?
C36 N5 C33 117.1(6) . . ?
C37 N6 Ni1 115.9(4) . . ?
C37 N6 C38 116.7(6) . . ?
C38 N6 Ni1 125.8(4) . . ?
C13 N7 Ni2 113.1(4) . . ?
C16 N7 Ni2 128.7(5) . . ?
C16 N7 C13 118.1(6) . . ?
C10 N8 Ni2 125.5(5) . . ?
C12 N8 Ni2 116.7(5) . . ?
C12 N8 C10 116.8(6) . . ?
C29 N9 Ni2 112.0(4) . . ?
C32 N9 Ni2 130.7(5) . . ?
C32 N9 C29 116.6(6) . . ?
C24 N10 Ni2 126.1(4) . . ?
C28 N10 Ni2 115.5(4) . . ?
C28 N10 C24 116.6(5) . . ?
C45 N11 Ni2 112.0(4) . . ?
C48 N11 Ni2 129.7(5) . . ?
C48 N11 C45 117.4(6) . . ?
C42 N12 Ni2 125.8(4) . . ?
C44 N12 Ni2 115.8(4) . . ?
C44 N12 C42 116.9(5) . . ?
C3 N13 C2 117.0(7) . . ?
C18 N14 C19 113.0(16) . . ?
C18A N14A C19A 115.9(18) . . ?
C34 N15 C35 114.4(7) . . ?
C15 N16 C14 116.6(7) . . ?
C30 N17 C31 115.7(7) . . ?
C47 N18 C46 114.6(7) . . ?
O11 N19 Gd1 57.9(3) . . ?
O11 N19 O12 116.0(6) . . ?
O12 N19 Gd1 58.3(3) . . ?
O13 N19 Gd1 176.9(6) . . ?
O13 N19 O11 122.0(7) . . ?
O13 N19 O12 122.1(7) . . ?
N1 C1 C2 122.7(8) . . ?
N13 C2 C1 120.8(8) . . ?
N13 C3 C4 121.3(8) . . ?
N1 C4 C3 121.3(7) . . ?
N1 C4 C5 115.9(6) . . ?
C3 C4 C5 122.8(7) . . ?
O1 C5 N2 129.9(7) . . ?
O1 C5 C4 116.9(7) . . ?
N2 C5 C4 113.1(7) . . ?
C7 C6 N2 121.6(6) . . ?
C7 C6 C11 118.8(6) . . ?
C11 C6 N2 119.5(6) . . ?
C8 C7 C6 120.3(7) . . ?
C7 C8 C9 121.3(7) . . ?
C8 C9 C10 119.8(7) . . ?
C9 C10 N8 120.2(6) . . ?
C11 C10 N8 121.1(6) . . ?
C11 C10 C9 118.5(6) . . ?
C10 C11 C6 121.2(6) . . ?
O2 C12 N8 129.1(7) . . ?
O2 C12 C13 117.6(7) . . ?
N8 C12 C13 113.3(7) . . ?
N7 C13 C12 118.1(6) . . ?
N7 C13 C14 119.0(7) . . ?
C14 C13 C12 122.9(7) . . ?
N16 C14 C13 123.2(8) . . ?
N16 C15 C16 122.7(8) . . ?
N7 C16 C15 120.4(8) . . ?
N3 C17 C18 118(3) . . ?
N3A C17A C18A 121(2) . . ?
N14 C18 C17 127(2) . . ?
N14A C18A C17A 120(2) . . ?
N14 C19 C20 123.6(16) . . ?
C20A C19A N14A 123.4(19) . . ?
N3 C20 C19 122.3(18) . . ?
N3 C20 C21 115.7(18) . . ?
C19 C20 C21 121.9(16) . . ?
N3A C20A C19A 120(2) . . ?
N3A C20A C21A 116.9(19) . . ?
C19A C20A C21A 123.3(17) . . ?
O3A C21 C20 116.8(18) . . ?
N4 C21 O3A 125.4(19) . . ?
N4 C21 C20 117.6(18) . . ?
O3 C21A N4 131.9(19) . . ?
O3 C21A C20A 116.4(19) . . ?
N4 C21A C20A 111.6(15) . . ?
C23 C22 N4 118.7(6) . . ?
C23 C22 C27 119.9(6) . . ?
C27 C22 N4 121.4(6) . . ?
C22 C23 C24 120.3(6) . . ?
C23 C24 N10 118.4(6) . . ?
C25 C24 N10 121.4(6) . . ?
C25 C24 C23 120.1(6) . . ?
C26 C25 C24 119.2(6) . . ?
C27 C26 C25 121.4(6) . . ?
C26 C27 C22 119.1(6) . . ?
O4 C28 N10 127.9(6) . . ?
O4 C28 C29 116.6(6) . . ?
N10 C28 C29 115.4(6) . . ?
N9 C29 C28 116.9(6) . . ?
N9 C29 C30 120.9(7) . . ?
C30 C29 C28 122.2(6) . . ?
N17 C30 C29 122.9(7) . . ?
N17 C31 C32 122.3(8) . . ?
N9 C32 C31 121.5(7) . . ?
N5 C33 C34 120.5(7) . . ?
N15 C34 C33 123.8(7) . . ?
N15 C35 C36 123.6(7) . . ?
N5 C36 C35 120.7(6) . . ?
N5 C36 C37 115.8(6) . . ?
C35 C36 C37 123.5(6) . . ?
O5 C37 N6 127.0(6) . . ?
O5 C37 C36 117.0(6) . . ?
N6 C37 C36 116.0(6) . . ?
C39 C38 N6 120.8(6) . . ?
C43 C38 N6 120.0(6) . . ?
C43 C38 C39 119.1(6) . . ?
C40 C39 C38 118.5(6) . . ?
C41 C40 C39 121.9(7) . . ?
C40 C41 C42 119.1(6) . . ?
C41 C42 N12 121.2(6) . . ?
C41 C42 C43 120.3(6) . . ?
C43 C42 N12 118.5(6) . . ?
C38 C43 C42 121.0(6) . . ?
O6 C44 N12 127.3(6) . . ?
O6 C44 C45 117.7(6) . . ?
N12 C44 C45 115.0(6) . . ?
N11 C45 C44 116.9(6) . . ?
N11 C45 C46 120.4(6) . . ?
C46 C45 C44 122.7(6) . . ?
N18 C46 C45 123.2(7) . . ?
N18 C47 C48 123.6(7) . . ?
N11 C48 C47 120.8(7) . . ?
C52 O14 C49 105.9(16) . . ?
O14 C49 C50 100.5(18) . . ?
C49 C50 C51 104.6(18) . . ?
C52 C51 C50 93.8(16) . . ?
O14 C52 C51 116.3(18) . . ?
C56 O15 C53 120(2) . . ?
O15 C53 C54 102(2) . . ?
C55 C54 C53 97(2) . . ?
C54 C55 C56 122(3) . . ?
O15 C56 C55 89(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_eb0029
_audit_block_doi                 10.5517/cc1jd6mr
_database_code_depnum_ccdc_archive 'CCDC 1411914'
_audit_update_record             
;
2015-07-09 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_compound_source        'Maria Angeles Palacios Lopez'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C132 H114 Mn3 N42 Ni4 O18, 2(C24 H20 P)'
_chemical_formula_sum            'C180 H144 Mn3 N42 Ni4 O18 P2'
_chemical_formula_weight         3644.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   18.9329(4)
_cell_length_b                   20.4784(4)
_cell_length_c                   25.2751(5)
_cell_angle_alpha                92.0192(16)
_cell_angle_beta                 98.6580(17)
_cell_angle_gamma                104.5213(16)
_cell_volume                     9351.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23186
_cell_measurement_theta_min      2.2333
_cell_measurement_theta_max      73.2796
_exptl_crystal_description       cuboid
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.1695
_exptl_crystal_size_mid          0.1164
_exptl_crystal_size_min          0.0895
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3758
_exptl_absorpt_coefficient_mu    2.772
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
Analytical numeric absorption correction using a multifaceted crystal
	model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3147
_diffrn_reflns_number            106563
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         73.44
_reflns_number_total             36654
_reflns_number_gt                22953
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'Shelxs Sheldrick'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_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.

#===============================================================================
The Following Model and Quality ALERTS were generated     - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure        !
043_ALERT_1_A Check Reported Molecular Weight ................    3644.97
044_ALERT_1_A Calculated and Reported Dx Differ ..............          ?
051_ALERT_1_B Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       9.33 Perc.
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ          ?
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?

Squeeze was used to treat the solvent region. Two molecules of what appeared to
be PPh4 could be seen but not refined

201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          4

These are atoms involved in disorder. Anisotropic refinement is not possible.

220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.79 Ratio
222_ALERT_3_B Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       4.62 Ratio
220_ALERT_2_C Large Non-Solvent    N     Ueq(max)/Ueq(min) ...       2.58 Ratio
220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.63 Ratio
230_ALERT_2_C Hirshfeld Test Diff for    O8E    --  C7E     ..       5.31 su
230_ALERT_2_C Hirshfeld Test Diff for    O18F   --  C17F    ..       6.75 su
232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni1    --  N1J     ..       5.57 su
369_ALERT_2_C Long   C(sp2)-C(sp2) Bond  C17G   -   C19G   ...       1.53 Ang.

There are some parts of the molecule with disorder and/or higher thermal motion.
Restraints have been applied to attempt to control this. Best solution is
presented.

910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          1
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         27
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600        987

Completeness meets IUCr requirements.

301_ALERT_3_G Note Main Residue  Disorder ....................       2.00 Perc.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      30.00 Deg.
              C16' -C14C -C16C    1.555   1.555   1.555
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      30.90 Deg.
              C20D -C19D -C20'    1.555   1.555   1.555
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ......      22.50 Deg.
              C23D -N24D -C23'    1.555   1.555   1.555

Disorder is confirmed.

860_ALERT_3_G Note: Number of Least-Squares Restraints .......         43
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety       C12B
720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........         30
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?

No action taken 
;
_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)+(0.1363P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         36654
_refine_ls_number_parameters     1807
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1650
_refine_ls_wR_factor_gt          0.1457
_refine_ls_goodness_of_fit_ref   0.709
_refine_ls_restrained_S_all      0.712
_refine_ls_shift/su_max          0.018
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.82347(3) 0.00330(3) 0.338001(19) 0.03138(11) Uani 1 1 d . . .
Ni2 Ni 0.24072(3) -0.29348(3) 0.41313(2) 0.03629(12) Uani 1 1 d . . .
Ni3 Ni 0.19377(3) -0.47380(2) 0.16988(2) 0.03232(12) Uani 1 1 d . . .
Ni5 Ni 0.78005(3) -0.04423(2) 0.063968(19) 0.03067(11) Uani 1 1 d . . .
Mn1 Mn -0.03843(3) -0.23562(3) 0.31637(2) 0.04154(13) Uani 1 1 d . . .
Mn2 Mn 0.49615(3) -0.10990(3) 0.30636(2) 0.03397(11) Uani 1 1 d . . .
Mn3 Mn 0.94895(3) 0.25088(2) 0.103342(19) 0.03241(11) Uani 1 1 d . . .
C1A C -0.2415(3) -0.3554(4) 0.3452(3) 0.105(2) Uani 1 1 d U . .
H1A1 H -0.2245 -0.3869 0.3691 0.157 Uiso 1 1 calc R . .
H1A2 H -0.2867 -0.3796 0.3209 0.157 Uiso 1 1 calc R . .
H1A3 H -0.2519 -0.3191 0.3666 0.157 Uiso 1 1 calc R . .
C2A C -0.1819(2) -0.3252(2) 0.3125(2) 0.0665(12) Uani 1 1 d U . .
O3A O -0.11734(14) -0.29983(14) 0.34127(11) 0.0533(6) Uani 1 1 d . . .
C4A C -0.1967(2) -0.3274(3) 0.2576(2) 0.0698(13) Uani 1 1 d . . .
H4A H -0.2469 -0.3441 0.2411 0.084 Uiso 1 1 calc R . .
C5A C -0.1436(2) -0.3069(2) 0.22334(17) 0.0549(9) Uani 1 1 d . . .
C6A C -0.1686(3) -0.3250(2) 0.16396(18) 0.0713(13) Uani 1 1 d . . .
H6A1 H -0.1533 -0.2847 0.1444 0.107 Uiso 1 1 calc R . .
H6A2 H -0.2226 -0.3418 0.1565 0.107 Uiso 1 1 calc R . .
H6A3 H -0.1462 -0.3601 0.1524 0.107 Uiso 1 1 calc R . .
N7A N -0.07527(15) -0.27312(14) 0.24206(11) 0.0410(6) Uani 1 1 d . . .
C8A C -0.01748(19) -0.25460(16) 0.20857(13) 0.0399(7) Uani 1 1 d . . .
H8A1 H -0.0399 -0.2600 0.1701 0.048 Uiso 1 1 calc R . .
H8A2 H 0.0168 -0.2840 0.2143 0.048 Uiso 1 1 calc R . .
C9A C 0.02397(19) -0.18091(17) 0.22487(14) 0.0422(7) Uani 1 1 d . . .
H9A1 H 0.0717 -0.1701 0.2114 0.051 Uiso 1 1 calc R . .
H9A2 H -0.0057 -0.1506 0.2093 0.051 Uiso 1 1 calc R . .
N10A N 0.03690(15) -0.17128(13) 0.28361(11) 0.0398(6) Uani 1 1 d . . .
C11A C 0.08814(19) -0.11918(17) 0.30808(16) 0.0468(8) Uani 1 1 d . . .
C12A C 0.1373(2) -0.07187(18) 0.27677(18) 0.0553(10) Uani 1 1 d . . .
H12A H 0.1638 -0.0973 0.2570 0.083 Uiso 1 1 calc R . .
H12B H 0.1730 -0.0368 0.3015 0.083 Uiso 1 1 calc R . .
H12C H 0.1071 -0.0506 0.2514 0.083 Uiso 1 1 calc R . .
C13A C 0.0992(2) -0.1048(2) 0.36461(17) 0.0572(10) Uani 1 1 d . . .
H13A H 0.1396 -0.0678 0.3796 0.069 Uiso 1 1 calc R . .
C14A C 0.0578(2) -0.1387(2) 0.39933(16) 0.0572(10) Uani 1 1 d . . .
O15A O 0.00137(15) -0.19149(13) 0.38651(10) 0.0527(6) Uani 1 1 d . . .
C16A C 0.0732(3) -0.1150(3) 0.45857(17) 0.0736(13) Uani 1 1 d . . .
H16A H 0.0344 -0.0943 0.4669 0.110 Uiso 1 1 calc R . .
H16B H 0.1213 -0.0817 0.4669 0.110 Uiso 1 1 calc R . .
H16C H 0.0738 -0.1538 0.4801 0.110 Uiso 1 1 calc R . .
C1B C 0.3476(2) 0.0100(2) 0.2697(2) 0.0756(14) Uani 1 1 d . . .
H1B1 H 0.3322 0.0054 0.3050 0.113 Uiso 1 1 calc R . .
H1B2 H 0.3038 0.0031 0.2419 0.113 Uiso 1 1 calc R . .
H1B3 H 0.3799 0.0554 0.2686 0.113 Uiso 1 1 calc R . .
C2B C 0.38894(19) -0.0421(2) 0.25985(18) 0.0552(10) Uani 1 1 d . . .
O3B O 0.44446(12) -0.04074(12) 0.29750(10) 0.0451(5) Uani 1 1 d . . .
C4B C 0.3691(2) -0.0836(2) 0.21432(18) 0.0606(11) Uani 1 1 d . . .
H4B H 0.3266 -0.0801 0.1905 0.073 Uiso 1 1 calc R . .
C5B C 0.40646(19) -0.13273(18) 0.19846(15) 0.0501(9) Uani 1 1 d . . .
C6B C 0.3841(3) -0.1670(2) 0.14284(18) 0.0776(15) Uani 1 1 d . . .
H6B1 H 0.4268 -0.1577 0.1241 0.116 Uiso 1 1 calc R . .
H6B2 H 0.3446 -0.1498 0.1232 0.116 Uiso 1 1 calc R . .
H6B3 H 0.3661 -0.2159 0.1449 0.116 Uiso 1 1 calc R . .
N7B N 0.46043(14) -0.14643(14) 0.23144(11) 0.0401(6) Uani 1 1 d . . .
C8B C 0.50213(18) -0.19343(18) 0.21514(14) 0.0428(7) Uani 1 1 d . . .
H8B1 H 0.5495 -0.1679 0.2053 0.051 Uiso 1 1 calc R . .
H8B2 H 0.4731 -0.2237 0.1837 0.051 Uiso 1 1 calc R . .
C9B C 0.51666(18) -0.23459(16) 0.26283(12) 0.0389(7) Uani 1 1 d . . .
H9B1 H 0.4709 -0.2690 0.2665 0.047 Uiso 1 1 calc R . .
H9B2 H 0.5551 -0.2581 0.2575 0.047 Uiso 1 1 calc R . .
N10B N 0.54164(13) -0.18778(12) 0.31120(10) 0.0336(5) Uani 1 1 d . . .
C11B C 0.57984(16) -0.20253(15) 0.35444(12) 0.0340(6) Uani 1 1 d . . .
C12B C 0.60194(19) -0.26871(17) 0.35503(14) 0.0446(8) Uani 1 1 d . . .
H12D H 0.5574 -0.3066 0.3480 0.067 Uiso 1 1 calc R . .
H12E H 0.6302 -0.2717 0.3903 0.067 Uiso 1 1 calc R . .
H12F H 0.6325 -0.2706 0.3272 0.067 Uiso 1 1 calc R . .
C13B C 0.60271(19) -0.15847(17) 0.40191(12) 0.0400(7) Uani 1 1 d . . .
H13B H 0.6350 -0.1709 0.4300 0.048 Uiso 1 1 calc R . .
C14B C 0.58269(18) -0.09955(17) 0.41127(12) 0.0397(7) Uani 1 1 d . . .
O15B O 0.53580(12) -0.07712(11) 0.37936(9) 0.0376(5) Uani 1 1 d . . .
C16B C 0.6165(3) -0.0554(2) 0.46198(14) 0.0627(11) Uani 1 1 d . . .
H16D H 0.6490 -0.0131 0.4534 0.094 Uiso 1 1 calc R . .
H16E H 0.6453 -0.0789 0.4863 0.094 Uiso 1 1 calc R . .
H16F H 0.5772 -0.0452 0.4794 0.094 Uiso 1 1 calc R . .
C1C C 1.1540(3) 0.2160(3) 0.0886(2) 0.0826(15) Uani 1 1 d . . .
H1C1 H 1.1313 0.1767 0.0629 0.124 Uiso 1 1 calc R . .
H1C2 H 1.1921 0.2052 0.1151 0.124 Uiso 1 1 calc R . .
H1C3 H 1.1766 0.2546 0.0696 0.124 Uiso 1 1 calc R . .
C2C C 1.0965(2) 0.23316(18) 0.11641(17) 0.0517(9) Uani 1 1 d . . .
O3C O 1.04213(12) 0.24687(10) 0.08380(9) 0.0397(5) Uani 1 1 d . . .
C4C C 1.1037(2) 0.2371(2) 0.17085(18) 0.0600(10) Uani 1 1 d . . .
H4C H 1.1441 0.2235 0.1900 0.072 Uiso 1 1 calc R . .
C5C C 1.05649(19) 0.2594(2) 0.20156(14) 0.0482(8) Uani 1 1 d . . .
C6C C 1.0809(2) 0.2727(3) 0.26213(16) 0.0720(13) Uani 1 1 d . . .
H6C1 H 1.0986 0.3216 0.2714 0.108 Uiso 1 1 calc R . .
H6C2 H 1.1209 0.2512 0.2735 0.108 Uiso 1 1 calc R . .
H6C3 H 1.0389 0.2539 0.2803 0.108 Uiso 1 1 calc R . .
N7C N 0.99418(14) 0.27130(12) 0.17946(10) 0.0346(5) Uani 1 1 d . . .
C8C C 0.9510(2) 0.30262(18) 0.21023(15) 0.0491(8) Uani 1 1 d . . .
H8C1 H 0.9635 0.3520 0.2068 0.059 Uiso 1 1 calc R . .
H8C2 H 0.9619 0.2946 0.2487 0.059 Uiso 1 1 calc R . .
C9C C 0.8714(2) 0.27234(19) 0.18905(16) 0.0502(9) Uani 1 1 d . . .
H9C1 H 0.8551 0.2273 0.2028 0.060 Uiso 1 1 calc R . .
H9C2 H 0.8415 0.3015 0.2011 0.060 Uiso 1 1 calc R . .
N10C N 0.86066(15) 0.26572(13) 0.12993(12) 0.0425(6) Uani 1 1 d . . .
C11C C 0.7962(2) 0.26215(19) 0.1014(2) 0.0607(11) Uani 1 1 d U . .
C12C C 0.7334(2) 0.2756(3) 0.1274(3) 0.0925(18) Uani 1 1 d U . .
H12G H 0.7299 0.2512 0.1599 0.139 Uiso 1 1 calc R . .
H12H H 0.6868 0.2601 0.1022 0.139 Uiso 1 1 calc R . .
H12I H 0.7431 0.3242 0.1368 0.139 Uiso 1 1 calc R . .
C13C C 0.7813(2) 0.2483(2) 0.0465(2) 0.0781(16) Uani 1 1 d . A .
H13C H 0.7321 0.2449 0.0295 0.094 Uiso 1 1 calc R . .
C14C C 0.8312(3) 0.2386(2) 0.01324(17) 0.0757(16) Uani 1 1 d DU . .
O15C O 0.89979(15) 0.24048(12) 0.03025(9) 0.0530(6) Uani 1 1 d . A .
C16C C 0.8249(8) 0.2135(6) -0.0488(3) 0.070(3) Uiso 0.484(19) 1 d PDU A 1
H16G H 0.8616 0.2454 -0.0652 0.106 Uiso 0.484(19) 1 calc PR A 1
H16H H 0.7751 0.2114 -0.0678 0.106 Uiso 0.484(19) 1 calc PR A 1
H16I H 0.8340 0.1685 -0.0511 0.106 Uiso 0.484(19) 1 calc PR A 1
C16' C 0.7972(5) 0.2362(4) -0.0433(3) 0.048(3) Uani 0.516(19) 1 d PDU A 2
H16X H 0.8204 0.2777 -0.0589 0.072 Uiso 0.516(19) 1 calc PR A 2
H16Y H 0.7442 0.2322 -0.0455 0.072 Uiso 0.516(19) 1 calc PR A 2
H16Z H 0.8045 0.1970 -0.0631 0.072 Uiso 0.516(19) 1 calc PR A 2
N1D N 0.24734(16) -0.55151(13) 0.15473(10) 0.0390(6) Uani 1 1 d . . .
C2D C 0.2757(2) -0.56559(18) 0.11178(14) 0.0529(9) Uani 1 1 d . . .
H2D H 0.2685 -0.5400 0.0817 0.063 Uiso 1 1 calc R . .
N3D N 0.3135(3) -0.61216(18) 0.10683(15) 0.0752(12) Uani 1 1 d . . .
C4D C 0.3201(4) -0.6488(2) 0.14943(19) 0.0876(18) Uani 1 1 d . . .
H4D H 0.3448 -0.6836 0.1475 0.105 Uiso 1 1 calc R . .
C5D C 0.2931(3) -0.6386(2) 0.19552(17) 0.0669(12) Uani 1 1 d . . .
H5D H 0.2991 -0.6651 0.2252 0.080 Uiso 1 1 calc R . .
C6D C 0.2567(2) -0.58828(15) 0.19693(13) 0.0417(7) Uani 1 1 d . . .
C7D C 0.2244(2) -0.57263(16) 0.24556(13) 0.0409(7) Uani 1 1 d . . .
O8D O 0.23611(16) -0.60414(12) 0.28588(10) 0.0529(6) Uani 1 1 d . . .
N9D N 0.18755(14) -0.52594(12) 0.23857(10) 0.0330(5) Uani 1 1 d . . .
C10D C 0.15668(18) -0.50765(15) 0.28334(12) 0.0350(6) Uani 1 1 d . . .
C11D C 0.08143(19) -0.52704(16) 0.28364(14) 0.0423(7) Uani 1 1 d . . .
H11D H 0.0490 -0.5539 0.2541 0.051 Uiso 1 1 calc R . .
C12D C 0.0535(2) -0.50698(18) 0.32756(17) 0.0516(9) Uani 1 1 d . . .
H12J H 0.0021 -0.5226 0.3286 0.062 Uiso 1 1 calc R . .
C13D C 0.0986(2) -0.46524(17) 0.36934(15) 0.0488(8) Uani 1 1 d . . .
H13D H 0.0782 -0.4509 0.3984 0.059 Uiso 1 1 calc R . .
C14D C 0.17432(19) -0.44393(15) 0.36914(13) 0.0384(7) Uani 1 1 d . . .
C15D C 0.20342(18) -0.46599(14) 0.32727(12) 0.0345(6) Uani 1 1 d . . .
H15D H 0.2554 -0.4531 0.3279 0.041 Uiso 1 1 calc R . .
N16D N 0.22168(17) -0.39783(14) 0.41107(11) 0.0423(6) Uani 1 1 d . . .
C17D C 0.2611(3) -0.4233(2) 0.44748(15) 0.0617(12) Uani 1 1 d . B .
O18D O 0.2638(2) -0.48403(15) 0.45248(12) 0.0888(12) Uani 1 1 d . . .
C19D C 0.3073(3) -0.3718(2) 0.49096(16) 0.0739(14) Uani 1 1 d DU . .
C20D C 0.3301(4) -0.3961(4) 0.5406(3) 0.0534(16) Uiso 0.593(6) 1 d PDU B 1
H20D H 0.3230 -0.4428 0.5458 0.064 Uiso 0.593(6) 1 calc PR B 1
C21D C 0.3642(3) -0.3446(3) 0.5814(3) 0.0509(16) Uiso 0.593(6) 1 d PDU B 1
H21D H 0.3858 -0.3567 0.6148 0.061 Uiso 0.593(6) 1 calc PR B 1
N22D N 0.3675(2) -0.2789(2) 0.57508(19) 0.0440(13) Uiso 0.593(6) 1 d PDU B 1
C23D C 0.3391(2) -0.2665(3) 0.5265(2) 0.0371(12) Uiso 0.593(6) 1 d PDU B 1
H23D H 0.3417 -0.2202 0.5221 0.044 Uiso 0.593(6) 1 calc PR B 1
C20' C 0.3675(6) -0.3787(6) 0.5325(4) 0.064(3) Uiso 0.407(6) 1 d PD B 2
H20' H 0.3728 -0.4230 0.5380 0.076 Uiso 0.407(6) 1 calc PR B 2
C21' C 0.4173(7) -0.3251(6) 0.5645(5) 0.076(3) Uiso 0.407(6) 1 d PD B 2
H21' H 0.4526 -0.3344 0.5921 0.091 Uiso 0.407(6) 1 calc PR B 2
N22' N 0.4169(5) -0.2603(5) 0.5574(4) 0.071(3) Uiso 0.407(6) 1 d PD B 2
C23' C 0.3649(5) -0.2488(6) 0.5190(3) 0.055(2) Uiso 0.407(6) 1 d PD B 2
H23' H 0.3635 -0.2035 0.5134 0.066 Uiso 0.407(6) 1 calc PR B 2
N24D N 0.30866(19) -0.30615(16) 0.48438(11) 0.0574(9) Uani 1 1 d DU B .
C5E C 0.0184(2) -0.3182(2) 0.44086(16) 0.0537(9) Uani 1 1 d . . .
H5E H -0.0274 -0.3248 0.4175 0.064 Uiso 1 1 calc R . .
C2E C 0.1465(2) -0.3017(2) 0.50785(15) 0.0543(9) Uani 1 1 d . . .
H2E H 0.1921 -0.2961 0.5313 0.065 Uiso 1 1 calc R . .
N3E N 0.0855(2) -0.31195(19) 0.52991(14) 0.0645(9) Uani 1 1 d . . .
C4E C 0.0219(3) -0.3199(2) 0.49588(19) 0.0683(12) Uani 1 1 d . . .
H4E H -0.0228 -0.3270 0.5102 0.082 Uiso 1 1 calc R . .
N1E N 0.14895(17) -0.29868(14) 0.45527(11) 0.0436(6) Uani 1 1 d . . .
C6E C 0.0846(2) -0.30666(16) 0.42132(14) 0.0427(8) Uani 1 1 d . . .
C7E C 0.08884(18) -0.30066(16) 0.36278(13) 0.0381(7) Uani 1 1 d . . .
O8E O 0.02860(12) -0.30710(11) 0.33091(9) 0.0401(5) Uani 1 1 d . . .
N9E N 0.15572(14) -0.29002(12) 0.35111(10) 0.0335(5) Uani 1 1 d . . .
C10E C 0.16303(16) -0.28672(15) 0.29630(12) 0.0330(6) Uani 1 1 d . . .
C11E C 0.19712(16) -0.22640(14) 0.27597(12) 0.0328(6) Uani 1 1 d . . .
H11E H 0.2138 -0.1856 0.2986 0.039 Uiso 1 1 calc R . .
C12E C 0.20644(17) -0.22635(15) 0.22305(13) 0.0353(6) Uani 1 1 d . . .
H12K H 0.2291 -0.1850 0.2094 0.042 Uiso 1 1 calc R . .
C13E C 0.18355(17) -0.28534(14) 0.18874(12) 0.0344(6) Uani 1 1 d . . .
H13E H 0.1915 -0.2845 0.1525 0.041 Uiso 1 1 calc R . .
C14E C 0.14878(16) -0.34554(14) 0.20876(12) 0.0338(6) Uani 1 1 d . . .
C15E C 0.13769(16) -0.34571(15) 0.26161(12) 0.0324(6) Uani 1 1 d . . .
H15E H 0.1124 -0.3865 0.2746 0.039 Uiso 1 1 calc R . .
N16E N 0.12712(14) -0.40851(12) 0.17676(10) 0.0339(5) Uani 1 1 d . . .
C17E C 0.0615(2) -0.42228(17) 0.14564(16) 0.0523(10) Uani 1 1 d . . .
O18E O 0.01689(18) -0.38622(13) 0.13754(15) 0.0882(13) Uani 1 1 d . . .
C19E C 0.0376(2) -0.49385(17) 0.12144(15) 0.0490(9) Uani 1 1 d . . .
C20E C -0.0321(2) -0.52163(19) 0.09329(19) 0.0665(13) Uani 1 1 d . . .
H20E H -0.0649 -0.4944 0.0830 0.080 Uiso 1 1 calc R . .
C21E C -0.0529(2) -0.59112(17) 0.08038(16) 0.0526(9) Uani 1 1 d . . .
H21E H -0.1016 -0.6118 0.0623 0.063 Uiso 1 1 calc R . .
N22E N -0.00639(15) -0.62919(13) 0.09268(11) 0.0400(6) Uani 1 1 d . . .
C23E C 0.06297(18) -0.59781(14) 0.11566(12) 0.0344(6) Uani 1 1 d . . .
H23E H 0.0974 -0.6245 0.1218 0.041 Uiso 1 1 calc R . .
N24E N 0.08730(14) -0.53194(12) 0.13058(10) 0.0351(5) Uani 1 1 d . . .
N1F N 0.21994(15) -0.43238(12) 0.09715(10) 0.0362(6) Uani 1 1 d . . .
C2F C 0.1823(2) -0.44546(17) 0.04677(13) 0.0443(8) Uani 1 1 d . . .
H2F H 0.1338 -0.4747 0.0425 0.053 Uiso 1 1 calc R . .
N3F N 0.20543(18) -0.42191(15) 0.00224(11) 0.0475(7) Uani 1 1 d . . .
C4F C 0.2736(2) -0.3813(2) 0.00947(15) 0.0518(9) Uani 1 1 d . . .
H4F H 0.2935 -0.3637 -0.0210 0.062 Uiso 1 1 calc R . .
C5F C 0.3169(2) -0.36373(19) 0.06019(14) 0.0486(8) Uani 1 1 d . . .
H5F H 0.3651 -0.3341 0.0644 0.058 Uiso 1 1 calc R . .
C6F C 0.28816(18) -0.39011(15) 0.10357(13) 0.0359(6) Uani 1 1 d . . .
C7F C 0.33121(17) -0.37329(15) 0.15997(13) 0.0372(7) Uani 1 1 d . . .
O8F O 0.39415(13) -0.33356(14) 0.16458(10) 0.0541(6) Uani 1 1 d . . .
N9F N 0.29607(13) -0.40416(12) 0.19677(10) 0.0321(5) Uani 1 1 d . . .
C10F C 0.33208(16) -0.38748(14) 0.25116(12) 0.0320(6) Uani 1 1 d . . .
C11F C 0.37575(17) -0.42615(15) 0.27641(13) 0.0375(7) Uani 1 1 d . . .
H11F H 0.3852 -0.4625 0.2567 0.045 Uiso 1 1 calc R . .
C12F C 0.40574(18) -0.41192(17) 0.33035(14) 0.0422(7) Uani 1 1 d . . .
H12L H 0.4365 -0.4380 0.3471 0.051 Uiso 1 1 calc R . .
C13F C 0.39121(18) -0.35951(16) 0.36054(13) 0.0386(7) Uani 1 1 d . . .
H13F H 0.4112 -0.3507 0.3976 0.046 Uiso 1 1 calc R . .
C14F C 0.34777(16) -0.32096(14) 0.33602(12) 0.0325(6) Uani 1 1 d . . .
C15F C 0.32028(16) -0.33348(14) 0.28084(11) 0.0300(6) Uani 1 1 d . . .
H15F H 0.2932 -0.3048 0.2634 0.036 Uiso 1 1 calc R . .
N16F N 0.32668(14) -0.27151(12) 0.36723(10) 0.0333(5) Uani 1 1 d . . .
C17F C 0.35380(16) -0.20717(15) 0.36001(12) 0.0339(6) Uani 1 1 d . . .
O18F O 0.39826(12) -0.18209(11) 0.32980(10) 0.0420(5) Uani 1 1 d . . .
C19F C 0.32535(17) -0.15939(16) 0.39304(12) 0.0364(7) Uani 1 1 d . . .
C20F C 0.3491(2) -0.09029(16) 0.39240(13) 0.0419(7) Uani 1 1 d . . .
H20F H 0.3851 -0.0701 0.3713 0.050 Uiso 1 1 calc R . .
C21F C 0.3187(2) -0.05119(16) 0.42362(13) 0.0457(8) Uani 1 1 d . . .
H21F H 0.3344 -0.0034 0.4234 0.055 Uiso 1 1 calc R . .
N22F N 0.26821(17) -0.07749(14) 0.45412(11) 0.0451(7) Uani 1 1 d . . .
C23F C 0.24865(19) -0.14489(16) 0.45180(13) 0.0389(7) Uani 1 1 d . . .
H23F H 0.2126 -0.1651 0.4728 0.047 Uiso 1 1 calc R . .
N24F N 0.27436(15) -0.18696(13) 0.42308(10) 0.0363(6) Uani 1 1 d . . .
N1G N 0.81604(13) -0.07276(13) 0.39077(9) 0.0338(5) Uani 1 1 d . . .
C2G C 0.78837(18) -0.07734(18) 0.43640(12) 0.0398(7) Uani 1 1 d . . .
H2G H 0.7709 -0.0403 0.4476 0.048 Uiso 1 1 calc R . .
N3G N 0.78279(15) -0.12846(16) 0.46775(10) 0.0436(7) Uani 1 1 d . . .
C4G C 0.80764(19) -0.1802(2) 0.45093(13) 0.0472(8) Uani 1 1 d . . .
H4G H 0.8044 -0.2183 0.4717 0.057 Uiso 1 1 calc R . .
C5G C 0.8378(2) -0.1800(2) 0.40440(13) 0.0485(9) Uani 1 1 d . . .
H5G H 0.8557 -0.2169 0.3935 0.058 Uiso 1 1 calc R . .
C6G C 0.84127(17) -0.12488(17) 0.37431(12) 0.0382(7) Uani 1 1 d . . .
C7G C 0.87360(16) -0.11730(16) 0.32300(11) 0.0333(6) Uani 1 1 d . . .
O8G O 0.88947(14) -0.16846(13) 0.30329(9) 0.0461(6) Uani 1 1 d . . .
N9G N 0.88077(13) -0.05750(13) 0.30466(9) 0.0327(5) Uani 1 1 d . . .
C10G C 0.91184(15) -0.04510(16) 0.25665(11) 0.0317(6) Uani 1 1 d . . .
C11G C 0.97745(16) 0.00570(16) 0.25793(12) 0.0337(6) Uani 1 1 d . . .
H11G H 1.0033 0.0292 0.2911 0.040 Uiso 1 1 calc R . .
C12G C 1.00421(16) 0.02134(16) 0.21120(12) 0.0348(6) Uani 1 1 d . . .
H12M H 1.0500 0.0542 0.2127 0.042 Uiso 1 1 calc R . .
C13G C 0.96595(16) -0.00973(15) 0.16151(11) 0.0311(6) Uani 1 1 d . . .
H13G H 0.9843 0.0028 0.1294 0.037 Uiso 1 1 calc R . .
C14G C 0.89997(15) -0.05968(14) 0.16011(11) 0.0277(5) Uani 1 1 d . . .
C15G C 0.87433(16) -0.07834(15) 0.20730(11) 0.0299(6) Uani 1 1 d . . .
H15G H 0.8309 -0.1140 0.2061 0.036 Uiso 1 1 calc R . .
N16G N 0.85344(13) -0.08883(12) 0.11014(9) 0.0293(5) Uani 1 1 d . . .
C17G C 0.85639(16) -0.14944(14) 0.09285(11) 0.0311(6) Uani 1 1 d . . .
O18G O 0.90011(12) -0.18317(11) 0.10887(9) 0.0402(5) Uani 1 1 d . . .
C19G C 0.79296(17) -0.18148(15) 0.04734(12) 0.0336(6) Uani 1 1 d . . .
C20G C 0.77213(19) -0.24995(16) 0.03276(13) 0.0397(7) Uani 1 1 d . . .
H20G H 0.7994 -0.2792 0.0490 0.048 Uiso 1 1 calc R . .
C21G C 0.7108(2) -0.27482(17) -0.00596(14) 0.0445(8) Uani 1 1 d . . .
H21G H 0.6958 -0.3220 -0.0159 0.053 Uiso 1 1 calc R . .
N22G N 0.67175(17) -0.23534(15) -0.03003(12) 0.0480(7) Uani 1 1 d . . .
C23G C 0.6958(2) -0.16961(18) -0.01404(13) 0.0471(8) Uani 1 1 d . . .
H23G H 0.6690 -0.1404 -0.0310 0.056 Uiso 1 1 calc R . .
N24G N 0.75428(15) -0.14092(13) 0.02373(10) 0.0359(6) Uani 1 1 d . . .
N1H N 0.92249(14) 0.06164(14) 0.38613(10) 0.0392(6) Uani 1 1 d . . .
C2H C 0.96590(19) 0.0431(2) 0.42639(13) 0.0470(8) Uani 1 1 d . . .
H2H H 0.9479 -0.0003 0.4388 0.056 Uiso 1 1 calc R . .
N3H N 1.03177(18) 0.0796(2) 0.45059(13) 0.0631(9) Uani 1 1 d . . .
C4H C 1.0542(3) 0.1419(3) 0.43343(17) 0.0811(16) Uani 1 1 d . . .
H4H H 1.1002 0.1706 0.4504 0.097 Uiso 1 1 calc R . .
C5H C 1.0130(3) 0.1660(3) 0.39195(15) 0.0733(14) Uani 1 1 d . . .
H5H H 1.0294 0.2103 0.3808 0.088 Uiso 1 1 calc R . .
C6H C 0.9469(2) 0.1219(2) 0.36774(14) 0.0520(9) Uani 1 1 d . . .
C7H C 0.9020(2) 0.14002(17) 0.31810(13) 0.0448(8) Uani 1 1 d . . .
O8H O 0.92038(18) 0.19803(13) 0.30270(10) 0.0645(8) Uani 1 1 d . . .
N9H N 0.84866(14) 0.08721(13) 0.29534(10) 0.0356(6) Uani 1 1 d . . .
C10H C 0.80959(16) 0.09522(14) 0.24400(12) 0.0314(6) Uani 1 1 d . . .
C11H C 0.74476(18) 0.11671(16) 0.23812(13) 0.0383(7) Uani 1 1 d . . .
H11H H 0.7263 0.1291 0.2688 0.046 Uiso 1 1 calc R . .
C12H C 0.70769(18) 0.11979(16) 0.18726(14) 0.0406(7) Uani 1 1 d . . .
H12N H 0.6643 0.1357 0.1834 0.049 Uiso 1 1 calc R . .
C13H C 0.73211(16) 0.10030(15) 0.14174(12) 0.0340(6) Uani 1 1 d . . .
H13H H 0.7051 0.1019 0.1071 0.041 Uiso 1 1 calc R . .
C14H C 0.79653(16) 0.07841(14) 0.14712(12) 0.0310(6) Uani 1 1 d . . .
C15H C 0.83546(16) 0.07696(14) 0.19843(11) 0.0299(6) Uani 1 1 d . . .
H15H H 0.8802 0.0633 0.2023 0.036 Uiso 1 1 calc R . .
N16H N 0.82012(13) 0.05335(12) 0.10116(9) 0.0288(5) Uani 1 1 d . . .
C17H C 0.88165(16) 0.09109(14) 0.08738(11) 0.0299(6) Uani 1 1 d . . .
O18H O 0.92228(12) 0.14591(10) 0.11005(8) 0.0351(4) Uani 1 1 d . . .
C19H C 0.90220(16) 0.06273(14) 0.03829(11) 0.0299(6) Uani 1 1 d . . .
C20H C 0.95732(17) 0.09898(16) 0.01203(12) 0.0357(6) Uani 1 1 d . . .
H20H H 0.9855 0.1433 0.0251 0.043 Uiso 1 1 calc R . .
C21H C 0.96930(18) 0.06781(17) -0.03387(13) 0.0405(7) Uani 1 1 d . . .
H21H H 1.0064 0.0919 -0.0525 0.049 Uiso 1 1 calc R . .
N22H N 0.93081(16) 0.00481(14) -0.05348(11) 0.0415(6) Uani 1 1 d . . .
C23H C 0.87927(17) -0.02568(16) -0.02568(11) 0.0344(6) Uani 1 1 d . . .
H23H H 0.8514 -0.0701 -0.0388 0.041 Uiso 1 1 calc R . .
N24H N 0.86267(14) -0.00039(12) 0.01867(9) 0.0325(5) Uani 1 1 d . . .
N1J N 0.75088(14) 0.05143(13) 0.37322(10) 0.0354(5) Uani 1 1 d . . .
C2J C 0.7695(2) 0.10675(17) 0.40754(13) 0.0424(7) Uani 1 1 d . . .
H2J H 0.8182 0.1185 0.4275 0.051 Uiso 1 1 calc R . .
N3J N 0.72631(19) 0.14655(17) 0.41616(12) 0.0542(8) Uani 1 1 d . . .
C4J C 0.6583(2) 0.1286(2) 0.38805(15) 0.0565(10) Uani 1 1 d . . .
H4J H 0.6261 0.1566 0.3922 0.068 Uiso 1 1 calc R . .
C5J C 0.6319(2) 0.07070(18) 0.35285(13) 0.0434(8) Uani 1 1 d . . .
H5J H 0.5823 0.0577 0.3346 0.052 Uiso 1 1 calc R . .
C6J C 0.68129(16) 0.03324(15) 0.34574(11) 0.0322(6) Uani 1 1 d . . .
C7J C 0.66209(16) -0.02538(14) 0.30384(11) 0.0302(6) Uani 1 1 d . . .
O8J O 0.59548(11) -0.04562(10) 0.28114(8) 0.0335(4) Uani 1 1 d . . .
N9J N 0.71913(13) -0.04552(11) 0.29364(9) 0.0287(5) Uani 1 1 d . . .
C10J C 0.70614(15) -0.09213(15) 0.24757(11) 0.0300(6) Uani 1 1 d . . .
C11J C 0.70687(15) -0.15949(14) 0.25158(11) 0.0299(6) Uani 1 1 d . . .
H11J H 0.7133 -0.1771 0.2857 0.036 Uiso 1 1 calc R . .
C12J C 0.69809(16) -0.20060(14) 0.20504(12) 0.0321(6) Uani 1 1 d . . .
H12O H 0.6976 -0.2469 0.2076 0.039 Uiso 1 1 calc R . .
C13J C 0.69003(16) -0.17549(15) 0.15485(11) 0.0322(6) Uani 1 1 d . . .
H13J H 0.6849 -0.2041 0.1234 0.039 Uiso 1 1 calc R . .
C14J C 0.68951(15) -0.10809(15) 0.15098(12) 0.0318(6) Uani 1 1 d . . .
C15J C 0.69605(15) -0.06722(14) 0.19735(11) 0.0287(6) Uani 1 1 d . . .
H15J H 0.6936 -0.0217 0.1947 0.034 Uiso 1 1 calc R . .
N16J N 0.68865(14) -0.07696(13) 0.10085(10) 0.0342(5) Uani 1 1 d . . .
C17J C 0.62750(19) -0.0593(2) 0.08175(14) 0.0499(9) Uani 1 1 d . . .
O18J O 0.56504(14) -0.07439(17) 0.09609(11) 0.0664(8) Uani 1 1 d . . .
C19J C 0.63779(19) -0.0145(2) 0.03555(15) 0.0500(9) Uani 1 1 d . . .
C20J C 0.5884(2) 0.0243(3) 0.01985(19) 0.0725(14) Uani 1 1 d . . .
H20J H 0.5470 0.0235 0.0371 0.087 Uiso 1 1 calc R . .
C21J C 0.6031(2) 0.0637(3) -0.0222(2) 0.0785(15) Uani 1 1 d . . .
H21J H 0.5699 0.0900 -0.0344 0.094 Uiso 1 1 calc R . .
N22J N 0.66209(18) 0.0670(2) -0.04680(15) 0.0651(10) Uani 1 1 d . . .
C23J C 0.7082(2) 0.03165(19) -0.02663(15) 0.0507(9) Uani 1 1 d . . .
H23J H 0.7518 0.0358 -0.0419 0.061 Uiso 1 1 calc R . .
N24J N 0.69913(15) -0.00938(14) 0.01331(10) 0.0400(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N9H 2.054(3) . ?
Ni1 N9G 2.078(2) . ?
Ni1 N1G 2.078(3) . ?
Ni1 N9J 2.103(2) . ?
Ni1 N1H 2.123(3) . ?
Ni1 N1J 2.154(3) . ?
Ni2 N16D 2.074(3) . ?
Ni2 N9E 2.088(3) . ?
Ni2 N16F 2.106(3) . ?
Ni2 N24F 2.108(3) . ?
Ni2 N24D 2.114(3) . ?
Ni2 N1E 2.153(3) . ?
Ni3 N9D 2.073(2) . ?
Ni3 N16E 2.075(3) . ?
Ni3 N9F 2.097(2) . ?
Ni3 N1F 2.126(3) . ?
Ni3 N24E 2.140(3) . ?
Ni3 N1D 2.143(3) . ?
Ni5 N16J 2.064(3) . ?
Ni5 N16H 2.084(2) . ?
Ni5 N16G 2.086(2) . ?
Ni5 N24G 2.102(3) . ?
Ni5 N24H 2.115(3) . ?
Ni5 N24J 2.125(3) . ?
Mn1 O15A 1.916(3) . ?
Mn1 O3A 1.927(3) . ?
Mn1 N7A 1.959(3) . ?
Mn1 N10A 1.986(3) . ?
Mn1 O8G 2.169(2) 1_455 ?
Mn1 O8E 2.172(2) . ?
Mn2 O15B 1.914(2) . ?
Mn2 O3B 1.914(2) . ?
Mn2 N7B 1.966(3) . ?
Mn2 N10B 1.993(3) . ?
Mn2 O8J 2.203(2) . ?
Mn2 O18F 2.234(2) . ?
Mn3 O15C 1.918(2) . ?
Mn3 O3C 1.922(2) . ?
Mn3 N7C 1.969(3) . ?
Mn3 N10C 1.979(3) . ?
Mn3 O18H 2.101(2) . ?
Mn3 N22E 2.427(3) 1_665 ?
C1A C2A 1.518(6) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
C2A O3A 1.296(5) . ?
C2A C4A 1.371(7) . ?
C4A C5A 1.419(6) . ?
C4A H4A 0.9500 . ?
C5A N7A 1.311(5) . ?
C5A C6A 1.507(6) . ?
C6A H6A1 0.9800 . ?
C6A H6A2 0.9800 . ?
C6A H6A3 0.9800 . ?
N7A C8A 1.466(4) . ?
C8A C9A 1.526(5) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C9A N10A 1.466(4) . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
N10A C11A 1.310(4) . ?
C11A C13A 1.422(5) . ?
C11A C12A 1.501(5) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A C14A 1.358(6) . ?
C13A H13A 0.9500 . ?
C14A O15A 1.307(5) . ?
C14A C16A 1.520(6) . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C1B C2B 1.507(6) . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
C2B O3B 1.302(4) . ?
C2B C4B 1.352(6) . ?
C4B C5B 1.445(6) . ?
C4B H4B 0.9500 . ?
C5B N7B 1.312(4) . ?
C5B C6B 1.500(6) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
N7B C8B 1.473(5) . ?
C8B C9B 1.525(5) . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C9B N10B 1.467(4) . ?
C9B H9B1 0.9900 . ?
C9B H9B2 0.9900 . ?
N10B C11B 1.305(4) . ?
C11B C13B 1.419(4) . ?
C11B C12B 1.515(4) . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B C14B 1.375(5) . ?
C13B H13B 0.9500 . ?
C14B O15B 1.290(4) . ?
C14B C16B 1.501(5) . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C1C C2C 1.486(5) . ?
C1C H1C1 0.9800 . ?
C1C H1C2 0.9800 . ?
C1C H1C3 0.9800 . ?
C2C O3C 1.313(4) . ?
C2C C4C 1.360(6) . ?
C4C C5C 1.414(6) . ?
C4C H4C 0.9500 . ?
C5C N7C 1.311(4) . ?
C5C C6C 1.525(5) . ?
C6C H6C1 0.9800 . ?
C6C H6C2 0.9800 . ?
C6C H6C3 0.9800 . ?
N7C C8C 1.451(4) . ?
C8C C9C 1.485(5) . ?
C8C H8C1 0.9900 . ?
C8C H8C2 0.9900 . ?
C9C N10C 1.474(5) . ?
C9C H9C1 0.9900 . ?
C9C H9C2 0.9900 . ?
N10C C11C 1.305(5) . ?
C11C C13C 1.377(7) . ?
C11C C12C 1.518(7) . ?
C12C H12G 0.9800 . ?
C12C H12H 0.9800 . ?
C12C H12I 0.9800 . ?
C13C C14C 1.400(8) . ?
C13C H13C 0.9500 . ?
C14C O15C 1.296(6) . ?
C14C C16' 1.469(6) . ?
C14C C16C 1.610(8) . ?
C16C H16G 0.9800 . ?
C16C H16H 0.9800 . ?
C16C H16I 0.9800 . ?
C16' H16X 0.9800 . ?
C16' H16Y 0.9800 . ?
C16' H16Z 0.9800 . ?
N1D C2D 1.335(4) . ?
N1D C6D 1.343(4) . ?
C2D N3D 1.340(5) . ?
C2D H2D 0.9500 . ?
N3D C4D 1.342(6) . ?
C4D C5D 1.370(6) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.379(5) . ?
C5D H5D 0.9500 . ?
C6D C7D 1.510(5) . ?
C7D O8D 1.246(4) . ?
C7D N9D 1.320(4) . ?
N9D C10D 1.429(4) . ?
C10D C11D 1.381(5) . ?
C10D C15D 1.415(4) . ?
C11D C12D 1.391(5) . ?
C11D H11D 0.9500 . ?
C12D C13D 1.369(5) . ?
C12D H12J 0.9500 . ?
C13D C14D 1.391(5) . ?
C13D H13D 0.9500 . ?
C14D C15D 1.376(4) . ?
C14D N16D 1.427(4) . ?
C15D H15D 0.9500 . ?
N16D C17D 1.304(5) . ?
C17D O18D 1.266(4) . ?
C17D C19D 1.501(6) . ?
C19D N24D 1.354(5) . ?
C19D C20D 1.412(8) . ?
C19D C20' 1.467(12) . ?
C20D C21D 1.405(9) . ?
C20D H20D 0.9500 . ?
C21D N22D 1.349(8) . ?
C21D H21D 0.9500 . ?
N22D C23D 1.323(7) . ?
C23D N24D 1.282(6) . ?
C23D H23D 0.9500 . ?
C20' C21' 1.393(16) . ?
C20' H20' 0.9500 . ?
C21' N22' 1.346(15) . ?
C21' H21' 0.9500 . ?
N22' C23' 1.348(14) . ?
C23' N24D 1.516(11) . ?
C23' H23' 0.9500 . ?
C5E C4E 1.384(6) . ?
C5E C6E 1.384(5) . ?
C5E H5E 0.9500 . ?
C2E N3E 1.330(5) . ?
C2E N1E 1.340(4) . ?
C2E H2E 0.9500 . ?
N3E C4E 1.340(6) . ?
C4E H4E 0.9500 . ?
N1E C6E 1.350(5) . ?
C6E C7E 1.501(5) . ?
C7E O8E 1.268(4) . ?
C7E N9E 1.310(4) . ?
N9E C10E 1.415(4) . ?
C10E C11E 1.397(4) . ?
C10E C15E 1.402(4) . ?
C11E C12E 1.375(4) . ?
C11E H11E 0.9500 . ?
C12E C13E 1.396(4) . ?
C12E H12K 0.9500 . ?
C13E C14E 1.395(4) . ?
C13E H13E 0.9500 . ?
C14E C15E 1.383(4) . ?
C14E N16E 1.431(4) . ?
C15E H15E 0.9500 . ?
N16E C17E 1.325(4) . ?
C17E O18E 1.253(4) . ?
C17E C19E 1.499(5) . ?
C19E N24E 1.365(4) . ?
C19E C20E 1.372(5) . ?
C20E C21E 1.391(5) . ?
C20E H20E 0.9500 . ?
C21E N22E 1.326(4) . ?
C21E H21E 0.9500 . ?
N22E C23E 1.340(4) . ?
N22E Mn3 2.427(3) 1_445 ?
C23E N24E 1.332(4) . ?
C23E H23E 0.9500 . ?
N1F C2F 1.345(4) . ?
N1F C6F 1.345(4) . ?
C2F N3F 1.332(4) . ?
C2F H2F 0.9500 . ?
N3F C4F 1.331(5) . ?
C4F C5F 1.396(5) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.365(5) . ?
C5F H5F 0.9500 . ?
C6F C7F 1.513(4) . ?
C7F O8F 1.249(4) . ?
C7F N9F 1.313(4) . ?
N9F C10F 1.428(4) . ?
C10F C11F 1.387(4) . ?
C10F C15F 1.397(4) . ?
C11F C12F 1.386(5) . ?
C11F H11F 0.9500 . ?
C12F C13F 1.401(4) . ?
C12F H12L 0.9500 . ?
C13F C14F 1.375(4) . ?
C13F H13F 0.9500 . ?
C14F C15F 1.404(4) . ?
C14F N16F 1.431(4) . ?
C15F H15F 0.9500 . ?
N16F C17F 1.319(4) . ?
C17F O18F 1.249(4) . ?
C17F C19F 1.512(4) . ?
C19F N24F 1.344(4) . ?
C19F C20F 1.374(4) . ?
C20F C21F 1.386(5) . ?
C20F H20F 0.9500 . ?
C21F N22F 1.338(5) . ?
C21F H21F 0.9500 . ?
N22F C23F 1.333(4) . ?
C23F N24F 1.334(4) . ?
C23F H23F 0.9500 . ?
N1G C2G 1.334(4) . ?
N1G C6G 1.351(4) . ?
C2G N3G 1.328(4) . ?
C2G H2G 0.9500 . ?
N3G C4G 1.343(5) . ?
C4G C5G 1.382(5) . ?
C4G H4G 0.9500 . ?
C5G C6G 1.377(5) . ?
C5G H5G 0.9500 . ?
C6G C7G 1.512(4) . ?
C7G O8G 1.266(4) . ?
C7G N9G 1.307(4) . ?
O8G Mn1 2.168(2) 1_655 ?
N9G C10G 1.430(4) . ?
C10G C15G 1.398(4) . ?
C10G C11G 1.401(4) . ?
C11G C12G 1.371(4) . ?
C11G H11G 0.9500 . ?
C12G C13G 1.395(4) . ?
C12G H12M 0.9500 . ?
C13G C14G 1.397(4) . ?
C13G H13G 0.9500 . ?
C14G C15G 1.385(4) . ?
C14G N16G 1.441(3) . ?
C15G H15G 0.9500 . ?
N16G C17G 1.319(4) . ?
C17G O18G 1.238(4) . ?
C17G C19G 1.527(4) . ?
C19G N24G 1.338(4) . ?
C19G C20G 1.378(4) . ?
C20G C21G 1.375(5) . ?
C20G H20G 0.9500 . ?
C21G N22G 1.331(5) . ?
C21G H21G 0.9500 . ?
N22G C23G 1.335(4) . ?
C23G N24G 1.341(4) . ?
C23G H23G 0.9500 . ?
N1H C6H 1.331(5) . ?
N1H C2H 1.337(4) . ?
C2H N3H 1.327(4) . ?
C2H H2H 0.9500 . ?
N3H C4H 1.347(6) . ?
C4H C5H 1.391(7) . ?
C4H H4H 0.9500 . ?
C5H C6H 1.387(5) . ?
C5H H5H 0.9500 . ?
C6H C7H 1.517(5) . ?
C7H O8H 1.245(4) . ?
C7H N9H 1.324(4) . ?
N9H C10H 1.430(4) . ?
C10H C15H 1.392(4) . ?
C10H C11H 1.394(4) . ?
C11H C12H 1.380(5) . ?
C11H H11H 0.9500 . ?
C12H C13H 1.385(4) . ?
C12H H12N 0.9500 . ?
C13H C14H 1.391(4) . ?
C13H H13H 0.9500 . ?
C14H C15H 1.397(4) . ?
C14H N16H 1.429(4) . ?
C15H H15H 0.9500 . ?
N16H C17H 1.329(4) . ?
C17H O18H 1.253(3) . ?
C17H C19H 1.495(4) . ?
C19H N24H 1.355(4) . ?
C19H C20H 1.391(4) . ?
C20H C21H 1.380(4) . ?
C20H H20H 0.9500 . ?
C21H N22H 1.347(4) . ?
C21H H21H 0.9500 . ?
N22H C23H 1.330(4) . ?
C23H N24H 1.331(4) . ?
C23H H23H 0.9500 . ?
N1J C2J 1.341(4) . ?
N1J C6J 1.348(4) . ?
C2J N3J 1.326(4) . ?
C2J H2J 0.9500 . ?
N3J C4J 1.329(5) . ?
C4J C5J 1.393(5) . ?
C4J H4J 0.9500 . ?
C5J C6J 1.376(4) . ?
C5J H5J 0.9500 . ?
C6J C7J 1.507(4) . ?
C7J O8J 1.263(3) . ?
C7J N9J 1.305(4) . ?
N9J C10J 1.430(4) . ?
C10J C15J 1.389(4) . ?
C10J C11J 1.390(4) . ?
C11J C12J 1.386(4) . ?
C11J H11J 0.9500 . ?
C12J C13J 1.387(4) . ?
C12J H12O 0.9500 . ?
C13J C14J 1.389(4) . ?
C13J H13J 0.9500 . ?
C14J C15J 1.387(4) . ?
C14J N16J 1.438(4) . ?
C15J H15J 0.9500 . ?
N16J C17J 1.325(4) . ?
C17J O18J 1.257(4) . ?
C17J C19J 1.517(5) . ?
C19J N24J 1.348(5) . ?
C19J C20J 1.394(6) . ?
C20J C21J 1.376(6) . ?
C20J H20J 0.9500 . ?
C21J N22J 1.346(6) . ?
C21J H21J 0.9500 . ?
N22J C23J 1.325(5) . ?
C23J N24J 1.339(4) . ?
C23J H23J 0.9500 . ?

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
N9H Ni1 N9G 100.69(10) . . ?
N9H Ni1 N1G 169.33(10) . . ?
N9G Ni1 N1G 79.06(10) . . ?
N9H Ni1 N9J 99.20(10) . . ?
N9G Ni1 N9J 95.84(9) . . ?
N1G Ni1 N9J 91.42(9) . . ?
N9H Ni1 N1H 78.45(11) . . ?
N9G Ni1 N1H 91.18(10) . . ?
N1G Ni1 N1H 90.88(10) . . ?
N9J Ni1 N1H 172.92(10) . . ?
N9H Ni1 N1J 86.77(10) . . ?
N9G Ni1 N1J 170.81(10) . . ?
N1G Ni1 N1J 94.61(10) . . ?
N9J Ni1 N1J 77.53(9) . . ?
N1H Ni1 N1J 95.61(10) . . ?
N16D Ni2 N9E 97.44(10) . . ?
N16D Ni2 N16F 99.38(10) . . ?
N9E Ni2 N16F 96.33(10) . . ?
N16D Ni2 N24F 171.61(11) . . ?
N9E Ni2 N24F 90.84(10) . . ?
N16F Ni2 N24F 78.32(10) . . ?
N16D Ni2 N24D 78.07(12) . . ?
N9E Ni2 N24D 168.13(12) . . ?
N16F Ni2 N24D 95.25(11) . . ?
N24F Ni2 N24D 94.04(11) . . ?
N16D Ni2 N1E 90.23(11) . . ?
N9E Ni2 N1E 77.85(11) . . ?
N16F Ni2 N1E 169.40(10) . . ?
N24F Ni2 N1E 92.79(11) . . ?
N24D Ni2 N1E 91.09(12) . . ?
N9D Ni3 N16E 103.69(10) . . ?
N9D Ni3 N9F 97.48(10) . . ?
N16E Ni3 N9F 97.65(10) . . ?
N9D Ni3 N1F 166.31(10) . . ?
N16E Ni3 N1F 89.86(10) . . ?
N9F Ni3 N1F 78.50(10) . . ?
N9D Ni3 N24E 93.18(10) . . ?
N16E Ni3 N24E 77.03(10) . . ?
N9F Ni3 N24E 168.98(10) . . ?
N1F Ni3 N24E 91.73(10) . . ?
N9D Ni3 N1D 77.65(10) . . ?
N16E Ni3 N1D 170.81(10) . . ?
N9F Ni3 N1D 91.15(10) . . ?
N1F Ni3 N1D 89.29(10) . . ?
N24E Ni3 N1D 93.84(10) . . ?
N16J Ni5 N16H 99.18(10) . . ?
N16J Ni5 N16G 99.36(9) . . ?
N16H Ni5 N16G 97.64(9) . . ?
N16J Ni5 N24G 88.33(10) . . ?
N16H Ni5 N24G 172.09(10) . . ?
N16G Ni5 N24G 78.57(10) . . ?
N16J Ni5 N24H 169.96(10) . . ?
N16H Ni5 N24H 78.08(9) . . ?
N16G Ni5 N24H 90.60(9) . . ?
N24G Ni5 N24H 94.93(10) . . ?
N16J Ni5 N24J 78.72(10) . . ?
N16H Ni5 N24J 88.43(10) . . ?
N16G Ni5 N24J 173.87(10) . . ?
N24G Ni5 N24J 95.51(10) . . ?
N24H Ni5 N24J 91.51(10) . . ?
O15A Mn1 O3A 93.45(12) . . ?
O15A Mn1 N7A 174.90(12) . . ?
O3A Mn1 N7A 91.12(12) . . ?
O15A Mn1 N10A 91.77(12) . . ?
O3A Mn1 N10A 174.39(12) . . ?
N7A Mn1 N10A 83.58(12) . . ?
O15A Mn1 O8G 89.95(10) . 1_455 ?
O3A Mn1 O8G 88.67(10) . 1_455 ?
N7A Mn1 O8G 87.90(10) . 1_455 ?
N10A Mn1 O8G 89.28(10) . 1_455 ?
O15A Mn1 O8E 90.37(10) . . ?
O3A Mn1 O8E 88.05(10) . . ?
N7A Mn1 O8E 92.05(10) . . ?
N10A Mn1 O8E 93.98(10) . . ?
O8G Mn1 O8E 176.72(9) 1_455 . ?
O15B Mn2 O3B 91.39(10) . . ?
O15B Mn2 N7B 176.40(11) . . ?
O3B Mn2 N7B 91.99(11) . . ?
O15B Mn2 N10B 92.93(10) . . ?
O3B Mn2 N10B 174.55(10) . . ?
N7B Mn2 N10B 83.77(11) . . ?
O15B Mn2 O8J 89.54(9) . . ?
O3B Mn2 O8J 92.27(9) . . ?
N7B Mn2 O8J 89.09(10) . . ?
N10B Mn2 O8J 91.09(9) . . ?
O15B Mn2 O18F 92.28(9) . . ?
O3B Mn2 O18F 91.80(9) . . ?
N7B Mn2 O18F 88.86(10) . . ?
N10B Mn2 O18F 84.72(9) . . ?
O8J Mn2 O18F 175.51(8) . . ?
O15C Mn3 O3C 93.49(11) . . ?
O15C Mn3 N7C 172.83(12) . . ?
O3C Mn3 N7C 91.14(10) . . ?
O15C Mn3 N10C 91.74(13) . . ?
O3C Mn3 N10C 172.32(10) . . ?
N7C Mn3 N10C 83.14(12) . . ?
O15C Mn3 O18H 92.41(9) . . ?
O3C Mn3 O18H 89.67(9) . . ?
N7C Mn3 O18H 93.08(9) . . ?
N10C Mn3 O18H 95.73(10) . . ?
O15C Mn3 N22E 88.02(10) . 1_665 ?
O3C Mn3 N22E 83.47(10) . 1_665 ?
N7C Mn3 N22E 87.08(10) . 1_665 ?
N10C Mn3 N22E 91.10(11) . 1_665 ?
O18H Mn3 N22E 173.14(9) . 1_665 ?
C2A C1A H1A1 109.5 . . ?
C2A C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
C2A C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
O3A C2A C4A 124.7(4) . . ?
O3A C2A C1A 113.7(4) . . ?
C4A C2A C1A 121.5(4) . . ?
C2A O3A Mn1 123.7(3) . . ?
C2A C4A C5A 125.7(4) . . ?
C2A C4A H4A 117.2 . . ?
C5A C4A H4A 117.2 . . ?
N7A C5A C4A 121.9(4) . . ?
N7A C5A C6A 120.6(4) . . ?
C4A C5A C6A 117.5(4) . . ?
C5A C6A H6A1 109.5 . . ?
C5A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C5A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C5A N7A C8A 123.7(3) . . ?
C5A N7A Mn1 125.1(3) . . ?
C8A N7A Mn1 111.1(2) . . ?
N7A C8A C9A 107.3(3) . . ?
N7A C8A H8A1 110.3 . . ?
C9A C8A H8A1 110.3 . . ?
N7A C8A H8A2 110.3 . . ?
C9A C8A H8A2 110.3 . . ?
H8A1 C8A H8A2 108.5 . . ?
N10A C9A C8A 108.2(3) . . ?
N10A C9A H9A1 110.1 . . ?
C8A C9A H9A1 110.1 . . ?
N10A C9A H9A2 110.1 . . ?
C8A C9A H9A2 110.1 . . ?
H9A1 C9A H9A2 108.4 . . ?
C11A N10A C9A 119.8(3) . . ?
C11A N10A Mn1 127.0(3) . . ?
C9A N10A Mn1 112.7(2) . . ?
N10A C11A C13A 122.0(4) . . ?
N10A C11A C12A 120.6(3) . . ?
C13A C11A C12A 117.5(3) . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C14A C13A C11A 126.4(4) . . ?
C14A C13A H13A 116.8 . . ?
C11A C13A H13A 116.8 . . ?
O15A C14A C13A 125.7(4) . . ?
O15A C14A C16A 113.6(4) . . ?
C13A C14A C16A 120.7(4) . . ?
C14A O15A Mn1 127.1(3) . . ?
C14A C16A H16A 109.5 . . ?
C14A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C14A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C2B C1B H1B1 109.5 . . ?
C2B C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
C2B C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
O3B C2B C4B 125.5(4) . . ?
O3B C2B C1B 113.9(4) . . ?
C4B C2B C1B 120.6(4) . . ?
C2B O3B Mn2 125.3(3) . . ?
C2B C4B C5B 126.2(3) . . ?
C2B C4B H4B 116.9 . . ?
C5B C4B H4B 116.9 . . ?
N7B C5B C4B 121.0(4) . . ?
N7B C5B C6B 119.9(4) . . ?
C4B C5B C6B 119.0(3) . . ?
C5B C6B H6B1 109.5 . . ?
C5B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C5B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C5B N7B C8B 122.0(3) . . ?
C5B N7B Mn2 126.6(3) . . ?
C8B N7B Mn2 111.45(19) . . ?
N7B C8B C9B 107.3(3) . . ?
N7B C8B H8B1 110.3 . . ?
C9B C8B H8B1 110.3 . . ?
N7B C8B H8B2 110.3 . . ?
C9B C8B H8B2 110.3 . . ?
H8B1 C8B H8B2 108.5 . . ?
N10B C9B C8B 107.9(3) . . ?
N10B C9B H9B1 110.1 . . ?
C8B C9B H9B1 110.1 . . ?
N10B C9B H9B2 110.1 . . ?
C8B C9B H9B2 110.1 . . ?
H9B1 C9B H9B2 108.4 . . ?
C11B N10B C9B 122.0(3) . . ?
C11B N10B Mn2 125.2(2) . . ?
C9B N10B Mn2 111.94(19) . . ?
N10B C11B C13B 122.6(3) . . ?
N10B C11B C12B 120.0(3) . . ?
C13B C11B C12B 117.5(3) . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C14B C13B C11B 126.4(3) . . ?
C14B C13B H13B 116.8 . . ?
C11B C13B H13B 116.8 . . ?
O15B C14B C13B 125.4(3) . . ?
O15B C14B C16B 114.5(3) . . ?
C13B C14B C16B 120.1(3) . . ?
C14B O15B Mn2 126.2(2) . . ?
C14B C16B H16D 109.5 . . ?
C14B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C14B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C2C C1C H1C1 109.5 . . ?
C2C C1C H1C2 109.5 . . ?
H1C1 C1C H1C2 109.5 . . ?
C2C C1C H1C3 109.5 . . ?
H1C1 C1C H1C3 109.5 . . ?
H1C2 C1C H1C3 109.5 . . ?
O3C C2C C4C 124.9(3) . . ?
O3C C2C C1C 113.8(4) . . ?
C4C C2C C1C 121.2(4) . . ?
C2C O3C Mn3 124.6(2) . . ?
C2C C4C C5C 126.0(3) . . ?
C2C C4C H4C 117.0 . . ?
C5C C4C H4C 117.0 . . ?
N7C C5C C4C 122.2(3) . . ?
N7C C5C C6C 119.3(4) . . ?
C4C C5C C6C 118.5(3) . . ?
C5C C6C H6C1 109.5 . . ?
C5C C6C H6C2 109.5 . . ?
H6C1 C6C H6C2 109.5 . . ?
C5C C6C H6C3 109.5 . . ?
H6C1 C6C H6C3 109.5 . . ?
H6C2 C6C H6C3 109.5 . . ?
C5C N7C C8C 121.8(3) . . ?
C5C N7C Mn3 125.7(2) . . ?
C8C N7C Mn3 112.5(2) . . ?
N7C C8C C9C 108.2(3) . . ?
N7C C8C H8C1 110.1 . . ?
C9C C8C H8C1 110.1 . . ?
N7C C8C H8C2 110.1 . . ?
C9C C8C H8C2 110.1 . . ?
H8C1 C8C H8C2 108.4 . . ?
N10C C9C C8C 109.1(3) . . ?
N10C C9C H9C1 109.9 . . ?
C8C C9C H9C1 109.9 . . ?
N10C C9C H9C2 109.9 . . ?
C8C C9C H9C2 109.9 . . ?
H9C1 C9C H9C2 108.3 . . ?
C11C N10C C9C 120.9(3) . . ?
C11C N10C Mn3 126.8(3) . . ?
C9C N10C Mn3 111.8(2) . . ?
N10C C11C C13C 122.9(4) . . ?
N10C C11C C12C 121.0(5) . . ?
C13C C11C C12C 116.1(4) . . ?
C11C C12C H12G 109.5 . . ?
C11C C12C H12H 109.5 . . ?
H12G C12C H12H 109.5 . . ?
C11C C12C H12I 109.5 . . ?
H12G C12C H12I 109.5 . . ?
H12H C12C H12I 109.5 . . ?
C11C C13C C14C 126.7(4) . . ?
C11C C13C H13C 116.6 . . ?
C14C C13C H13C 116.6 . . ?
O15C C14C C13C 124.2(4) . . ?
O15C C14C C16' 125.5(6) . . ?
C13C C14C C16' 109.7(6) . . ?
O15C C14C C16C 99.9(7) . . ?
C13C C14C C16C 135.4(6) . . ?
C16' C14C C16C 29.8(4) . . ?
C14C O15C Mn3 127.3(3) . . ?
C14C C16C H16G 109.5 . . ?
C14C C16C H16H 109.5 . . ?
C14C C16C H16I 109.5 . . ?
C14C C16' H16X 109.5 . . ?
C14C C16' H16Y 109.5 . . ?
H16X C16' H16Y 109.5 . . ?
C14C C16' H16Z 109.5 . . ?
H16X C16' H16Z 109.5 . . ?
H16Y C16' H16Z 109.5 . . ?
C2D N1D C6D 116.8(3) . . ?
C2D N1D Ni3 130.0(2) . . ?
C6D N1D Ni3 113.1(2) . . ?
N1D C2D N3D 126.5(4) . . ?
N1D C2D H2D 116.7 . . ?
N3D C2D H2D 116.7 . . ?
C2D N3D C4D 114.8(4) . . ?
N3D C4D C5D 123.5(4) . . ?
N3D C4D H4D 118.2 . . ?
C5D C4D H4D 118.2 . . ?
C4D C5D C6D 117.0(4) . . ?
C4D C5D H5D 121.5 . . ?
C6D C5D H5D 121.5 . . ?
N1D C6D C5D 121.4(3) . . ?
N1D C6D C7D 116.9(3) . . ?
C5D C6D C7D 121.7(3) . . ?
O8D C7D N9D 129.3(3) . . ?
O8D C7D C6D 117.3(3) . . ?
N9D C7D C6D 113.4(3) . . ?
C7D N9D C10D 116.4(3) . . ?
C7D N9D Ni3 118.1(2) . . ?
C10D N9D Ni3 124.57(18) . . ?
C11D C10D C15D 118.9(3) . . ?
C11D C10D N9D 121.4(3) . . ?
C15D C10D N9D 119.6(3) . . ?
C10D C11D C12D 119.5(3) . . ?
C10D C11D H11D 120.2 . . ?
C12D C11D H11D 120.2 . . ?
C13D C12D C11D 121.4(3) . . ?
C13D C12D H12J 119.3 . . ?
C11D C12D H12J 119.3 . . ?
C12D C13D C14D 119.8(3) . . ?
C12D C13D H13D 120.1 . . ?
C14D C13D H13D 120.1 . . ?
C15D C14D C13D 119.6(3) . . ?
C15D C14D N16D 119.8(3) . . ?
C13D C14D N16D 120.6(3) . . ?
C14D C15D C10D 120.6(3) . . ?
C14D C15D H15D 119.7 . . ?
C10D C15D H15D 119.7 . . ?
C17D N16D C14D 116.8(3) . . ?
C17D N16D Ni2 118.2(3) . . ?
C14D N16D Ni2 124.7(2) . . ?
O18D C17D N16D 130.1(4) . . ?
O18D C17D C19D 116.6(3) . . ?
N16D C17D C19D 113.2(3) . . ?
N24D C19D C20D 123.8(4) . . ?
N24D C19D C20' 112.0(6) . . ?
C20D C19D C20' 30.9(4) . . ?
N24D C19D C17D 117.2(3) . . ?
C20D C19D C17D 116.9(4) . . ?
C20' C19D C17D 128.5(5) . . ?
C21D C20D C19D 113.7(6) . . ?
C21D C20D H20D 123.1 . . ?
C19D C20D H20D 123.1 . . ?
N22D C21D C20D 122.7(6) . . ?
N22D C21D H21D 118.7 . . ?
C20D C21D H21D 118.7 . . ?
C23D N22D C21D 114.4(5) . . ?
N24D C23D N22D 131.4(5) . . ?
N24D C23D H23D 114.3 . . ?
N22D C23D H23D 114.3 . . ?
C21' C20' C19D 124.8(10) . . ?
C21' C20' H20' 117.6 . . ?
C19D C20' H20' 117.6 . . ?
N22' C21' C20' 121.8(12) . . ?
N22' C21' H21' 119.1 . . ?
C20' C21' H21' 119.1 . . ?
C21' N22' C23' 117.7(11) . . ?
N22' C23' N24D 121.7(9) . . ?
N22' C23' H23' 119.1 . . ?
N24D C23' H23' 119.1 . . ?
C23D N24D C19D 113.5(4) . . ?
C23D N24D C23' 22.5(3) . . ?
C19D N24D C23' 121.9(5) . . ?
C23D N24D Ni2 132.2(3) . . ?
C19D N24D Ni2 112.8(2) . . ?
C23' N24D Ni2 124.3(4) . . ?
C4E C5E C6E 117.2(4) . . ?
C4E C5E H5E 121.4 . . ?
C6E C5E H5E 121.4 . . ?
N3E C2E N1E 125.5(4) . . ?
N3E C2E H2E 117.3 . . ?
N1E C2E H2E 117.3 . . ?
C2E N3E C4E 116.1(4) . . ?
N3E C4E C5E 122.9(4) . . ?
N3E C4E H4E 118.5 . . ?
C5E C4E H4E 118.5 . . ?
C2E N1E C6E 118.1(3) . . ?
C2E N1E Ni2 129.6(3) . . ?
C6E N1E Ni2 112.0(2) . . ?
N1E C6E C5E 120.3(3) . . ?
N1E C6E C7E 117.2(3) . . ?
C5E C6E C7E 122.5(3) . . ?
O8E C7E N9E 128.0(3) . . ?
O8E C7E C6E 117.3(3) . . ?
N9E C7E C6E 114.6(3) . . ?
C7E O8E Mn1 129.5(2) . . ?
C7E N9E C10E 117.3(3) . . ?
C7E N9E Ni2 117.3(2) . . ?
C10E N9E Ni2 124.73(19) . . ?
C11E C10E C15E 118.8(3) . . ?
C11E C10E N9E 121.7(3) . . ?
C15E C10E N9E 119.5(3) . . ?
C12E C11E C10E 119.6(3) . . ?
C12E C11E H11E 120.2 . . ?
C10E C11E H11E 120.2 . . ?
C11E C12E C13E 121.9(3) . . ?
C11E C12E H12K 119.1 . . ?
C13E C12E H12K 119.1 . . ?
C14E C13E C12E 118.6(3) . . ?
C14E C13E H13E 120.7 . . ?
C12E C13E H13E 120.7 . . ?
C15E C14E C13E 119.8(3) . . ?
C15E C14E N16E 118.4(3) . . ?
C13E C14E N16E 121.7(3) . . ?
C14E C15E C10E 121.2(3) . . ?
C14E C15E H15E 119.4 . . ?
C10E C15E H15E 119.4 . . ?
C17E N16E C14E 116.1(3) . . ?
C17E N16E Ni3 118.3(2) . . ?
C14E N16E Ni3 125.28(19) . . ?
O18E C17E N16E 129.3(3) . . ?
O18E C17E C19E 118.2(3) . . ?
N16E C17E C19E 112.3(3) . . ?
N24E C19E C20E 120.6(3) . . ?
N24E C19E C17E 117.0(3) . . ?
C20E C19E C17E 122.3(3) . . ?
C19E C20E C21E 117.7(3) . . ?
C19E C20E H20E 121.2 . . ?
C21E C20E H20E 121.2 . . ?
N22E C21E C20E 121.6(3) . . ?
N22E C21E H21E 119.2 . . ?
C20E C21E H21E 119.2 . . ?
C21E N22E C23E 117.5(3) . . ?
C21E N22E Mn3 121.2(2) . 1_445 ?
C23E N22E Mn3 117.9(2) . 1_445 ?
N24E C23E N22E 124.9(3) . . ?
N24E C23E H23E 117.5 . . ?
N22E C23E H23E 117.5 . . ?
C23E N24E C19E 117.1(3) . . ?
C23E N24E Ni3 130.3(2) . . ?
C19E N24E Ni3 112.5(2) . . ?
C2F N1F C6F 116.7(3) . . ?
C2F N1F Ni3 130.7(2) . . ?
C6F N1F Ni3 112.4(2) . . ?
N3F C2F N1F 127.1(3) . . ?
N3F C2F H2F 116.4 . . ?
N1F C2F H2F 116.4 . . ?
C4F N3F C2F 115.1(3) . . ?
N3F C4F C5F 122.3(3) . . ?
N3F C4F H4F 118.8 . . ?
C5F C4F H4F 118.8 . . ?
C6F C5F C4F 118.4(3) . . ?
C6F C5F H5F 120.8 . . ?
C4F C5F H5F 120.8 . . ?
N1F C6F C5F 120.4(3) . . ?
N1F C6F C7F 117.9(3) . . ?
C5F C6F C7F 121.8(3) . . ?
O8F C7F N9F 130.0(3) . . ?
O8F C7F C6F 116.2(3) . . ?
N9F C7F C6F 113.8(3) . . ?
C7F N9F C10F 116.5(2) . . ?
C7F N9F Ni3 117.0(2) . . ?
C10F N9F Ni3 126.6(2) . . ?
C11F C10F C15F 118.7(3) . . ?
C11F C10F N9F 121.3(3) . . ?
C15F C10F N9F 119.9(3) . . ?
C12F C11F C10F 120.2(3) . . ?
C12F C11F H11F 119.9 . . ?
C10F C11F H11F 119.9 . . ?
C11F C12F C13F 120.8(3) . . ?
C11F C12F H12L 119.6 . . ?
C13F C12F H12L 119.6 . . ?
C14F C13F C12F 119.5(3) . . ?
C14F C13F H13F 120.3 . . ?
C12F C13F H13F 120.3 . . ?
C13F C14F C15F 119.6(3) . . ?
C13F C14F N16F 120.1(3) . . ?
C15F C14F N16F 120.2(3) . . ?
C10F C15F C14F 121.0(3) . . ?
C10F C15F H15F 119.5 . . ?
C14F C15F H15F 119.5 . . ?
C17F N16F C14F 118.0(3) . . ?
C17F N16F Ni2 116.4(2) . . ?
C14F N16F Ni2 124.6(2) . . ?
O18F C17F N16F 128.5(3) . . ?
O18F C17F C19F 117.8(3) . . ?
N16F C17F C19F 113.7(3) . . ?
C17F O18F Mn2 156.6(2) . . ?
N24F C19F C20F 120.3(3) . . ?
N24F C19F C17F 117.4(3) . . ?
C20F C19F C17F 122.3(3) . . ?
C19F C20F C21F 117.5(3) . . ?
C19F C20F H20F 121.2 . . ?
C21F C20F H20F 121.2 . . ?
N22F C21F C20F 123.2(3) . . ?
N22F C21F H21F 118.4 . . ?
C20F C21F H21F 118.4 . . ?
C23F N22F C21F 114.6(3) . . ?
N22F C23F N24F 126.9(3) . . ?
N22F C23F H23F 116.6 . . ?
N24F C23F H23F 116.6 . . ?
C23F N24F C19F 117.5(3) . . ?
C23F N24F Ni2 128.9(2) . . ?
C19F N24F Ni2 113.5(2) . . ?
C2G N1G C6G 117.5(3) . . ?
C2G N1G Ni1 129.1(2) . . ?
C6G N1G Ni1 113.3(2) . . ?
N3G C2G N1G 126.5(3) . . ?
N3G C2G H2G 116.7 . . ?
N1G C2G H2G 116.7 . . ?
C2G N3G C4G 115.5(3) . . ?
N3G C4G C5G 122.3(3) . . ?
N3G C4G H4G 118.9 . . ?
C5G C4G H4G 118.9 . . ?
C6G C5G C4G 118.2(3) . . ?
C6G C5G H5G 120.9 . . ?
C4G C5G H5G 120.9 . . ?
N1G C6G C5G 119.9(3) . . ?
N1G C6G C7G 116.0(3) . . ?
C5G C6G C7G 124.0(3) . . ?
O8G C7G N9G 128.6(3) . . ?
O8G C7G C6G 117.2(3) . . ?
N9G C7G C6G 114.1(3) . . ?
C7G O8G Mn1 144.1(2) . 1_655 ?
C7G N9G C10G 118.3(2) . . ?
C7G N9G Ni1 115.50(19) . . ?
C10G N9G Ni1 124.6(2) . . ?
C15G C10G C11G 119.0(3) . . ?
C15G C10G N9G 121.1(3) . . ?
C11G C10G N9G 119.7(3) . . ?
C12G C11G C10G 119.8(3) . . ?
C12G C11G H11G 120.1 . . ?
C10G C11G H11G 120.1 . . ?
C11G C12G C13G 121.7(3) . . ?
C11G C12G H12M 119.1 . . ?
C13G C12G H12M 119.1 . . ?
C12G C13G C14G 118.5(3) . . ?
C12G C13G H13G 120.8 . . ?
C14G C13G H13G 120.8 . . ?
C15G C14G C13G 120.3(3) . . ?
C15G C14G N16G 117.9(2) . . ?
C13G C14G N16G 121.6(2) . . ?
C14G C15G C10G 120.6(3) . . ?
C14G C15G H15G 119.7 . . ?
C10G C15G H15G 119.7 . . ?
C17G N16G C14G 117.1(2) . . ?
C17G N16G Ni5 117.39(19) . . ?
C14G N16G Ni5 125.47(17) . . ?
O18G C17G N16G 130.1(3) . . ?
O18G C17G C19G 117.8(3) . . ?
N16G C17G C19G 112.0(3) . . ?
N24G C19G C20G 120.1(3) . . ?
N24G C19G C17G 117.3(3) . . ?
C20G C19G C17G 122.5(3) . . ?
C21G C20G C19G 118.2(3) . . ?
C21G C20G H20G 120.9 . . ?
C19G C20G H20G 120.9 . . ?
N22G C21G C20G 122.6(3) . . ?
N22G C21G H21G 118.7 . . ?
C20G C21G H21G 118.7 . . ?
C21G N22G C23G 115.6(3) . . ?
N22G C23G N24G 126.1(3) . . ?
N22G C23G H23G 117.0 . . ?
N24G C23G H23G 117.0 . . ?
C19G N24G C23G 117.4(3) . . ?
C19G N24G Ni5 113.25(19) . . ?
C23G N24G Ni5 127.8(2) . . ?
C6H N1H C2H 118.1(3) . . ?
C6H N1H Ni1 112.2(2) . . ?
C2H N1H Ni1 129.1(2) . . ?
N3H C2H N1H 126.0(4) . . ?
N3H C2H H2H 117.0 . . ?
N1H C2H H2H 117.0 . . ?
C2H N3H C4H 115.4(4) . . ?
N3H C4H C5H 123.0(4) . . ?
N3H C4H H4H 118.5 . . ?
C5H C4H H4H 118.5 . . ?
C6H C5H C4H 116.4(4) . . ?
C6H C5H H5H 121.8 . . ?
C4H C5H H5H 121.8 . . ?
N1H C6H C5H 121.0(4) . . ?
N1H C6H C7H 118.3(3) . . ?
C5H C6H C7H 120.7(4) . . ?
O8H C7H N9H 129.0(3) . . ?
O8H C7H C6H 119.4(3) . . ?
N9H C7H C6H 111.5(3) . . ?
C7H N9H C10H 116.7(3) . . ?
C7H N9H Ni1 118.2(2) . . ?
C10H N9H Ni1 125.03(19) . . ?
C15H C10H C11H 119.3(3) . . ?
C15H C10H N9H 118.1(3) . . ?
C11H C10H N9H 122.5(3) . . ?
C12H C11H C10H 119.4(3) . . ?
C12H C11H H11H 120.3 . . ?
C10H C11H H11H 120.3 . . ?
C11H C12H C13H 121.7(3) . . ?
C11H C12H H12N 119.2 . . ?
C13H C12H H12N 119.2 . . ?
C12H C13H C14H 119.4(3) . . ?
C12H C13H H13H 120.3 . . ?
C14H C13H H13H 120.3 . . ?
C13H C14H C15H 119.2(3) . . ?
C13H C14H N16H 120.6(3) . . ?
C15H C14H N16H 120.1(3) . . ?
C10H C15H C14H 121.0(3) . . ?
C10H C15H H15H 119.5 . . ?
C14H C15H H15H 119.5 . . ?
C17H N16H C14H 116.4(2) . . ?
C17H N16H Ni5 116.69(18) . . ?
C14H N16H Ni5 125.66(18) . . ?
O18H C17H N16H 128.0(3) . . ?
O18H C17H C19H 118.4(3) . . ?
N16H C17H C19H 113.6(2) . . ?
C17H O18H Mn3 142.5(2) . . ?
N24H C19H C20H 120.2(3) . . ?
N24H C19H C17H 116.8(3) . . ?
C20H C19H C17H 122.9(3) . . ?
C21H C20H C19H 117.2(3) . . ?
C21H C20H H20H 121.4 . . ?
C19H C20H H20H 121.4 . . ?
N22H C21H C20H 123.1(3) . . ?
N22H C21H H21H 118.4 . . ?
C20H C21H H21H 118.4 . . ?
C23H N22H C21H 115.2(3) . . ?
N22H C23H N24H 126.7(3) . . ?
N22H C23H H23H 116.6 . . ?
N24H C23H H23H 116.6 . . ?
C23H N24H C19H 117.5(3) . . ?
C23H N24H Ni5 129.1(2) . . ?
C19H N24H Ni5 113.37(19) . . ?
C2J N1J C6J 117.5(3) . . ?
C2J N1J Ni1 127.9(2) . . ?
C6J N1J Ni1 112.08(19) . . ?
N3J C2J N1J 126.0(3) . . ?
N3J C2J H2J 117.0 . . ?
N1J C2J H2J 117.0 . . ?
C2J N3J C4J 115.7(3) . . ?
N3J C4J C5J 123.3(3) . . ?
N3J C4J H4J 118.4 . . ?
C5J C4J H4J 118.4 . . ?
C6J C5J C4J 116.8(3) . . ?
C6J C5J H5J 121.6 . . ?
C4J C5J H5J 121.6 . . ?
N1J C6J C5J 120.7(3) . . ?
N1J C6J C7J 117.6(3) . . ?
C5J C6J C7J 121.6(3) . . ?
O8J C7J N9J 128.6(3) . . ?
O8J C7J C6J 117.4(3) . . ?
N9J C7J C6J 113.8(2) . . ?
C7J O8J Mn2 132.54(19) . . ?
C7J N9J C10J 115.9(2) . . ?
C7J N9J Ni1 117.92(19) . . ?
C10J N9J Ni1 125.46(18) . . ?
C15J C10J C11J 119.8(3) . . ?
C15J C10J N9J 117.6(3) . . ?
C11J C10J N9J 122.4(3) . . ?
C12J C11J C10J 119.1(3) . . ?
C12J C11J H11J 120.5 . . ?
C10J C11J H11J 120.5 . . ?
C11J C12J C13J 121.3(3) . . ?
C11J C12J H12O 119.3 . . ?
C13J C12J H12O 119.3 . . ?
C12J C13J C14J 119.5(3) . . ?
C12J C13J H13J 120.3 . . ?
C14J C13J H13J 120.3 . . ?
C15J C14J C13J 119.5(3) . . ?
C15J C14J N16J 117.9(3) . . ?
C13J C14J N16J 122.5(3) . . ?
C14J C15J C10J 120.8(3) . . ?
C14J C15J H15J 119.6 . . ?
C10J C15J H15J 119.6 . . ?
C17J N16J C14J 116.5(3) . . ?
C17J N16J Ni5 118.1(2) . . ?
C14J N16J Ni5 124.59(19) . . ?
O18J C17J N16J 129.9(3) . . ?
O18J C17J C19J 117.9(3) . . ?
N16J C17J C19J 112.2(3) . . ?
N24J C19J C20J 121.4(3) . . ?
N24J C19J C17J 117.6(3) . . ?
C20J C19J C17J 120.7(4) . . ?
C21J C20J C19J 116.0(4) . . ?
C21J C20J H20J 122.0 . . ?
C19J C20J H20J 122.0 . . ?
N22J C21J C20J 123.5(4) . . ?
N22J C21J H21J 118.3 . . ?
C20J C21J H21J 118.3 . . ?
C23J N22J C21J 115.8(3) . . ?
N22J C23J N24J 126.1(4) . . ?
N22J C23J H23J 116.9 . . ?
N24J C23J H23J 116.9 . . ?
C23J N24J C19J 116.9(3) . . ?
C23J N24J Ni5 128.8(2) . . ?
C19J N24J Ni5 111.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        67.68
_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.553
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.062
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -112.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -37.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  2 omega -109.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -37.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  3 omega -121.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164 -164.0000  109.0000 66

#__ type_ start__ end____ width___ exp.time_
  4 omega  -82.00  -54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164 -164.0000 -134.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega   60.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  179.0000   30.0000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega   86.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  179.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  7 omega   68.00   95.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  164.0000 -109.0000 27

#__ type_ start__ end____ width___ exp.time_
  8 omega   32.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000 -120.0000 34

#__ type_ start__ end____ width___ exp.time_
  9 omega   32.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000  -90.0000 35

#__ type_ start__ end____ width___ exp.time_
 10 omega   32.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000    0.0000 44

#__ type_ start__ end____ width___ exp.time_
 11 omega   43.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -45.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
 12 omega  101.00  164.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  125.0000 -150.0000 63

#__ type_ start__ end____ width___ exp.time_
 13 omega   80.00  119.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
 14 omega   95.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -164.0000   45.0000 44

#__ type_ start__ end____ width___ exp.time_
 15 omega   39.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -116.0000 -102.0000 28

#__ type_ start__ end____ width___ exp.time_
 16 omega  134.00  161.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  164.0000 -109.0000 27

#__ type_ start__ end____ width___ exp.time_
 17 omega   88.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -116.0000 -102.0000 27

#__ type_ start__ end____ width___ exp.time_
 18 omega   80.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000    0.0000 62

#__ type_ start__ end____ width___ exp.time_
 19 omega  143.00  168.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  125.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   83.00  162.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000 -150.0000 79

#__ type_ start__ end____ width___ exp.time_
 21 omega   29.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667  -77.0000  120.0000 109

#__ type_ start__ end____ width___ exp.time_
 22 omega   81.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   45.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
 23 omega   30.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667 -110.0000   47.0000 83

#__ type_ start__ end____ width___ exp.time_
 24 omega  -67.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164   37.0000 -180.0000 103

#__ type_ start__ end____ width___ exp.time_
 25 omega -129.00  -34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  179.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 26 omega -119.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -77.0000  -90.0000 112

#__ type_ start__ end____ width___ exp.time_
 27 omega -119.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3164  -77.0000    0.0000 112

#__ type_ start__ end____ width___ exp.time_
 28 omega    7.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164   77.0000 -180.0000 112

#__ type_ start__ end____ width___ exp.time_
 29 omega   68.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3164  164.0000  134.0000 52

#__ type_ start__ end____ width___ exp.time_
 30 omega   46.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   15.0000  120.0000 132

#__ type_ start__ end____ width___ exp.time_
 31 omega   74.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1667   77.0000  -60.0000 37

;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 12 2 0.0684 1.0000 12.0000 2.0000 -0.2701 -0.0852 0.9390
0 -13 -2 0.0859 0.0000 -13.0000 -2.0000 0.2024 0.0654 -1.0091
10 -10 0 0.0950 10.0000 -10.0000 0.0000 -0.6768 -0.1978 -0.7016
-12 0 -2 0.0377 -12.0000 0.0000 -2.0000 1.0039 0.2897 -0.0910
0 1 16 0.0421 0.0000 1.0000 16.0000 -0.5251 0.8182 0.2254
-1 0 -16 0.0413 -1.0000 0.0000 -16.0000 0.5928 -0.7985 -0.1552
3 -13 6 0.0887 3.0000 -13.0000 6.0000 -0.2897 0.3827 -0.9164
12 -1 -7 0.0590 12.0000 -1.0000 -7.0000 -0.7039 -0.7443 -0.0691
-5 -10 5 0.0781 -5.0000 -10.0000 5.0000 0.3370 0.5541 -0.7454
-3 13 1 0.0705 -3.0000 13.0000 1.0000 0.0646 -0.0190 0.9817
5 0 -16 0.0429 5.0000 0.0000 -16.0000 0.1230 -0.9953 -0.1191
1 12 -8 0.0682 1.0000 12.0000 -8.0000 0.0515 -0.6048 0.8457
4 -11 -8 0.0836 4.0000 -11.0000 -8.0000 0.0609 -0.4035 -0.8886
6 0 12 0.0585 6.0000 -0.0000 12.0000 -0.8557 0.4266 0.1481
6 -11 7 0.0835 6.0000 -11.0000 7.0000 -0.5780 0.3101 -0.7366
-7 1 15 0.0450 -7.0000 1.0000 15.0000 0.0552 0.9959 0.1739
# 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 0.243 0.271 0.904 3599 1138 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_hastalli
_database_code_depnum_ccdc_archive 'CCDC 1551794'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C32 H24 Cu2 N12 O6, 2(H2 O)'
_chemical_formula_sum            'C32 H28 Cu2 N12 O8'
_chemical_formula_weight         835.74
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6178(19)
_cell_length_b                   11.658(3)
_cell_length_c                   11.819(3)
_cell_angle_alpha                116.889(5)
_cell_angle_beta                 100.695(5)
_cell_angle_gamma                101.227(5)
_cell_volume                     872.2(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    16527
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.522
_cell_measurement_theta_min      5.907
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.361400
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.0581 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.3614.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5403
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.051
_diffrn_reflns_theta_min         2.034
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2292
_reflns_number_total             3682
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.662
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0807
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1068P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2182
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5) O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Rotating group:
 O1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.20966(10) 0.37999(7) 0.17015(7) 0.0371(3) Uani 1 1 d . . . . .
O1 O 0.0579(6) 0.5015(4) 0.2734(4) 0.0442(11) Uani 1 1 d . . . . .
H1A H 0.0380 0.5481 0.2194 0.066 Uiso 1 1 d GR . . . .
H1B H -0.0555 0.4517 0.2607 0.066 Uiso 1 1 d GR . . . .
O2 O -0.0020(6) 0.3041(4) -0.2070(4) 0.0430(10) Uani 1 1 d . . . . .
O3 O 0.7334(6) 0.3558(5) 0.2789(5) 0.0539(12) Uani 1 1 d . . . . .
N1 N -0.0341(7) 0.2057(5) 0.0340(5) 0.0399(12) Uani 1 1 d . . . . .
N2 N -0.3246(10) -0.0135(6) -0.1836(7) 0.0651(18) Uani 1 1 d . . . . .
N3 N 0.1571(6) 0.4130(5) 0.0189(5) 0.0328(11) Uani 1 1 d . . . . .
N4 N 0.4585(7) 0.3570(5) 0.1569(5) 0.0352(11) Uani 1 1 d . . . . .
N5 N 0.2837(7) 0.3469(5) 0.3227(5) 0.0380(12) Uani 1 1 d . . . . .
N6 N 0.4367(9) 0.3038(7) 0.5268(6) 0.0588(16) Uani 1 1 d . . . . .
C1 C -0.1381(10) 0.1057(7) 0.0437(7) 0.0509(18) Uani 1 1 d . . . . .
H1 H -0.1133 0.1088 0.1270 0.061 Uiso 1 1 calc R . . . .
C2 C -0.2807(11) -0.0016(7) -0.0655(8) 0.057(2) Uani 1 1 d . . . . .
H2 H -0.3508 -0.0706 -0.0545 0.069 Uiso 1 1 calc R . . . .
C3 C -0.2186(10) 0.0888(7) -0.1923(7) 0.0517(18) Uani 1 1 d . . . . .
H3 H -0.2442 0.0854 -0.2757 0.062 Uiso 1 1 calc R . . . .
C4 C -0.0773(8) 0.1957(6) -0.0858(6) 0.0364(14) Uani 1 1 d . . . . .
C5 C 0.0341(8) 0.3130(6) -0.0951(6) 0.0353(13) Uani 1 1 d . . . . .
C6 C 0.2823(8) 0.5284(6) 0.0299(6) 0.0310(12) Uani 1 1 d . . . . .
C7 C 0.3765(9) 0.6385(6) 0.1608(6) 0.0359(13) Uani 1 1 d . . . . .
H7 H 0.3458 0.6364 0.2343 0.043 Uiso 1 1 calc R . . . .
C8 C 0.5122(9) 0.7484(6) 0.1819(6) 0.0406(14) Uani 1 1 d . . . . .
H8 H 0.5737 0.8226 0.2703 0.049 Uiso 1 1 calc R . . . .
C9 C 0.3320(8) 0.5337(6) -0.0749(6) 0.0314(12) Uani 1 1 d . . . . .
H9 H 0.2697 0.4607 -0.1638 0.038 Uiso 1 1 calc R . . . .
C10 C 0.4384(9) 0.2464(6) -0.0771(6) 0.0419(15) Uani 1 1 d . . . . .
H10 H 0.3444 0.1693 -0.0930 0.050 Uiso 1 1 calc R . . . .
C11 C 0.5275(8) 0.3547(6) 0.0508(6) 0.0339(13) Uani 1 1 d . . . . .
C12 C 0.5672(9) 0.3549(6) 0.2575(6) 0.0373(14) Uani 1 1 d . . . . .
C13 C 0.4611(9) 0.3433(5) 0.3492(6) 0.0364(14) Uani 1 1 d . . . . .
C14 C 0.5355(10) 0.3223(7) 0.4516(7) 0.0471(16) Uani 1 1 d . . . . .
H14 H 0.6618 0.3211 0.4687 0.057 Uiso 1 1 calc R . . . .
C15 C 0.2592(12) 0.3075(7) 0.4982(7) 0.059(2) Uani 1 1 d . . . . .
H15 H 0.1832 0.2925 0.5486 0.070 Uiso 1 1 calc R . . . .
C16 C 0.1828(10) 0.3319(7) 0.4002(7) 0.0472(16) Uani 1 1 d . . . . .
H16 H 0.0589 0.3381 0.3868 0.057 Uiso 1 1 calc R . . . .
O2W O -0.2256(16) 0.0956(11) 0.2995(11) 0.074(4) Uani 0.5 1 d . . P . .
H2WA H -0.3300 0.0645 0.3078 0.112 Uiso 0.5 1 d G . P . .
H2WB H -0.1600 0.1693 0.3712 0.112 Uiso 0.5 1 d G . P . .
O1W O -0.1049(15) 0.0870(10) -0.4716(9) 0.063(3) Uani 0.5 1 d . . P . .
H1WA H -0.1858 0.1071 -0.5159 0.095 Uiso 0.5 1 d G . P . .
H1WB H -0.0987 0.1282 -0.3878 0.095 Uiso 0.5 1 d G . P . .


_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
Cu1 O1 2.105(4) . ?
Cu1 N1 2.152(5) . ?
Cu1 N3 1.980(5) . ?
Cu1 N4 1.990(5) . ?
Cu1 N5 2.013(5) . ?
O1 H1A 1.0172 . ?
O1 H1B 0.8856 . ?
O2 C5 1.251(7) . ?
O3 C12 1.241(7) . ?
N1 C1 1.340(8) . ?
N1 C4 1.338(8) . ?
N2 C2 1.308(9) . ?
N2 C3 1.360(8) . ?
N3 C5 1.318(7) . ?
N3 C6 1.426(7) . ?
N4 C11 1.438(7) . ?
N4 C12 1.330(8) . ?
N5 C13 1.343(8) . ?
N5 C16 1.348(8) . ?
N6 C14 1.327(9) . ?
N6 C15 1.346(10) . ?
C1 H1 0.9500 . ?
C1 C2 1.379(10) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.361(8) . ?
C4 C5 1.523(8) . ?
C6 C7 1.410(8) . ?
C6 C9 1.385(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.368(8) . ?
C8 H8 0.9500 . ?
C8 C10 1.382(8) 2_665 ?
C9 H9 0.9500 . ?
C9 C11 1.389(8) 2_665 ?
C10 C8 1.382(8) 2_665 ?
C10 H10 0.9500 . ?
C10 C11 1.378(8) . ?
C11 C9 1.389(8) 2_665 ?
C12 C13 1.504(8) . ?
C13 C14 1.383(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.369(10) . ?
C16 H16 0.9500 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8503 . ?
O1W H1WA 0.8699 . ?
O1W H1WB 0.8699 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 95.24(18) . . ?
N3 Cu1 O1 94.64(18) . . ?
N3 Cu1 N1 80.26(19) . . ?
N3 Cu1 N4 94.62(19) . . ?
N3 Cu1 N5 175.4(2) . . ?
N4 Cu1 O1 148.21(19) . . ?
N4 Cu1 N1 116.3(2) . . ?
N4 Cu1 N5 80.9(2) . . ?
N5 Cu1 O1 88.97(19) . . ?
N5 Cu1 N1 102.20(19) . . ?
Cu1 O1 H1A 99.0 . . ?
Cu1 O1 H1B 111.4 . . ?
H1A O1 H1B 106.3 . . ?
C1 N1 Cu1 133.4(5) . . ?
C4 N1 Cu1 109.9(4) . . ?
C4 N1 C1 116.6(6) . . ?
C2 N2 C3 115.1(6) . . ?
C5 N3 Cu1 117.3(4) . . ?
C5 N3 C6 123.0(5) . . ?
C6 N3 Cu1 118.1(4) . . ?
C11 N4 Cu1 122.5(4) . . ?
C12 N4 Cu1 116.8(4) . . ?
C12 N4 C11 120.5(5) . . ?
C13 N5 Cu1 113.0(4) . . ?
C13 N5 C16 117.9(5) . . ?
C16 N5 Cu1 129.1(5) . . ?
C14 N6 C15 116.0(6) . . ?
N1 C1 H1 119.6 . . ?
N1 C1 C2 120.9(6) . . ?
C2 C1 H1 119.6 . . ?
N2 C2 C1 123.5(6) . . ?
N2 C2 H2 118.2 . . ?
C1 C2 H2 118.2 . . ?
N2 C3 H3 118.8 . . ?
N2 C3 C4 122.4(7) . . ?
C4 C3 H3 118.8 . . ?
N1 C4 C3 121.5(6) . . ?
N1 C4 C5 116.5(5) . . ?
C3 C4 C5 121.9(6) . . ?
O2 C5 N3 128.2(5) . . ?
O2 C5 C4 117.3(5) . . ?
N3 C5 C4 114.4(5) . . ?
C7 C6 N3 115.9(5) . . ?
C9 C6 N3 125.1(5) . . ?
C9 C6 C7 118.6(5) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C10 121.3(6) . 2_665 ?
C10 C8 H8 119.4 2_665 . ?
C6 C9 H9 119.8 . . ?
C6 C9 C11 120.4(5) . 2_665 ?
C11 C9 H9 119.8 2_665 . ?
C8 C10 H10 120.5 2_665 . ?
C11 C10 C8 119.0(6) . 2_665 ?
C11 C10 H10 120.5 . . ?
C9 C11 N4 120.2(5) 2_665 . ?
C10 C11 N4 118.8(5) . . ?
C10 C11 C9 120.7(5) . 2_665 ?
O3 C12 N4 128.7(6) . . ?
O3 C12 C13 119.6(6) . . ?
N4 C12 C13 111.6(5) . . ?
N5 C13 C12 116.6(5) . . ?
N5 C13 C14 120.6(6) . . ?
C14 C13 C12 122.7(6) . . ?
N6 C14 C13 122.3(7) . . ?
N6 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
N6 C15 H15 118.4 . . ?
N6 C15 C16 123.2(7) . . ?
C16 C15 H15 118.4 . . ?
N5 C16 C15 119.8(7) . . ?
N5 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
H2WA O2W H2WB 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 -174.5(5) . . . . ?
Cu1 N1 C4 C3 175.6(5) . . . . ?
Cu1 N1 C4 C5 -7.0(6) . . . . ?
Cu1 N3 C5 O2 -169.5(5) . . . . ?
Cu1 N3 C5 C4 11.0(7) . . . . ?
Cu1 N3 C6 C7 -27.5(6) . . . . ?
Cu1 N3 C6 C9 145.0(5) . . . . ?
Cu1 N4 C11 C9 105.0(6) . . . 2_665 ?
Cu1 N4 C11 C10 -68.2(6) . . . . ?
Cu1 N4 C12 O3 -171.9(5) . . . . ?
Cu1 N4 C12 C13 11.2(6) . . . . ?
Cu1 N5 C13 C12 -3.8(6) . . . . ?
Cu1 N5 C13 C14 179.6(4) . . . . ?
Cu1 N5 C16 C15 178.8(5) . . . . ?
O3 C12 C13 N5 178.1(5) . . . . ?
O3 C12 C13 C14 -5.5(9) . . . . ?
N1 C1 C2 N2 -0.3(12) . . . . ?
N1 C4 C5 O2 178.6(5) . . . . ?
N1 C4 C5 N3 -1.9(8) . . . . ?
N2 C3 C4 N1 0.3(11) . . . . ?
N2 C3 C4 C5 -177.0(7) . . . . ?
N3 C6 C7 C8 173.9(6) . . . . ?
N3 C6 C9 C11 -172.1(5) . . . 2_665 ?
N4 C12 C13 N5 -4.6(7) . . . . ?
N4 C12 C13 C14 171.8(5) . . . . ?
N5 C13 C14 N6 0.6(10) . . . . ?
N6 C15 C16 N5 3.2(11) . . . . ?
C1 N1 C4 C3 -0.6(9) . . . . ?
C1 N1 C4 C5 176.9(6) . . . . ?
C2 N2 C3 C4 0.0(11) . . . . ?
C3 N2 C2 C1 0.0(12) . . . . ?
C3 C4 C5 O2 -4.0(9) . . . . ?
C3 C4 C5 N3 175.5(6) . . . . ?
C4 N1 C1 C2 0.5(10) . . . . ?
C5 N3 C6 C7 167.2(5) . . . . ?
C5 N3 C6 C9 -20.3(9) . . . . ?
C6 N3 C5 O2 -4.1(10) . . . . ?
C6 N3 C5 C4 176.4(5) . . . . ?
C6 C7 C8 C10 -0.8(10) . . . 2_665 ?
C7 C6 C9 C11 0.3(8) . . . 2_665 ?
C8 C10 C11 N4 171.7(6) 2_665 . . . ?
C8 C10 C11 C9 -1.5(9) 2_665 . . 2_665 ?
C9 C6 C7 C8 0.8(9) . . . . ?
C11 N4 C12 O3 2.9(10) . . . . ?
C11 N4 C12 C13 -174.1(5) . . . . ?
C12 N4 C11 C9 -69.4(8) . . . 2_665 ?
C12 N4 C11 C10 117.4(6) . . . . ?
C12 C13 C14 N6 -175.7(6) . . . . ?
C13 N5 C16 C15 -2.9(9) . . . . ?
C14 N6 C15 C16 -1.5(11) . . . . ?
C15 N6 C14 C13 -0.4(10) . . . . ?
C16 N5 C13 C12 177.6(5) . . . . ?
C16 N5 C13 C14 1.1(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_j15_2
_database_code_depnum_ccdc_archive 'CCDC 1551798'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-01-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'C48 H30 N18 Ni2 O6, H12 Na1 O6, H4 Na1.5 O11.5, 1.5(O1)'
_chemical_formula_sum            'C48 H67.50 N18 Na2.50 Ni2 O25'
_chemical_formula_weight         1471.59
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   13.9631(4)
_cell_length_b                   13.9631(4)
_cell_length_c                   21.1354(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3568.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5664
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      55.548
_cell_measurement_theta_min      5.119
_shelx_estimated_absorpt_T_max   0.885
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.8424
_exptl_absorpt_correction_T_min  0.782066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
'SAD V2.05 (?, 2016) was used for absorption correction. R(int) was 0.0479 before and 0.0354 after correction. The Ratio of minimum to maximum transmission is 0.7821. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1530
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20600
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.560
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2066
_reflns_number_total             2397
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1064P)²+2.6209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1650
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3_$1-H3B_$1
 1 with sigma of 0.1
 O3-H3A
 1 with sigma of 0.001
3. Others
 Fixed Sof: Na2(0.25) O6(0.08333) H3A(0.5) H3B(0.16667) O1W(0.08333)
 O2W(0.16667)
4.a Rotating group:
 O2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.3333 0.6667 0.41224(2) 0.0221(2) Uani 1 3 d S T P . .
Na1 Na 1.0000 1.0000 0.5000 0.0459(8) Uani 1 6 d S T P . .
O1 O 0.66937(16) 0.84578(19) 0.36781(10) 0.0418(6) Uani 1 1 d . . . . .
O2 O 0.8595(2) 0.8644(2) 0.43163(15) 0.0594(7) Uani 1 1 d . . . . .
H2A H 0.8179 0.8053 0.4527 0.089 Uiso 1 1 d GR . . . .
H2B H 0.8897 0.8486 0.4010 0.089 Uiso 1 1 d GR . . . .
N1 N 0.19860(19) 0.6453(2) 0.46863(10) 0.0288(5) Uani 1 1 d . . . . .
N2 N 0.0819(3) 0.5868(3) 0.55882(14) 0.0524(8) Uani 1 1 d . . . . .
N3 N 0.48198(18) 0.71733(19) 0.36497(10) 0.0245(5) Uani 1 1 d . . . . .
C1 C 0.1595(3) 0.5880(3) 0.52204(14) 0.0387(7) Uani 1 1 d . . . . .
H1 H 0.1894 0.5448 0.5348 0.046 Uiso 1 1 calc R . . . .
C2 C 0.0411(3) 0.6499(3) 0.53976(18) 0.0554(10) Uani 1 1 d . . . . .
H2 H -0.0121 0.6529 0.5649 0.067 Uiso 1 1 calc R . . . .
C3 C 0.0733(3) 0.7113(3) 0.48463(16) 0.0449(8) Uani 1 1 d . . . . .
H3 H 0.0425 0.7538 0.4720 0.054 Uiso 1 1 calc R . . . .
C4 C 0.1543(2) 0.7061(2) 0.44902(12) 0.0289(6) Uani 1 1 d . . . . .
C5 C 0.5710(2) 0.8008(2) 0.38837(12) 0.0279(6) Uani 1 1 d . . . . .
C6 C 0.4921(2) 0.6706(2) 0.30710(11) 0.0242(6) Uani 1 1 d . . . . .
C7 C 0.4927(3) 0.7206(3) 0.2500 0.0246(8) Uani 1 2 d S T P . .
H7 H 0.4935 0.7876 0.2500 0.030 Uiso 1 2 calc RS T P . .
C8 C 0.4958(2) 0.5731(2) 0.30710(13) 0.0322(6) Uani 1 1 d . . . . .
H8 H 0.4963 0.5397 0.3451 0.039 Uiso 1 1 calc R . . . .
C9 C 0.4986(4) 0.5258(4) 0.2500 0.0355(9) Uani 1 2 d S T P . .
H9 H 0.5025 0.4612 0.2500 0.043 Uiso 1 2 calc RS T P . .
Na2 Na 0.9422(3) 0.8482(3) 0.2500 0.0336(7) Uani 0.5 2 d S T P . .
O3 O 1.0000 1.0000 0.3187(2) 0.0582(12) Uani 1 3 d DS T P . .
O4 O 0.9276(3) 0.7469(3) 0.34726(18) 0.0855(10) Uani 1 1 d . . . . .
O5 O 0.7672(4) 0.8442(5) 0.2500 0.0895(17) Uani 1 2 d S T P . .
O6 O 0.795(2) 0.651(3) 0.2500 0.090(10) Uani 0.1667 2 d S T P . .
H3A H 1.077(2) 1.057(5) 0.331(3) 0.08(3) Uiso 0.5 1 d D . . . .
H3B H 1.0000 1.0000 0.363(4) 0.03(3) Uiso 0.5 3 d DS T P A 1
O1W O 0.3333 0.6667 0.6372(12) 0.078(7) Uiso 0.25 3 d S T P . .
O2W O 0.509(2) 0.725(2) 0.6545(12) 0.098(7) Uiso 0.1667 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.118(2) . ?
Ni1 N1 2.118(2) 3_565 ?
Ni1 N1 2.118(2) 2_665 ?
Ni1 N3 2.083(2) 2_665 ?
Ni1 N3 2.083(2) . ?
Ni1 N3 2.083(2) 3_565 ?
Na1 O2 2.410(3) . ?
Na1 O2 2.410(3) 2_765 ?
Na1 O2 2.410(3) 7_776 ?
Na1 O2 2.410(3) 9_656 ?
Na1 O2 2.410(3) 8_566 ?
Na1 O2 2.410(3) 3_675 ?
O1 C5 1.268(3) . ?
O2 H2A 0.8589 . ?
O2 H2B 0.8590 . ?
N1 C1 1.332(4) . ?
N1 C4 1.342(4) . ?
N2 C1 1.326(4) . ?
N2 C2 1.329(5) . ?
N3 C5 1.303(4) . ?
N3 C6 1.426(3) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.382(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(4) . ?
C4 C5 1.509(4) 2_665 ?
C5 C4 1.509(4) 3_565 ?
C6 C7 1.392(3) . ?
C6 C8 1.388(4) . ?
C7 C6 1.392(3) 10_556 ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.386(3) . ?
C9 C8 1.385(3) 10_556 ?
C9 H9 0.9300 . ?
Na2 Na2 3.209(6) 3_675 ?
Na2 Na2 3.208(6) 2_765 ?
Na2 O3 2.353(4) . ?
Na2 O3 2.353(4) 12_676 ?
Na2 O4 2.446(4) . ?
Na2 O4 2.446(4) 10_556 ?
Na2 O5 2.622(7) 2_765 ?
Na2 O5 2.416(6) . ?
Na2 O6 2.48(4) . ?
O3 Na2 2.353(4) 3_675 ?
O3 Na2 2.353(4) 2_765 ?
O3 H3A 1.0001(11) . ?
O3 H3B 0.94(8) . ?
O5 Na2 2.622(7) 3_675 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 91.44(9) . 3_565 ?
N1 Ni1 N1 91.44(9) . 2_665 ?
N1 Ni1 N1 91.44(9) 3_565 2_665 ?
N3 Ni1 N1 78.07(9) 2_665 . ?
N3 Ni1 N1 91.99(9) 3_565 . ?
N3 Ni1 N1 169.03(9) 3_565 3_565 ?
N3 Ni1 N1 91.99(9) 2_665 3_565 ?
N3 Ni1 N1 169.03(9) 2_665 2_665 ?
N3 Ni1 N1 78.06(9) 3_565 2_665 ?
N3 Ni1 N1 78.06(9) . 3_565 ?
N3 Ni1 N1 91.99(9) . 2_665 ?
N3 Ni1 N1 169.03(9) . . ?
N3 Ni1 N3 98.91(7) 2_665 . ?
N3 Ni1 N3 98.90(7) 2_665 3_565 ?
N3 Ni1 N3 98.91(7) 3_565 . ?
O2 Na1 O2 87.75(11) . 2_765 ?
O2 Na1 O2 87.75(11) 3_675 . ?
O2 Na1 O2 92.25(11) 3_675 8_566 ?
O2 Na1 O2 92.25(11) . 8_566 ?
O2 Na1 O2 180.0 7_776 . ?
O2 Na1 O2 180.00(12) 9_656 3_675 ?
O2 Na1 O2 87.75(11) 9_656 7_776 ?
O2 Na1 O2 87.75(11) 7_776 8_566 ?
O2 Na1 O2 92.25(11) 9_656 2_765 ?
O2 Na1 O2 87.75(11) 3_675 2_765 ?
O2 Na1 O2 92.25(11) 3_675 7_776 ?
O2 Na1 O2 180.0 8_566 2_765 ?
O2 Na1 O2 87.75(11) 9_656 8_566 ?
O2 Na1 O2 92.25(11) 9_656 . ?
O2 Na1 O2 92.25(11) 7_776 2_765 ?
Na1 O2 H2A 109.8 . . ?
Na1 O2 H2B 110.0 . . ?
H2A O2 H2B 109.0 . . ?
C1 N1 Ni1 129.1(2) . . ?
C1 N1 C4 117.4(2) . . ?
C4 N1 Ni1 113.26(17) . . ?
C1 N2 C2 115.6(3) . . ?
C5 N3 Ni1 117.67(17) . . ?
C5 N3 C6 117.8(2) . . ?
C6 N3 Ni1 124.48(17) . . ?
N1 C1 H1 116.9 . . ?
N2 C1 N1 126.2(3) . . ?
N2 C1 H1 116.9 . . ?
N2 C2 H2 118.2 . . ?
N2 C2 C3 123.5(3) . . ?
C3 C2 H2 118.2 . . ?
C2 C3 H3 121.8 . . ?
C2 C3 C4 116.5(3) . . ?
C4 C3 H3 121.8 . . ?
N1 C4 C3 120.7(3) . . ?
N1 C4 C5 116.8(2) . 2_665 ?
C3 C4 C5 122.5(3) . 2_665 ?
O1 C5 N3 128.7(2) . . ?
O1 C5 C4 117.3(2) . 3_565 ?
N3 C5 C4 114.0(2) . 3_565 ?
C7 C6 N3 119.4(2) . . ?
C8 C6 N3 120.7(2) . . ?
C8 C6 C7 119.9(3) . . ?
C6 C7 C6 120.2(3) 10_556 . ?
C6 C7 H7 119.9 . . ?
C6 C7 H7 119.9 10_556 . ?
C6 C8 H8 120.3 . . ?
C9 C8 C6 119.4(3) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C8 121.2(4) 10_556 . ?
C8 C9 H9 119.4 10_556 . ?
C8 C9 H9 119.4 . . ?
Na2 Na2 Na2 60.001(1) 2_765 3_675 ?
O3 Na2 Na2 47.02(8) . 2_765 ?
O3 Na2 Na2 47.02(8) 12_676 2_765 ?
O3 Na2 Na2 47.02(8) 12_676 3_675 ?
O3 Na2 Na2 47.02(8) . 3_675 ?
O3 Na2 O3 76.2(2) . 12_676 ?
O3 Na2 O4 83.93(14) . . ?
O3 Na2 O4 158.62(18) 12_676 . ?
O3 Na2 O4 83.93(14) 12_676 10_556 ?
O3 Na2 O4 158.62(18) . 10_556 ?
O3 Na2 O5 80.32(13) . 2_765 ?
O3 Na2 O5 84.76(15) 12_676 . ?
O3 Na2 O5 80.32(13) 12_676 2_765 ?
O3 Na2 O5 84.76(15) . . ?
O3 Na2 O6 136.1(3) . . ?
O3 Na2 O6 136.1(3) 12_676 . ?
O4 Na2 Na2 121.47(12) 10_556 3_675 ?
O4 Na2 Na2 112.71(14) . 2_765 ?
O4 Na2 Na2 112.71(14) 10_556 2_765 ?
O4 Na2 Na2 121.47(12) . 3_675 ?
O4 Na2 O4 114.4(2) 10_556 . ?
O4 Na2 O5 88.81(13) . 2_765 ?
O4 Na2 O5 88.81(13) 10_556 2_765 ?
O4 Na2 O6 64.8(3) 10_556 . ?
O4 Na2 O6 64.8(3) . . ?
O5 Na2 Na2 113.33(19) . 2_765 ?
O5 Na2 Na2 47.67(16) 2_765 2_765 ?
O5 Na2 Na2 53.33(19) . 3_675 ?
O5 Na2 Na2 107.67(16) 2_765 3_675 ?
O5 Na2 O4 101.30(15) . 10_556 ?
O5 Na2 O4 101.30(15) . . ?
O5 Na2 O5 161.0(2) . 2_765 ?
O5 Na2 O6 72.9(7) . . ?
O6 Na2 Na2 126.3(7) . 3_675 ?
O6 Na2 Na2 173.7(7) . 2_765 ?
O6 Na2 O5 126.1(7) . 2_765 ?
Na2 O3 Na2 85.95(16) 3_675 2_765 ?
Na2 O3 Na2 85.95(16) . 2_765 ?
Na2 O3 Na2 85.95(16) . 3_675 ?
Na2 O3 H3A 129(4) . . ?
Na2 O3 H3A 116(5) 3_675 . ?
Na2 O3 H3A 54(4) 2_765 . ?
Na2 O3 H3B 128.08(10) 3_675 . ?
Na2 O3 H3B 128.08(10) 2_765 . ?
Na2 O3 H3B 128.08(11) . . ?
H3A O3 H3B 75(4) . . ?
Na2 O5 Na2 79.0(2) . 3_675 ?

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
Ni1 N1 C1 N2 172.5(3) . . . . ?
Ni1 N1 C4 C3 -172.9(2) . . . . ?
Ni1 N1 C4 C5 5.2(3) . . . 2_665 ?
Ni1 N3 C5 O1 -179.7(2) . . . . ?
Ni1 N3 C5 C4 2.2(3) . . . 3_565 ?
Ni1 N3 C6 C7 95.1(3) . . . . ?
Ni1 N3 C6 C8 -81.7(3) . . . . ?
N2 C2 C3 C4 -1.1(6) . . . . ?
N3 C6 C7 C6 -174.0(2) . . . 10_556 ?
N3 C6 C8 C9 175.9(3) . . . . ?
C1 N1 C4 C3 2.1(4) . . . . ?
C1 N1 C4 C5 -179.8(3) . . . 2_665 ?
C1 N2 C2 C3 1.7(6) . . . . ?
C2 N2 C1 N1 -0.4(6) . . . . ?
C2 C3 C4 N1 -0.9(5) . . . . ?
C2 C3 C4 C5 -178.9(3) . . . 2_665 ?
C4 N1 C1 N2 -1.5(5) . . . . ?
C5 N3 C6 C7 -81.6(3) . . . . ?
C5 N3 C6 C8 101.6(3) . . . . ?
C6 N3 C5 O1 -2.8(4) . . . . ?
C6 N3 C5 C4 179.1(2) . . . 3_565 ?
C6 C8 C9 C8 -1.2(6) . . . 10_556 ?
C7 C6 C8 C9 -0.8(5) . . . . ?
C8 C6 C7 C6 2.8(5) . . . 10_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_j31a
_database_code_depnum_ccdc_archive 'CCDC 1551800'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C48 H40 N18 Ni3 O11, 16(H2 O), 2(O)'
_chemical_formula_sum            'C48 H76 N18 Ni3 O29'
_chemical_formula_weight         1545.39
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.076(3)
_cell_length_b                   20.453(4)
_cell_length_c                   24.811(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.72(3)
_cell_angle_gamma                90
_cell_volume                     6590(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3949
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.722
_cell_measurement_theta_min      4.718
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.911
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9112
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_unetI/netI     0.1496
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42709
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.643
_diffrn_reflns_theta_min         1.858
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9575
_reflns_number_total             15299
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         15299
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0935
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²+20.6712P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1894
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O13W-H13A = O13W-H13B
 0.9 with sigma of 0.02
 H13B-H13A
 1.4 with sigma of 0.02
3. Others
 Sof(O1W')=Sof(H1WC)=Sof(H1WD)=1-FVAR(1)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(1)
4.a Free rotating group:
 O8W(H8WA,H8WB), O12W(H12A,H12B), O1W(H1WA,H1WB), O10W(H10C,H10D), O1W'(H1WC,
 H1WD), O14W(H14A,H14B), O2W(H2WA,H2WB), O18W(H13A,H18A,H18B), O3W(H3WA,H3WB),
 O11W(H11C,H11D), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O15W(H15A,H15B), O6W(H6WA,
 H6WB), O7W(H7WA,H7WB), O9W(H9WA,H9WB)
4.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C27(H27),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C39(H39),
 C40(H40), C41(H41), C43(H43), C46(H46), C47(H47), C48(H48)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.61042(6) 0.84488(4) 0.41947(3) 0.01344(17) Uani 1 1 d . . . . .
Ni2 Ni 0.70431(6) 0.52634(4) 0.34816(3) 0.01360(17) Uani 1 1 d . . . . .
Ni3 Ni 1.10362(6) 0.36684(4) 0.35296(3) 0.01607(18) Uani 1 1 d . . . . .
O1 O 0.3214(3) 0.7654(2) 0.37091(19) 0.0314(11) Uani 1 1 d . . . . .
O2 O 0.3878(3) 0.5555(2) 0.33221(17) 0.0217(10) Uani 1 1 d . . . . .
O3 O 0.8059(3) 0.8615(2) 0.29909(16) 0.0232(10) Uani 1 1 d . . . . .
O4 O 0.8494(3) 0.6478(2) 0.24712(16) 0.0222(10) Uani 1 1 d . . . . .
O5 O 0.7509(3) 0.7565(2) 0.56066(16) 0.0225(10) Uani 1 1 d . . . . .
O6 O 0.7787(4) 0.5221(2) 0.51736(16) 0.0268(11) Uani 1 1 d . . . . .
O7 O 1.1411(3) 0.4553(2) 0.32243(17) 0.0252(10) Uani 1 1 d . . . . .
H7A H 1.1617 0.4830 0.3491 0.038 Uiso 1 1 d GR . . . .
H7B H 1.0869 0.4725 0.3025 0.038 Uiso 1 1 d GR . . . .
O8 O 1.2157(3) 0.3303(2) 0.30891(17) 0.0227(10) Uani 1 1 d . . . . .
H8A H 1.2233 0.2883 0.3153 0.034 Uiso 1 1 d GR . . . .
H8B H 1.2745 0.3501 0.3185 0.034 Uiso 1 1 d GR . . . .
O8W O 0.9515(3) 0.7652(2) 0.28461(18) 0.0244(10) Uani 1 1 d . . . . .
H8WA H 0.9219 0.7284 0.2744 0.037 Uiso 1 1 d G . . . .
H8WB H 0.9054 0.7926 0.2936 0.037 Uiso 1 1 d G . . . .
O9 O 1.2164(3) 0.3754(2) 0.41776(16) 0.0224(10) Uani 1 1 d . . . . .
H9A H 1.2255 0.4166 0.4259 0.034 Uiso 1 1 d GR . . . .
H9B H 1.2736 0.3591 0.4090 0.034 Uiso 1 1 d GR . . . .
O10 O 1.0686(3) 0.2797(2) 0.38839(18) 0.0257(10) Uani 1 1 d . . . . .
H10A H 1.0353 0.2541 0.3639 0.039 Uiso 1 1 d GR . . . .
H10B H 1.0294 0.2869 0.4143 0.039 Uiso 1 1 d GR . . . .
O11 O 0.9905(3) 0.3469(2) 0.29095(16) 0.0246(10) Uani 1 1 d . . . . .
H11A H 0.9628 0.3837 0.2780 0.037 Uiso 1 1 d GR . . . .
H11B H 0.9421 0.3227 0.3028 0.037 Uiso 1 1 d GR . . . .
N1 N 0.4821(4) 0.8734(2) 0.45552(19) 0.0164(11) Uani 1 1 d . . . . .
N2 N 0.3946(4) 0.9295(2) 0.5202(2) 0.0231(12) Uani 1 1 d . . . . .
N3 N 0.4941(4) 0.7934(2) 0.37444(18) 0.0159(11) Uani 1 1 d . . . . .
N4 N 0.5603(4) 0.5685(2) 0.32423(18) 0.0130(10) Uani 1 1 d . . . . .
N5 N 0.5512(4) 0.3393(3) 0.3769(2) 0.0257(12) Uani 1 1 d . . . . .
N6 N 0.6011(4) 0.4479(2) 0.35775(19) 0.0166(11) Uani 1 1 d . . . . .
N7 N 0.5982(4) 0.9230(2) 0.36485(19) 0.0158(11) Uani 1 1 d . . . . .
N8 N 0.5364(4) 1.0262(3) 0.3303(2) 0.0249(12) Uani 1 1 d . . . . .
N9 N 0.7273(4) 0.8243(2) 0.37276(18) 0.0134(10) Uani 1 1 d . . . . .
N10 N 0.7962(4) 0.6005(2) 0.32401(19) 0.0157(11) Uani 1 1 d . . . . .
N11 N 0.6982(5) 0.4325(3) 0.1879(2) 0.0370(15) Uani 1 1 d . . . . .
N12 N 0.7226(4) 0.4978(2) 0.2681(2) 0.0200(11) Uani 1 1 d . . . . .
N13 N 0.7202(4) 0.8949(2) 0.4733(2) 0.0188(11) Uani 1 1 d . . . . .
N14 N 0.8446(5) 0.9779(3) 0.4972(2) 0.0331(14) Uani 1 1 d . . . . .
N15 N 0.6477(4) 0.7751(2) 0.47982(19) 0.0161(11) Uani 1 1 d . . . . .
N16 N 0.7039(4) 0.5494(2) 0.43086(19) 0.0148(10) Uani 1 1 d . . . . .
N17 N 0.9876(4) 0.4118(2) 0.39302(19) 0.0184(11) Uani 1 1 d . . . . .
N18 N 0.8361(4) 0.4750(2) 0.38677(18) 0.0135(10) Uani 1 1 d . . . . .
C1 C 0.3947(5) 0.8423(3) 0.4363(2) 0.0169(13) Uani 1 1 d . . . . .
C2 C 0.4768(5) 0.9144(3) 0.4965(2) 0.0223(14) Uani 1 1 d . . . . .
H2 H 0.5393 0.9353 0.5104 0.027 Uiso 1 1 calc R . . . .
C3 C 0.3092(5) 0.8973(3) 0.5017(3) 0.0267(15) Uani 1 1 d . . . . .
H3 H 0.2485 0.9047 0.5184 0.032 Uiso 1 1 calc R . . . .
C4 C 0.3056(5) 0.8531(3) 0.4589(2) 0.0228(14) Uani 1 1 d . . . . .
H4 H 0.2436 0.8312 0.4459 0.027 Uiso 1 1 calc R . . . .
C5 C 0.4008(5) 0.7961(3) 0.3901(2) 0.0194(13) Uani 1 1 d . . . . .
C6 C 0.5100(4) 0.7476(3) 0.3328(2) 0.0140(12) Uani 1 1 d . . . . .
C7 C 0.5209(4) 0.7677(3) 0.2807(2) 0.0159(13) Uani 1 1 d . . . . .
H7 H 0.5127 0.8125 0.2711 0.019 Uiso 1 1 calc R . . . .
C8 C 0.5443(5) 0.7216(3) 0.2421(2) 0.0198(13) Uani 1 1 d . . . . .
H8 H 0.5521 0.7352 0.2062 0.024 Uiso 1 1 calc R . . . .
C9 C 0.5561(4) 0.6561(3) 0.2565(2) 0.0174(13) Uani 1 1 d . . . . .
H9 H 0.5728 0.6250 0.2305 0.021 Uiso 1 1 calc R . . . .
C10 C 0.5437(4) 0.6363(3) 0.3084(2) 0.0160(12) Uani 1 1 d . . . . .
C11 C 0.5189(4) 0.6812(3) 0.3461(2) 0.0166(13) Uani 1 1 d . . . . .
H11 H 0.5077 0.6671 0.3814 0.020 Uiso 1 1 calc R . . . .
C12 C 0.4798(5) 0.5363(3) 0.3355(2) 0.0176(13) Uani 1 1 d . . . . .
C13 C 0.5017(5) 0.4670(3) 0.3510(2) 0.0173(13) Uani 1 1 d . . . . .
C14 C 0.4248(5) 0.4229(3) 0.3581(3) 0.0243(15) Uani 1 1 d . . . . .
H14 H 0.3547 0.4361 0.3543 0.029 Uiso 1 1 calc R . . . .
C15 C 0.4526(5) 0.3581(3) 0.3709(3) 0.0276(15) Uani 1 1 d . . . . .
H15 H 0.4004 0.3270 0.3755 0.033 Uiso 1 1 calc R . . . .
C16 C 0.6200(5) 0.3859(3) 0.3708(3) 0.0235(14) Uani 1 1 d . . . . .
H16 H 0.6904 0.3733 0.3764 0.028 Uiso 1 1 calc R . . . .
C17 C 0.6664(5) 0.9216(3) 0.3283(2) 0.0169(13) Uani 1 1 d . . . . .
C18 C 0.5378(5) 0.9747(3) 0.3634(2) 0.0222(14) Uani 1 1 d . . . . .
H18 H 0.4894 0.9755 0.3891 0.027 Uiso 1 1 calc R . . . .
C19 C 0.6034(5) 1.0229(3) 0.2941(3) 0.0281(16) Uani 1 1 d . . . . .
H19 H 0.6056 1.0581 0.2692 0.034 Uiso 1 1 calc R . . . .
C20 C 0.6706(5) 0.9705(3) 0.2907(3) 0.0244(14) Uani 1 1 d . . . . .
H20 H 0.7168 0.9688 0.2639 0.029 Uiso 1 1 calc R . . . .
C21 C 0.7392(4) 0.8634(3) 0.3323(2) 0.0145(12) Uani 1 1 d . . . . .
C22 C 0.7936(4) 0.7688(3) 0.3798(2) 0.0145(12) Uani 1 1 d . . . . .
C23 C 0.8772(5) 0.7674(3) 0.4187(2) 0.0199(14) Uani 1 1 d . . . . .
H23 H 0.8945 0.8050 0.4403 0.024 Uiso 1 1 calc R . . . .
C24 C 0.9368(5) 0.7111(3) 0.4264(2) 0.0220(14) Uani 1 1 d . . . . .
H24 H 0.9953 0.7103 0.4530 0.026 Uiso 1 1 calc R . . . .
C25 C 0.9105(5) 0.6559(3) 0.3952(2) 0.0202(13) Uani 1 1 d . . . . .
H25 H 0.9500 0.6170 0.4010 0.024 Uiso 1 1 calc R . . . .
C26 C 0.8268(4) 0.6574(3) 0.3555(2) 0.0140(12) Uani 1 1 d . . . . .
C27 C 0.7686(5) 0.7140(3) 0.3478(2) 0.0179(13) Uani 1 1 d . . . . .
H27 H 0.7113 0.7154 0.3204 0.021 Uiso 1 1 calc R . . . .
C28 C 0.8085(4) 0.6030(3) 0.2728(2) 0.0160(13) Uani 1 1 d . . . . .
C29 C 0.7707(5) 0.5429(3) 0.2410(2) 0.0178(13) Uani 1 1 d . . . . .
C30 C 0.7861(5) 0.5339(4) 0.1874(2) 0.0286(16) Uani 1 1 d . . . . .
H30 H 0.8220 0.5652 0.1685 0.034 Uiso 1 1 calc R . . . .
C31 C 0.7475(6) 0.4775(4) 0.1624(3) 0.0370(18) Uani 1 1 d . . . . .
H31 H 0.7564 0.4706 0.1254 0.044 Uiso 1 1 calc R . . . .
C32 C 0.6891(5) 0.4453(3) 0.2394(3) 0.0271(15) Uani 1 1 d . . . . .
H32 H 0.6545 0.4132 0.2582 0.032 Uiso 1 1 calc R . . . .
C33 C 0.7595(5) 0.8585(3) 0.5161(2) 0.0186(13) Uani 1 1 d . . . . .
C34 C 0.7642(5) 0.9521(3) 0.4668(3) 0.0267(15) Uani 1 1 d . . . . .
H34 H 0.7350 0.9777 0.4370 0.032 Uiso 1 1 calc R . . . .
C35 C 0.8797(5) 0.9416(3) 0.5408(3) 0.0351(18) Uani 1 1 d . . . . .
H35 H 0.9349 0.9584 0.5652 0.042 Uiso 1 1 calc R . . . .
C36 C 0.8403(5) 0.8824(3) 0.5516(3) 0.0244(15) Uani 1 1 d . . . . .
H36 H 0.8673 0.8580 0.5827 0.029 Uiso 1 1 calc R . . . .
C37 C 0.7158(4) 0.7914(3) 0.5204(2) 0.0141(12) Uani 1 1 d . . . . .
C38 C 0.6112(4) 0.7087(3) 0.4779(2) 0.0150(12) Uani 1 1 d . . . . .
C39 C 0.5147(5) 0.6931(3) 0.4913(2) 0.0198(14) Uani 1 1 d . . . . .
H39 H 0.4724 0.7257 0.5045 0.024 Uiso 1 1 calc R . . . .
C40 C 0.4805(5) 0.6293(3) 0.4851(2) 0.0210(14) Uani 1 1 d . . . . .
H40 H 0.4138 0.6185 0.4940 0.025 Uiso 1 1 calc R . . . .
C41 C 0.5412(5) 0.5805(3) 0.4662(2) 0.0187(13) Uani 1 1 d . . . . .
H41 H 0.5166 0.5368 0.4624 0.022 Uiso 1 1 calc R . . . .
C42 C 0.6375(5) 0.5964(3) 0.4531(2) 0.0155(13) Uani 1 1 d . . . . .
C43 C 0.6744(4) 0.6609(3) 0.4603(2) 0.0150(12) Uani 1 1 d . . . . .
H43 H 0.7422 0.6715 0.4530 0.018 Uiso 1 1 calc R . . . .
C44 C 0.7672(4) 0.5174(3) 0.4658(2) 0.0157(13) Uani 1 1 d . . . . .
C45 C 0.8412(4) 0.4744(3) 0.4411(2) 0.0145(12) Uani 1 1 d . . . . .
C46 C 0.9154(5) 0.4388(3) 0.4727(3) 0.0211(14) Uani 1 1 d . . . . .
H46 H 0.9166 0.4368 0.5110 0.025 Uiso 1 1 calc R . . . .
C47 C 0.9870(5) 0.4066(3) 0.4466(2) 0.0202(14) Uani 1 1 d . . . . .
H47 H 1.0372 0.3801 0.4670 0.024 Uiso 1 1 calc R . . . .
C48 C 0.9107(5) 0.4443(3) 0.3653(2) 0.0175(13) Uani 1 1 d . . . . .
H48 H 0.9092 0.4457 0.3269 0.021 Uiso 1 1 calc R . . . .
O16W O 1.2081(6) 0.6775(3) 0.4426(2) 0.0659(19) Uani 1 1 d . . . . .
O12W O 0.8303(5) 0.2996(3) 0.3430(2) 0.0473(14) Uani 1 1 d . . . . .
H12A H 0.8001 0.2658 0.3270 0.071 Uiso 1 1 d G . . . .
H12B H 0.8487 0.2906 0.3771 0.071 Uiso 1 1 d G . . . .
O1W O 1.1253(14) 0.8169(14) 0.3485(12) 0.077(8) Uani 0.66(5) 1 d . . P A 1
H1WA H 1.0875 0.8062 0.3186 0.116 Uiso 0.66(5) 1 d G . P A 1
H1WB H 1.1843 0.7968 0.3502 0.116 Uiso 0.66(5) 1 d G . P A 1
O10W O 1.0715(4) 0.4677(3) 0.1565(2) 0.0455(14) Uani 1 1 d . . . . .
H10C H 1.1137 0.4864 0.1366 0.068 Uiso 1 1 d G . . . .
H10D H 1.0989 0.4317 0.1701 0.068 Uiso 1 1 d G . . . .
O1W' O 1.1182(14) 0.782(2) 0.3700(11) 0.034(10) Uani 0.34(5) 1 d . . P A 2
H1WC H 1.1112 0.7840 0.3347 0.051 Uiso 0.34(5) 1 d G . P A 2
H1WD H 1.1797 0.7683 0.3817 0.051 Uiso 0.34(5) 1 d G . P A 2
O14W O 1.0805(4) 0.6403(3) 0.2791(3) 0.0618(18) Uani 1 1 d . . . . .
H14A H 1.0426 0.6529 0.3038 0.093 Uiso 1 1 d G . . . .
H14B H 1.1434 0.6538 0.2877 0.093 Uiso 1 1 d G . . . .
O2W O 0.7254(4) 0.7041(2) 0.16391(18) 0.0294(11) Uani 1 1 d . . . . .
H2WA H 0.7524 0.7056 0.1335 0.044 Uiso 1 1 d G . . . .
H2WB H 0.7657 0.6822 0.1878 0.044 Uiso 1 1 d G . . . .
O18W O 0.2267(4) 0.5522(2) 0.39358(18) 0.0329(11) Uani 1 1 d . . . . .
H13A H 1.0876 0.8651 0.5531 0.049 Uiso 1 1 d DG . . . .
H18A H 0.2376 0.5319 0.4245 0.049 Uiso 1 1 d G . . . .
H18B H 0.2852 0.5603 0.3815 0.049 Uiso 1 1 d G . . . .
O3W O 0.5585(4) 0.6304(3) 0.11239(19) 0.0376(12) Uani 1 1 d . . . . .
H3WA H 0.6053 0.6493 0.1350 0.056 Uiso 1 1 d G . . . .
H3WB H 0.5863 0.6160 0.0845 0.056 Uiso 1 1 d G . . . .
O11W O 0.2654(4) 0.6778(3) 0.1828(2) 0.0458(14) Uani 1 1 d . . . . .
H11C H 0.2845 0.6845 0.2171 0.069 Uiso 1 1 d G . . . .
H11D H 0.3195 0.6735 0.1658 0.069 Uiso 1 1 d G . . . .
O4W O 1.0078(4) 0.5166(3) 0.2531(2) 0.0432(14) Uani 1 1 d . . . . .
H4WA H 1.0188 0.5580 0.2593 0.065 Uiso 1 1 d G . . . .
H4WB H 1.0209 0.5071 0.2205 0.065 Uiso 1 1 d G . . . .
O13W O 1.0689(5) 0.8463(4) 0.5209(3) 0.0602(17) Uani 1 1 d D . . . .
H13B H 1.118(6) 0.817(4) 0.518(3) 0.11(5) Uiso 1 1 d D . . . .
O5W O 1.0649(5) 0.9069(3) 0.4163(2) 0.0566(17) Uani 1 1 d . . . . .
H5WA H 1.0914 0.8744 0.4001 0.085 Uiso 1 1 d G . . . .
H5WB H 1.0165 0.9250 0.3942 0.085 Uiso 1 1 d G . . . .
O15W O 0.9882(5) 0.6677(3) 0.1638(2) 0.0536(16) Uani 1 1 d . . . . .
H15A H 1.0479 0.6617 0.1523 0.080 Uiso 1 1 d G . . . .
H15B H 0.9931 0.6600 0.1984 0.080 Uiso 1 1 d G . . . .
O6W O 0.2855(4) 0.6668(2) 0.29343(18) 0.0279(11) Uani 1 1 d . . . . .
H6WA H 0.3256 0.6374 0.3100 0.042 Uiso 1 1 d G . . . .
H6WB H 0.2958 0.7042 0.3099 0.042 Uiso 1 1 d G . . . .
O17W O 1.1454(5) 0.5877(3) 0.1208(2) 0.067(2) Uani 1 1 d . . . . .
O7W O 1.1978(5) 0.7314(3) 0.5433(2) 0.0530(16) Uani 1 1 d . . . . .
H7WA H 1.2484 0.7561 0.5571 0.080 Uiso 1 1 d G . . . .
H7WB H 1.2175 0.7080 0.5172 0.080 Uiso 1 1 d G . . . .
O9W O 0.3845(4) 0.7112(3) 0.0997(2) 0.0410(13) Uani 1 1 d . . . . .
H9WA H 0.4352 0.6857 0.0937 0.061 Uiso 1 1 d G . . . .
H9WB H 0.4073 0.7507 0.1058 0.061 Uiso 1 1 d G . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.076(5) . ?
Ni1 N3 2.067(5) . ?
Ni1 N7 2.089(5) . ?
Ni1 N9 2.066(5) . ?
Ni1 N13 2.107(5) . ?
Ni1 N15 2.085(5) . ?
Ni2 N4 2.093(5) . ?
Ni2 N6 2.127(5) . ?
Ni2 N10 2.068(5) . ?
Ni2 N12 2.110(5) . ?
Ni2 N16 2.106(5) . ?
Ni2 N18 2.145(5) . ?
Ni3 O7 2.043(4) . ?
Ni3 O8 2.067(4) . ?
Ni3 O9 2.058(4) . ?
Ni3 O10 2.062(4) . ?
Ni3 O11 2.046(4) . ?
Ni3 N17 2.118(5) . ?
O1 C5 1.258(7) . ?
O2 C12 1.259(7) . ?
O3 C21 1.269(7) . ?
O4 C28 1.269(7) . ?
O5 C37 1.270(7) . ?
O6 C44 1.273(7) . ?
O7 H7A 0.8883 . ?
O7 H7B 0.8885 . ?
O8 H8A 0.8775 . ?
O8 H8B 0.8774 . ?
O8W H8WA 0.8704 . ?
O8W H8WB 0.8701 . ?
O9 H9A 0.8704 . ?
O9 H9B 0.8706 . ?
O10 H10A 0.8793 . ?
O10 H10B 0.8807 . ?
O11 H11A 0.8797 . ?
O11 H11B 0.8801 . ?
N1 C1 1.346(7) . ?
N1 C2 1.325(8) . ?
N2 C2 1.321(8) . ?
N2 C3 1.331(8) . ?
N3 C5 1.323(8) . ?
N3 C6 1.428(7) . ?
N4 C10 1.449(7) . ?
N4 C12 1.301(8) . ?
N5 C15 1.337(8) . ?
N5 C16 1.332(8) . ?
N6 C13 1.349(7) . ?
N6 C16 1.326(7) . ?
N7 C17 1.345(7) . ?
N7 C18 1.318(8) . ?
N8 C18 1.334(8) . ?
N8 C19 1.328(8) . ?
N9 C21 1.306(7) . ?
N9 C22 1.427(7) . ?
N10 C26 1.432(7) . ?
N10 C28 1.301(7) . ?
N11 C31 1.325(9) . ?
N11 C32 1.323(8) . ?
N12 C29 1.341(8) . ?
N12 C32 1.334(8) . ?
N13 C33 1.348(7) . ?
N13 C34 1.322(8) . ?
N14 C34 1.328(8) . ?
N14 C35 1.347(9) . ?
N15 C37 1.307(7) . ?
N15 C38 1.438(7) . ?
N16 C42 1.446(7) . ?
N16 C44 1.303(7) . ?
N17 C47 1.335(7) . ?
N17 C48 1.329(7) . ?
N18 C45 1.341(7) . ?
N18 C48 1.323(7) . ?
C1 C4 1.369(8) . ?
C1 C5 1.495(8) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.391(9) . ?
C4 H4 0.9500 . ?
C6 C7 1.380(8) . ?
C6 C11 1.398(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.402(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.377(8) . ?
C10 C11 1.377(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.488(8) . ?
C13 C14 1.376(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.401(9) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C20 1.373(8) . ?
C17 C21 1.521(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.395(9) . ?
C20 H20 0.9500 . ?
C22 C23 1.371(8) . ?
C22 C27 1.389(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(8) . ?
C26 C27 1.388(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.512(8) . ?
C29 C30 1.380(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.376(10) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C36 1.384(8) . ?
C33 C37 1.495(8) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.356(9) . ?
C36 H36 0.9500 . ?
C38 C39 1.379(8) . ?
C38 C43 1.385(8) . ?
C39 H39 0.9500 . ?
C39 C40 1.382(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(8) . ?
C41 H41 0.9500 . ?
C41 C42 1.376(8) . ?
C42 C43 1.408(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.493(8) . ?
C45 C46 1.381(8) . ?
C46 H46 0.9500 . ?
C46 C47 1.368(9) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
O12W H12A 0.8695 . ?
O12W H12B 0.8705 . ?
O1W H1WA 0.8701 . ?
O1W H1WB 0.8702 . ?
O10W H10C 0.8703 . ?
O10W H10D 0.8698 . ?
O1W' H1WC 0.8706 . ?
O1W' H1WD 0.8704 . ?
O14W H14A 0.8699 . ?
O14W H14B 0.8697 . ?
O2W H2WA 0.8704 . ?
O2W H2WB 0.8697 . ?
O18W H18A 0.8696 . ?
O18W H18B 0.8695 . ?
O3W H3WA 0.8702 . ?
O3W H3WB 0.8702 . ?
O11W H11C 0.8699 . ?
O11W H11D 0.8702 . ?
O4W H4WA 0.8702 . ?
O4W H4WB 0.8697 . ?
O13W H13A 0.8929 . ?
O13W H13B 0.89(2) . ?
O5W H5WA 0.8703 . ?
O5W H5WB 0.8694 . ?
O15W H15A 0.8698 . ?
O15W H15B 0.8699 . ?
O6W H6WA 0.8699 . ?
O6W H6WB 0.8703 . ?
O7W H7WA 0.8702 . ?
O7W H7WB 0.8692 . ?
O9W H9WA 0.8704 . ?
O9W H9WB 0.8695 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N7 93.45(19) . . ?
N1 Ni1 N13 96.67(19) . . ?
N1 Ni1 N15 90.90(19) . . ?
N3 Ni1 N1 78.17(19) . . ?
N3 Ni1 N7 92.47(18) . . ?
N3 Ni1 N13 173.4(2) . . ?
N3 Ni1 N15 97.74(19) . . ?
N7 Ni1 N13 91.99(18) . . ?
N9 Ni1 N1 170.82(18) . . ?
N9 Ni1 N3 97.99(19) . . ?
N9 Ni1 N7 78.31(19) . . ?
N9 Ni1 N13 87.72(19) . . ?
N9 Ni1 N15 97.91(19) . . ?
N15 Ni1 N7 169.53(19) . . ?
N15 Ni1 N13 78.03(19) . . ?
N4 Ni2 N6 77.37(18) . . ?
N4 Ni2 N12 92.54(19) . . ?
N4 Ni2 N16 94.53(18) . . ?
N4 Ni2 N18 167.77(18) . . ?
N6 Ni2 N18 93.89(18) . . ?
N10 Ni2 N4 98.58(18) . . ?
N10 Ni2 N6 169.63(18) . . ?
N10 Ni2 N12 78.24(19) . . ?
N10 Ni2 N16 100.70(19) . . ?
N10 Ni2 N18 91.42(18) . . ?
N12 Ni2 N6 92.30(19) . . ?
N12 Ni2 N18 96.39(18) . . ?
N16 Ni2 N6 89.20(18) . . ?
N16 Ni2 N12 172.93(19) . . ?
N16 Ni2 N18 76.61(18) . . ?
O7 Ni3 O8 84.74(18) . . ?
O7 Ni3 O9 91.88(17) . . ?
O7 Ni3 O10 176.54(18) . . ?
O7 Ni3 O11 94.67(18) . . ?
O7 Ni3 N17 90.35(19) . . ?
O8 Ni3 N17 174.65(18) . . ?
O9 Ni3 O8 87.51(17) . . ?
O9 Ni3 O10 85.13(17) . . ?
O9 Ni3 N17 94.79(18) . . ?
O10 Ni3 O8 96.86(18) . . ?
O10 Ni3 N17 88.16(19) . . ?
O11 Ni3 O8 91.44(17) . . ?
O11 Ni3 O9 173.24(18) . . ?
O11 Ni3 O10 88.37(18) . . ?
O11 Ni3 N17 86.84(18) . . ?
Ni3 O7 H7A 110.7 . . ?
Ni3 O7 H7B 110.3 . . ?
H7A O7 H7B 108.2 . . ?
Ni3 O8 H8A 109.4 . . ?
Ni3 O8 H8B 110.0 . . ?
H8A O8 H8B 108.9 . . ?
H8WA O8W H8WB 109.5 . . ?
Ni3 O9 H9A 109.3 . . ?
Ni3 O9 H9B 109.3 . . ?
H9A O9 H9B 109.4 . . ?
Ni3 O10 H10A 109.7 . . ?
Ni3 O10 H10B 110.2 . . ?
H10A O10 H10B 108.7 . . ?
Ni3 O11 H11A 109.6 . . ?
Ni3 O11 H11B 110.2 . . ?
H11A O11 H11B 108.7 . . ?
C1 N1 Ni1 114.2(4) . . ?
C2 N1 Ni1 128.7(4) . . ?
C2 N1 C1 117.0(5) . . ?
C2 N2 C3 115.1(5) . . ?
C5 N3 Ni1 117.8(4) . . ?
C5 N3 C6 117.1(5) . . ?
C6 N3 Ni1 124.4(4) . . ?
C10 N4 Ni2 125.0(4) . . ?
C12 N4 Ni2 117.0(4) . . ?
C12 N4 C10 116.3(5) . . ?
C16 N5 C15 115.9(6) . . ?
C13 N6 Ni2 112.5(4) . . ?
C16 N6 Ni2 130.3(4) . . ?
C16 N6 C13 117.1(5) . . ?
C17 N7 Ni1 114.5(4) . . ?
C18 N7 Ni1 129.2(4) . . ?
C18 N7 C17 116.1(5) . . ?
C19 N8 C18 114.4(6) . . ?
C21 N9 Ni1 118.0(4) . . ?
C21 N9 C22 117.1(5) . . ?
C22 N9 Ni1 124.9(4) . . ?
C26 N10 Ni2 124.9(4) . . ?
C28 N10 Ni2 117.0(4) . . ?
C28 N10 C26 116.3(5) . . ?
C32 N11 C31 115.3(6) . . ?
C29 N12 Ni2 113.2(4) . . ?
C32 N12 Ni2 131.2(4) . . ?
C32 N12 C29 115.5(5) . . ?
C33 N13 Ni1 113.6(4) . . ?
C34 N13 Ni1 128.8(4) . . ?
C34 N13 C33 116.9(5) . . ?
C34 N14 C35 114.1(6) . . ?
C37 N15 Ni1 117.3(4) . . ?
C37 N15 C38 117.4(5) . . ?
C38 N15 Ni1 125.1(4) . . ?
C42 N16 Ni2 126.2(3) . . ?
C44 N16 Ni2 117.5(4) . . ?
C44 N16 C42 116.2(5) . . ?
C47 N17 Ni3 121.4(4) . . ?
C48 N17 Ni3 121.0(4) . . ?
C48 N17 C47 117.6(5) . . ?
C45 N18 Ni2 113.3(4) . . ?
C48 N18 Ni2 130.1(4) . . ?
C48 N18 C45 116.6(5) . . ?
N1 C1 C4 120.4(5) . . ?
N1 C1 C5 116.9(5) . . ?
C4 C1 C5 122.8(5) . . ?
N1 C2 H2 116.3 . . ?
N2 C2 N1 127.4(6) . . ?
N2 C2 H2 116.3 . . ?
N2 C3 H3 118.8 . . ?
N2 C3 C4 122.4(6) . . ?
C4 C3 H3 118.8 . . ?
C1 C4 C3 117.7(6) . . ?
C1 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
O1 C5 N3 128.1(6) . . ?
O1 C5 C1 119.2(6) . . ?
N3 C5 C1 112.6(5) . . ?
C7 C6 N3 121.4(5) . . ?
C7 C6 C11 119.7(5) . . ?
C11 C6 N3 118.8(5) . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.6(5) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.9(6) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(6) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 N4 120.3(5) . . ?
C9 C10 C11 120.0(6) . . ?
C11 C10 N4 119.6(5) . . ?
C6 C11 H11 119.8 . . ?
C10 C11 C6 120.5(5) . . ?
C10 C11 H11 119.8 . . ?
O2 C12 N4 128.2(5) . . ?
O2 C12 C13 117.9(5) . . ?
N4 C12 C13 113.8(5) . . ?
N6 C13 C12 117.4(5) . . ?
N6 C13 C14 120.2(6) . . ?
C14 C13 C12 122.4(6) . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.3(6) . . ?
C15 C14 H14 120.8 . . ?
N5 C15 C14 121.3(6) . . ?
N5 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
N5 C16 H16 116.4 . . ?
N6 C16 N5 127.1(6) . . ?
N6 C16 H16 116.4 . . ?
N7 C17 C20 121.7(6) . . ?
N7 C17 C21 115.6(5) . . ?
C20 C17 C21 122.7(6) . . ?
N7 C18 N8 128.1(6) . . ?
N7 C18 H18 116.0 . . ?
N8 C18 H18 116.0 . . ?
N8 C19 H19 118.3 . . ?
N8 C19 C20 123.4(6) . . ?
C20 C19 H19 118.3 . . ?
C17 C20 C19 116.3(6) . . ?
C17 C20 H20 121.8 . . ?
C19 C20 H20 121.8 . . ?
O3 C21 N9 129.3(5) . . ?
O3 C21 C17 117.0(5) . . ?
N9 C21 C17 113.5(5) . . ?
C23 C22 N9 121.7(5) . . ?
C23 C22 C27 120.1(5) . . ?
C27 C22 N9 118.2(5) . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.1(5) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.8(5) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.1(5) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 N10 121.1(5) . . ?
C25 C26 C27 119.5(5) . . ?
C27 C26 N10 119.3(5) . . ?
C22 C27 H27 119.8 . . ?
C26 C27 C22 120.3(5) . . ?
C26 C27 H27 119.8 . . ?
O4 C28 N10 128.7(5) . . ?
O4 C28 C29 117.2(5) . . ?
N10 C28 C29 114.1(5) . . ?
N12 C29 C28 116.2(5) . . ?
N12 C29 C30 121.4(6) . . ?
C30 C29 C28 122.4(6) . . ?
C29 C30 H30 121.4 . . ?
C31 C30 C29 117.3(6) . . ?
C31 C30 H30 121.4 . . ?
N11 C31 C30 122.7(6) . . ?
N11 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
N11 C32 N12 127.8(6) . . ?
N11 C32 H32 116.1 . . ?
N12 C32 H32 116.1 . . ?
N13 C33 C36 120.0(6) . . ?
N13 C33 C37 116.6(5) . . ?
C36 C33 C37 123.2(5) . . ?
N13 C34 N14 127.6(6) . . ?
N13 C34 H34 116.2 . . ?
N14 C34 H34 116.2 . . ?
N14 C35 H35 118.3 . . ?
N14 C35 C36 123.4(6) . . ?
C36 C35 H35 118.3 . . ?
C33 C36 H36 121.0 . . ?
C35 C36 C33 117.9(6) . . ?
C35 C36 H36 121.0 . . ?
O5 C37 N15 127.9(5) . . ?
O5 C37 C33 117.8(5) . . ?
N15 C37 C33 114.3(5) . . ?
C39 C38 N15 121.3(5) . . ?
C39 C38 C43 120.6(5) . . ?
C43 C38 N15 118.0(5) . . ?
C38 C39 H39 120.5 . . ?
C38 C39 C40 119.0(6) . . ?
C40 C39 H39 120.5 . . ?
C39 C40 H40 119.2 . . ?
C39 C40 C41 121.6(6) . . ?
C41 C40 H40 119.2 . . ?
C40 C41 H41 120.5 . . ?
C42 C41 C40 119.0(6) . . ?
C42 C41 H41 120.5 . . ?
C41 C42 N16 122.7(5) . . ?
C41 C42 C43 120.0(5) . . ?
C43 C42 N16 117.3(5) . . ?
C38 C43 C42 119.6(5) . . ?
C38 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
O6 C44 N16 128.5(5) . . ?
O6 C44 C45 116.8(5) . . ?
N16 C44 C45 114.4(5) . . ?
N18 C45 C44 116.8(5) . . ?
N18 C45 C46 121.6(5) . . ?
C46 C45 C44 121.5(5) . . ?
C45 C46 H46 121.3 . . ?
C47 C46 C45 117.4(6) . . ?
C47 C46 H46 121.3 . . ?
N17 C47 C46 121.1(6) . . ?
N17 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
N17 C48 H48 117.3 . . ?
N18 C48 N17 125.3(5) . . ?
N18 C48 H48 117.3 . . ?
H12A O12W H12B 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
H10C O10W H10D 109.5 . . ?
H1WC O1W' H1WD 109.4 . . ?
H14A O14W H14B 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?
H18A O18W H18B 109.5 . . ?
H3WA O3W H3WB 109.5 . . ?
H11C O11W H11D 109.5 . . ?
H4WA O4W H4WB 109.5 . . ?
H13A O13W H13B 103.7 . . ?
H5WA O5W H5WB 109.5 . . ?
H15A O15W H15B 109.5 . . ?
H6WA O6W H6WB 109.5 . . ?
H7WA O7W H7WB 109.5 . . ?
H9WA O9W H9WB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C1 C4 175.6(5) . . . . ?
Ni1 N1 C1 C5 -4.0(6) . . . . ?
Ni1 N1 C2 N2 -176.8(5) . . . . ?
Ni1 N3 C5 O1 -174.9(5) . . . . ?
Ni1 N3 C5 C1 5.3(7) . . . . ?
Ni1 N3 C6 C7 -82.6(6) . . . . ?
Ni1 N3 C6 C11 94.7(6) . . . . ?
Ni1 N7 C17 C20 -177.8(5) . . . . ?
Ni1 N7 C17 C21 1.0(6) . . . . ?
Ni1 N7 C18 N8 175.0(5) . . . . ?
Ni1 N9 C21 O3 178.4(5) . . . . ?
Ni1 N9 C21 C17 3.5(6) . . . . ?
Ni1 N9 C22 C23 -81.0(6) . . . . ?
Ni1 N9 C22 C27 96.0(6) . . . . ?
Ni1 N13 C33 C36 173.0(5) . . . . ?
Ni1 N13 C33 C37 -3.3(7) . . . . ?
Ni1 N13 C34 N14 -168.4(5) . . . . ?
Ni1 N15 C37 O5 -178.7(5) . . . . ?
Ni1 N15 C37 C33 -1.7(7) . . . . ?
Ni1 N15 C38 C39 -80.9(6) . . . . ?
Ni1 N15 C38 C43 96.7(6) . . . . ?
Ni2 N4 C10 C9 81.6(6) . . . . ?
Ni2 N4 C10 C11 -96.1(6) . . . . ?
Ni2 N4 C12 O2 169.0(5) . . . . ?
Ni2 N4 C12 C13 -14.7(6) . . . . ?
Ni2 N6 C13 C12 3.2(6) . . . . ?
Ni2 N6 C13 C14 -177.3(4) . . . . ?
Ni2 N6 C16 N5 179.0(5) . . . . ?
Ni2 N10 C26 C25 83.4(6) . . . . ?
Ni2 N10 C26 C27 -93.6(6) . . . . ?
Ni2 N10 C28 O4 170.1(5) . . . . ?
Ni2 N10 C28 C29 -11.7(6) . . . . ?
Ni2 N12 C29 C28 3.6(6) . . . . ?
Ni2 N12 C29 C30 -177.6(5) . . . . ?
Ni2 N12 C32 N11 175.4(5) . . . . ?
Ni2 N16 C42 C41 87.1(6) . . . . ?
Ni2 N16 C42 C43 -91.8(6) . . . . ?
Ni2 N16 C44 O6 -178.4(5) . . . . ?
Ni2 N16 C44 C45 7.5(6) . . . . ?
Ni2 N18 C45 C44 -9.7(6) . . . . ?
Ni2 N18 C45 C46 174.1(4) . . . . ?
Ni2 N18 C48 N17 -177.4(4) . . . . ?
Ni3 N17 C47 C46 176.2(5) . . . . ?
Ni3 N17 C48 N18 -178.6(4) . . . . ?
O2 C12 C13 N6 -175.9(5) . . . . ?
O2 C12 C13 C14 4.7(8) . . . . ?
O4 C28 C29 N12 -176.4(5) . . . . ?
O4 C28 C29 C30 4.8(9) . . . . ?
O6 C44 C45 N18 -173.0(5) . . . . ?
O6 C44 C45 C46 3.2(8) . . . . ?
N1 C1 C4 C3 0.5(9) . . . . ?
N1 C1 C5 O1 179.4(5) . . . . ?
N1 C1 C5 N3 -0.7(8) . . . . ?
N2 C3 C4 C1 1.2(10) . . . . ?
N3 C6 C7 C8 175.1(5) . . . . ?
N3 C6 C11 C10 -174.0(5) . . . . ?
N4 C10 C11 C6 175.2(5) . . . . ?
N4 C12 C13 N6 7.4(7) . . . . ?
N4 C12 C13 C14 -172.1(6) . . . . ?
N6 C13 C14 C15 -1.5(9) . . . . ?
N7 C17 C20 C19 2.6(9) . . . . ?
N7 C17 C21 O3 -178.5(5) . . . . ?
N7 C17 C21 N9 -2.9(7) . . . . ?
N8 C19 C20 C17 -1.5(10) . . . . ?
N9 C22 C23 C24 176.4(6) . . . . ?
N9 C22 C27 C26 -175.8(5) . . . . ?
N10 C26 C27 C22 176.6(5) . . . . ?
N10 C28 C29 N12 5.1(7) . . . . ?
N10 C28 C29 C30 -173.6(6) . . . . ?
N12 C29 C30 C31 1.9(10) . . . . ?
N13 C33 C36 C35 -2.1(9) . . . . ?
N13 C33 C37 O5 -179.3(5) . . . . ?
N13 C33 C37 N15 3.3(8) . . . . ?
N14 C35 C36 C33 -0.4(11) . . . . ?
N15 C38 C39 C40 175.4(5) . . . . ?
N15 C38 C43 C42 -174.2(5) . . . . ?
N16 C42 C43 C38 175.7(5) . . . . ?
N16 C44 C45 N18 1.8(8) . . . . ?
N16 C44 C45 C46 178.0(5) . . . . ?
N18 C45 C46 C47 3.2(9) . . . . ?
C1 N1 C2 N2 -1.5(9) . . . . ?
C2 N1 C1 C4 -0.4(8) . . . . ?
C2 N1 C1 C5 -179.9(5) . . . . ?
C2 N2 C3 C4 -2.8(9) . . . . ?
C3 N2 C2 N1 3.1(10) . . . . ?
C4 C1 C5 O1 -0.1(9) . . . . ?
C4 C1 C5 N3 179.7(6) . . . . ?
C5 N3 C6 C7 107.2(7) . . . . ?
C5 N3 C6 C11 -75.5(7) . . . . ?
C5 C1 C4 C3 -180.0(6) . . . . ?
C6 N3 C5 O1 -4.0(9) . . . . ?
C6 N3 C5 C1 176.2(5) . . . . ?
C6 C7 C8 C9 0.1(9) . . . . ?
C7 C6 C11 C10 3.3(9) . . . . ?
C7 C8 C9 C10 0.8(9) . . . . ?
C8 C9 C10 N4 -177.3(5) . . . . ?
C8 C9 C10 C11 0.4(9) . . . . ?
C9 C10 C11 C6 -2.5(9) . . . . ?
C10 N4 C12 O2 3.2(9) . . . . ?
C10 N4 C12 C13 179.6(4) . . . . ?
C11 C6 C7 C8 -2.1(9) . . . . ?
C12 N4 C10 C9 -113.9(6) . . . . ?
C12 N4 C10 C11 68.4(7) . . . . ?
C12 C13 C14 C15 177.9(6) . . . . ?
C13 N6 C16 N5 1.7(9) . . . . ?
C13 C14 C15 N5 0.7(10) . . . . ?
C15 N5 C16 N6 -2.5(10) . . . . ?
C16 N5 C15 C14 1.2(9) . . . . ?
C16 N6 C13 C12 -179.0(5) . . . . ?
C16 N6 C13 C14 0.5(8) . . . . ?
C17 N7 C18 N8 -0.4(9) . . . . ?
C18 N7 C17 C20 -1.8(8) . . . . ?
C18 N7 C17 C21 177.0(5) . . . . ?
C18 N8 C19 C20 -0.4(9) . . . . ?
C19 N8 C18 N7 1.5(9) . . . . ?
C20 C17 C21 O3 0.3(8) . . . . ?
C20 C17 C21 N9 175.9(5) . . . . ?
C21 N9 C22 C23 101.9(6) . . . . ?
C21 N9 C22 C27 -81.1(7) . . . . ?
C21 C17 C20 C19 -176.1(5) . . . . ?
C22 N9 C21 O3 -4.3(9) . . . . ?
C22 N9 C21 C17 -179.2(5) . . . . ?
C22 C23 C24 C25 -0.8(10) . . . . ?
C23 C22 C27 C26 1.2(9) . . . . ?
C23 C24 C25 C26 1.6(10) . . . . ?
C24 C25 C26 N10 -177.9(6) . . . . ?
C24 C25 C26 C27 -1.0(9) . . . . ?
C25 C26 C27 C22 -0.4(9) . . . . ?
C26 N10 C28 O4 4.3(9) . . . . ?
C26 N10 C28 C29 -177.5(5) . . . . ?
C27 C22 C23 C24 -0.6(9) . . . . ?
C28 N10 C26 C25 -112.1(6) . . . . ?
C28 N10 C26 C27 70.9(7) . . . . ?
C28 C29 C30 C31 -179.4(6) . . . . ?
C29 N12 C32 N11 0.4(10) . . . . ?
C29 C30 C31 N11 -0.8(11) . . . . ?
C31 N11 C32 N12 0.6(11) . . . . ?
C32 N11 C31 C30 -0.3(11) . . . . ?
C32 N12 C29 C28 179.6(5) . . . . ?
C32 N12 C29 C30 -1.7(9) . . . . ?
C33 N13 C34 N14 1.4(10) . . . . ?
C34 N13 C33 C36 1.7(9) . . . . ?
C34 N13 C33 C37 -174.6(5) . . . . ?
C34 N14 C35 C36 3.1(11) . . . . ?
C35 N14 C34 N13 -3.7(10) . . . . ?
C36 C33 C37 O5 4.5(9) . . . . ?
C36 C33 C37 N15 -172.8(6) . . . . ?
C37 N15 C38 C39 105.0(7) . . . . ?
C37 N15 C38 C43 -77.5(7) . . . . ?
C37 C33 C36 C35 173.9(6) . . . . ?
C38 N15 C37 O5 -4.1(9) . . . . ?
C38 N15 C37 C33 172.9(5) . . . . ?
C38 C39 C40 C41 0.5(9) . . . . ?
C39 C38 C43 C42 3.4(8) . . . . ?
C39 C40 C41 C42 -0.3(9) . . . . ?
C40 C41 C42 N16 -177.2(5) . . . . ?
C40 C41 C42 C43 1.7(8) . . . . ?
C41 C42 C43 C38 -3.2(8) . . . . ?
C42 N16 C44 O6 -0.2(9) . . . . ?
C42 N16 C44 C45 -174.2(5) . . . . ?
C43 C38 C39 C40 -2.1(9) . . . . ?
C44 N16 C42 C41 -91.0(7) . . . . ?
C44 N16 C42 C43 90.2(6) . . . . ?
C44 C45 C46 C47 -172.8(5) . . . . ?
C45 N18 C48 N17 2.1(9) . . . . ?
C45 C46 C47 N17 2.8(9) . . . . ?
C47 N17 C48 N18 3.6(9) . . . . ?
C48 N17 C47 C46 -6.0(9) . . . . ?
C48 N18 C45 C44 170.7(5) . . . . ?
C48 N18 C45 C46 -5.6(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_j32_csm
_database_code_depnum_ccdc_archive 'CCDC 1551799'
_audit_update_record             
;
2017-07-17 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H24 Cu2 N12 O6, 8(H2 O)'
_chemical_formula_sum            'C32 H40 Cu2 N12 O14'
_chemical_formula_weight         943.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.397(6)
_cell_length_b                   11.832(3)
_cell_length_c                   15.242(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.617(5)
_cell_angle_gamma                90
_cell_volume                     4160.3(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16563
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      48.786
_cell_measurement_theta_min      4.610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11145
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_min         1.766
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2588
_reflns_number_total             3689
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3689
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0749
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0553P)²+45.8711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1861
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB), O4W(H4WA,H4WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C16(H16), C15(H15), C14(H14), C10(H10), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.30606(3) 0.00194(7) 0.13778(5) 0.0179(3) Uani 1 1 d . . . . .
O2 O 0.1985(2) 0.5829(4) 0.1208(3) 0.0269(12) Uani 1 1 d . . . . .
O3 O 0.3270(2) 0.3139(4) 0.2559(3) 0.0217(11) Uani 1 1 d . . . . .
O1 O 0.2654(3) -0.0497(4) 0.2393(3) 0.0276(12) Uani 1 1 d . . . . .
H1A H 0.2731 -0.0113 0.2866 0.08(4) Uiso 1 1 d G . . . .
H1B H 0.2295 -0.0619 0.2319 0.09(4) Uiso 1 1 d G . . . .
N1 N 0.1837(2) 0.6598(4) -0.1048(4) 0.0205(13) Uani 1 1 d . . . . .
N2 N 0.1584(3) 0.8520(5) -0.1339(4) 0.0260(14) Uani 1 1 d . . . . .
N3 N 0.1955(2) 0.4785(4) -0.0088(3) 0.0169(12) Uani 1 1 d . . . . .
N5 N 0.3843(2) 0.0381(4) 0.2349(3) 0.0192(12) Uani 1 1 d . . . . .
N6 N 0.4691(3) 0.0047(5) 0.3407(4) 0.0379(16) Uani 1 1 d . . . . .
N4 N 0.2931(2) 0.1620(4) 0.1645(3) 0.0158(12) Uani 1 1 d . . . . .
C4 C 0.1843(3) 0.6761(5) -0.0177(4) 0.0170(14) Uani 1 1 d . . . . .
C1 C 0.1712(3) 0.7487(5) -0.1598(4) 0.0244(16) Uani 1 1 d . . . . .
H1 H 0.1716 0.7372 -0.2200 0.029 Uiso 1 1 calc R . . . .
C2 C 0.1605(3) 0.8671(6) -0.0463(4) 0.0231(16) Uani 1 1 d . . . . .
H2 H 0.1526 0.9386 -0.0258 0.028 Uiso 1 1 calc R . . . .
C3 C 0.1736(3) 0.7813(5) 0.0145(5) 0.0222(15) Uani 1 1 d . . . . .
H3 H 0.1753 0.7939 0.0751 0.027 Uiso 1 1 calc R . . . .
H8 H 0.110(3) 0.353(6) 0.003(5) 0.027 Uiso 1 1 d R . . . .
C5 C 0.1943(3) 0.5715(5) 0.0387(4) 0.0163(14) Uani 1 1 d . . . . .
C6 C 0.1940(3) 0.3729(5) 0.0372(4) 0.0181(15) Uani 1 1 d . . . . .
C8 C 0.1417(3) 0.3183(6) 0.0333(5) 0.0254(16) Uani 1 1 d . . . . .
C7 C 0.2445(3) 0.3242(5) 0.0824(4) 0.0135(13) Uani 1 1 d . . . . .
H7 H 0.2797 0.3616 0.0858 0.016 Uiso 1 1 calc R . . . .
C13 C 0.3822(3) 0.1456(5) 0.2650(4) 0.0190(14) Uani 1 1 d . . . . .
C16 C 0.4281(3) -0.0268(6) 0.2748(5) 0.0274(17) Uani 1 1 d . . . . .
H16 H 0.4297 -0.1006 0.2543 0.033 Uiso 1 1 calc R . . . .
C15 C 0.4673(3) 0.1127(7) 0.3682(5) 0.0357(19) Uani 1 1 d . . . . .
H15 H 0.4960 0.1381 0.4136 0.043 Uiso 1 1 calc R . . . .
C14 C 0.4243(3) 0.1873(6) 0.3310(5) 0.0283(17) Uani 1 1 d . . . . .
H14 H 0.4239 0.2620 0.3498 0.034 Uiso 1 1 calc R . . . .
C12 C 0.3308(3) 0.2146(5) 0.2245(4) 0.0179(14) Uani 1 1 d . . . . .
C11 C 0.2420(3) 0.2193(5) 0.1226(4) 0.0178(14) Uani 1 1 d . . . . .
C10 C 0.1891(3) 0.1635(6) 0.1174(4) 0.0214(15) Uani 1 1 d . . . . .
H10 H 0.1875 0.0931 0.1440 0.026 Uiso 1 1 calc R . . . .
C9 C 0.1387(3) 0.2131(6) 0.0726(5) 0.0288(17) Uani 1 1 d . . . . .
H9 H 0.1033 0.1761 0.0689 0.035 Uiso 1 1 calc R . . . .
O2W O 0.4956(3) 0.4692(6) 0.1348(4) 0.0493(16) Uani 1 1 d . . . . .
H2WA H 0.5281 0.4682 0.1695 0.074 Uiso 1 1 d G . . . .
H2WB H 0.4709 0.4690 0.1704 0.074 Uiso 1 1 d G . . . .
O3W O 0.5151(3) 0.3477(5) -0.0133(4) 0.0569(18) Uani 1 1 d . . . . .
H3WA H 0.5102 0.3940 0.0279 0.085 Uiso 1 1 d G . . . .
H3WB H 0.5178 0.3852 -0.0601 0.085 Uiso 1 1 d G . . . .
O1W O 0.4052(2) 0.4750(4) 0.2359(4) 0.0391(14) Uani 1 1 d . . . . .
H1WA H 0.3813 0.4284 0.2558 0.059 Uiso 1 1 d G . . . .
H1WB H 0.3840 0.5360 0.2018 0.059 Uiso 1 1 d G . . . .
O4W O 0.0561(3) 0.6589(7) -0.0897(6) 0.079(3) Uani 1 1 d . . . . .
H4WA H 0.0323 0.6042 -0.0986 0.118 Uiso 1 1 d G . . . .
H4WB H 0.0397 0.7155 -0.0701 0.118 Uiso 1 1 d G . . . .


_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
Cu1 O1 2.041(5) . ?
Cu1 N1 2.004(5) 7 ?
Cu1 N3 1.974(5) 7 ?
Cu1 N5 2.195(6) . ?
Cu1 N4 1.971(5) . ?
O2 C5 1.247(7) . ?
O3 C12 1.277(7) . ?
O1 H1A 0.8460 . ?
O1 H1B 0.8410 . ?
N1 Cu1 2.003(5) 7 ?
N1 C4 1.339(8) . ?
N1 C1 1.345(8) . ?
N2 C1 1.335(8) . ?
N2 C2 1.340(9) . ?
N3 Cu1 1.974(5) 7 ?
N3 C5 1.319(8) . ?
N3 C6 1.436(8) . ?
N5 C13 1.356(8) . ?
N5 C16 1.342(9) . ?
N6 C16 1.321(9) . ?
N6 C15 1.346(10) . ?
N4 C12 1.316(8) . ?
N4 C11 1.429(8) . ?
C4 C3 1.376(9) . ?
C4 C5 1.503(8) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.375(9) . ?
C3 H3 0.9300 . ?
C6 C8 1.377(10) . ?
C6 C7 1.389(9) . ?
C8 H8 0.90(7) . ?
C8 C9 1.389(10) . ?
C7 H7 0.9300 . ?
C7 C11 1.389(9) . ?
C13 C14 1.376(10) . ?
C13 C12 1.499(9) . ?
C16 H16 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.386(10) . ?
C14 H14 0.9300 . ?
C11 C10 1.395(9) . ?
C10 H10 0.9300 . ?
C10 C9 1.390(10) . ?
C9 H9 0.9300 . ?
O2W H2WA 0.8517 . ?
O2W H2WB 0.8551 . ?
O3W H3WA 0.8563 . ?
O3W H3WB 0.8512 . ?
O1W H1WA 0.8766 . ?
O1W H1WB 0.9756 . ?
O4W H4WA 0.8498 . ?
O4W H4WB 0.8493 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N5 89.3(2) . . ?
N1 Cu1 O1 89.7(2) 7 . ?
N1 Cu1 N5 103.5(2) 7 . ?
N3 Cu1 O1 149.0(2) 7 . ?
N3 Cu1 N1 81.1(2) 7 7 ?
N3 Cu1 N5 121.5(2) 7 . ?
N4 Cu1 O1 91.4(2) . . ?
N4 Cu1 N1 177.0(2) . 7 ?
N4 Cu1 N3 96.6(2) . 7 ?
N4 Cu1 N5 79.2(2) . . ?
Cu1 O1 H1A 115.1 . . ?
Cu1 O1 H1B 122.0 . . ?
H1A O1 H1B 105.8 . . ?
C4 N1 Cu1 113.9(4) . 7 ?
C4 N1 C1 118.1(6) . . ?
C1 N1 Cu1 127.8(4) . 7 ?
C1 N2 C2 116.4(6) . . ?
C5 N3 Cu1 116.7(4) . 7 ?
C5 N3 C6 117.0(5) . . ?
C6 N3 Cu1 126.2(4) . 7 ?
C13 N5 Cu1 109.8(4) . . ?
C16 N5 Cu1 133.0(5) . . ?
C16 N5 C13 116.8(6) . . ?
C16 N6 C15 116.6(6) . . ?
C12 N4 Cu1 119.3(4) . . ?
C12 N4 C11 120.0(5) . . ?
C11 N4 Cu1 120.6(4) . . ?
N1 C4 C3 120.8(6) . . ?
N1 C4 C5 115.0(5) . . ?
C3 C4 C5 124.1(6) . . ?
N1 C1 H1 117.7 . . ?
N2 C1 N1 124.6(6) . . ?
N2 C1 H1 117.7 . . ?
N2 C2 H2 118.7 . . ?
N2 C2 C3 122.7(6) . . ?
C3 C2 H2 118.7 . . ?
C4 C3 H3 121.3 . . ?
C2 C3 C4 117.4(6) . . ?
C2 C3 H3 121.3 . . ?
O2 C5 N3 129.5(6) . . ?
O2 C5 C4 117.6(5) . . ?
N3 C5 C4 112.9(5) . . ?
C8 C6 N3 118.8(6) . . ?
C8 C6 C7 120.2(6) . . ?
C7 C6 N3 121.0(6) . . ?
C6 C8 H8 117(5) . . ?
C6 C8 C9 120.7(7) . . ?
C9 C8 H8 122(5) . . ?
C6 C7 H7 120.1 . . ?
C11 C7 C6 119.7(6) . . ?
C11 C7 H7 120.1 . . ?
N5 C13 C14 121.5(6) . . ?
N5 C13 C12 116.3(6) . . ?
C14 C13 C12 122.2(6) . . ?
N5 C16 H16 117.1 . . ?
N6 C16 N5 125.8(6) . . ?
N6 C16 H16 117.1 . . ?
N6 C15 H15 118.8 . . ?
N6 C15 C14 122.3(7) . . ?
C14 C15 H15 118.8 . . ?
C13 C14 C15 116.9(7) . . ?
C13 C14 H14 121.6 . . ?
C15 C14 H14 121.6 . . ?
O3 C12 N4 127.9(6) . . ?
O3 C12 C13 116.7(6) . . ?
N4 C12 C13 115.3(6) . . ?
C7 C11 N4 121.9(6) . . ?
C7 C11 C10 120.0(6) . . ?
C10 C11 N4 118.0(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 C11 120.0(6) . . ?
C9 C10 H10 120.0 . . ?
C8 C9 C10 119.4(7) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
H2WA O2W H2WB 103.6 . . ?
H3WA O3W H3WB 108.5 . . ?
H1WA O1W H1WB 110.5 . . ?
H4WA O4W H4WB 109.6 . . ?

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
Cu1 N1 C4 C3 -175.4(5) 7 . . . ?
Cu1 N1 C4 C5 1.9(7) 7 . . . ?
Cu1 N1 C1 N2 171.9(5) 7 . . . ?
Cu1 N3 C5 O2 -175.1(6) 7 . . . ?
Cu1 N3 C5 C4 7.4(7) 7 . . . ?
Cu1 N3 C6 C8 -78.6(7) 7 . . . ?
Cu1 N3 C6 C7 99.3(6) 7 . . . ?
Cu1 N5 C13 C14 175.7(5) . . . . ?
Cu1 N5 C13 C12 -2.6(7) . . . . ?
Cu1 N5 C16 N6 -171.1(6) . . . . ?
Cu1 N4 C12 O3 -173.1(5) . . . . ?
Cu1 N4 C12 C13 2.1(7) . . . . ?
Cu1 N4 C11 C7 -131.0(5) . . . . ?
Cu1 N4 C11 C10 44.7(7) . . . . ?
N1 C4 C3 C2 2.3(10) . . . . ?
N1 C4 C5 O2 176.1(6) . . . . ?
N1 C4 C5 N3 -6.1(8) . . . . ?
N2 C2 C3 C4 -0.9(11) . . . . ?
N3 C6 C8 C9 176.4(6) . . . . ?
N3 C6 C7 C11 -176.8(5) . . . . ?
N5 C13 C14 C15 -3.1(10) . . . . ?
N5 C13 C12 O3 176.4(6) . . . . ?
N5 C13 C12 N4 0.6(8) . . . . ?
N6 C15 C14 C13 1.2(12) . . . . ?
N4 C11 C10 C9 -176.2(6) . . . . ?
C4 N1 C1 N2 -1.1(11) . . . . ?
C1 N1 C4 C3 -1.4(10) . . . . ?
C1 N1 C4 C5 175.9(6) . . . . ?
C1 N2 C2 C3 -1.4(11) . . . . ?
C2 N2 C1 N1 2.5(11) . . . . ?
C3 C4 C5 O2 -6.7(10) . . . . ?
C3 C4 C5 N3 171.1(6) . . . . ?
C5 N3 C6 C8 97.2(7) . . . . ?
C5 N3 C6 C7 -85.0(7) . . . . ?
C5 C4 C3 C2 -174.7(6) . . . . ?
C6 N3 C5 O2 8.8(10) . . . . ?
C6 N3 C5 C4 -168.7(6) . . . . ?
C6 C8 C9 C10 1.0(11) . . . . ?
C6 C7 C11 N4 175.6(5) . . . . ?
C6 C7 C11 C10 -0.1(9) . . . . ?
C8 C6 C7 C11 1.0(9) . . . . ?
C7 C6 C8 C9 -1.4(10) . . . . ?
C7 C11 C10 C9 -0.3(9) . . . . ?
C13 N5 C16 N6 0.1(11) . . . . ?
C16 N5 C13 C14 2.5(9) . . . . ?
C16 N5 C13 C12 -175.7(6) . . . . ?
C16 N6 C15 C14 1.2(12) . . . . ?
C15 N6 C16 N5 -2.0(12) . . . . ?
C14 C13 C12 O3 -1.9(9) . . . . ?
C14 C13 C12 N4 -177.6(6) . . . . ?
C12 N4 C11 C7 52.1(8) . . . . ?
C12 N4 C11 C10 -132.2(6) . . . . ?
C12 C13 C14 C15 175.1(6) . . . . ?
C11 N4 C12 O3 3.8(10) . . . . ?
C11 N4 C12 C13 179.0(5) . . . . ?
C11 C10 C9 C8 -0.1(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dc170_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1551797'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_audit_creation_date             2017-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H30 N19 Ni2 O13 Tb, 4(O), C4 H8 O'
_chemical_formula_sum            'C52 H53 N19 Ni2 O17.50 Tb'
_chemical_formula_weight         1500.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.2817(6)
_cell_length_b                   24.8997(8)
_cell_length_c                   20.7090(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.977(5)
_cell_angle_gamma                90
_cell_volume                     6514.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15039
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.7047
_cell_measurement_theta_min      2.9421
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.82835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66009
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.800
_diffrn_reflns_theta_min         2.943
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10292
_reflns_number_total             20407
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.237
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         20407
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0643
_refine_ls_restrained_S_all      0.956
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1005P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1927
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C50-C49 = C51-C50 = C52-C51
 1.5 with sigma of 0.02
 O14-C49 = O14-C52
 1.35 with sigma of 0.02
 N14-C19 \\sim N14-C18A
 with sigma of 0.02
 C20-C19 \\sim C18A-C17 \\sim C18-C17
 with sigma of 0.02
 O3-C21 \\sim O3A-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20A)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(N14A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(O3A)=Sof(N3A)=Sof(N14A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(O16A)=1-FVAR(1)
 Sof(O3)=Sof(N3)=Sof(N14)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(C21)=Sof(O16)=FVAR(1)
 Sof(O19A)=1-FVAR(2)
 Sof(O19)=FVAR(2)
 Fixed Sof: O14(0.5) C49(0.5) H49a(0.5) H49b(0.5) C50(0.5) H50a(0.5) H50b(0.5)
 C51(0.5) H51a(0.5) H51b(0.5) C52(0.5) H52a(0.5) H52b(0.5) O18(0.5) O15(0.5)
 C53(0.5) H53a(0.5) H53b(0.5) C54(0.5) H54a(0.5) H54b(0.5) C55(0.5) H55a(0.5)
 H55b(0.5) C56(0.5) H56a(0.5) H56b(0.5) O20(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49a,H49b), C50(H50a,H50b), C51(H51a,H51b), C52(H52a,H52b), C53(H53a,
 H53b), C54(H54a,H54b), C55(H55a,H55b), C56(H56a,H56b)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C17A(H17A), C18(H18), C18A(H18A), C19(H19), C19A(H19A),
 C23(H23), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C43(H43), C46(H46),
 C47(H47), C48(H48)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.45565(2) 0.28633(2) 0.37627(2) 0.02390(9) Uani 1 1 d . . . . .
Ni1 Ni 0.68433(6) 0.10136(3) 0.68310(4) 0.02319(17) Uani 1 1 d . . . . .
Ni2 Ni 0.73200(6) 0.37580(3) 0.65260(4) 0.02247(17) Uani 1 1 d . . . . .
O1 O 1.0064(4) 0.1317(2) 0.7462(3) 0.0560(16) Uani 1 1 d . . . . .
O2 O 1.0408(4) 0.3208(2) 0.7287(3) 0.0487(14) Uani 1 1 d . . . . .
O3 O 0.5329(12) 0.1375(5) 0.4802(5) 0.041(3) Uani 0.558(19) 1 d D U P A 1
O3A O 0.4911(13) 0.1278(6) 0.4873(7) 0.041(4) Uani 0.442(19) 1 d D U P A 2
O4 O 0.5977(3) 0.30639(18) 0.4654(2) 0.0290(10) Uani 1 1 d . . . . .
O5 O 0.5289(4) 0.17392(18) 0.8052(2) 0.0321(10) Uani 1 1 d . . . . .
O6 O 0.5527(4) 0.35020(18) 0.7817(2) 0.0332(10) Uani 1 1 d . . . . .
O7 O 0.5882(4) 0.21641(18) 0.3901(2) 0.0355(11) Uani 1 1 d . . . . .
O8 O 0.3875(4) 0.21841(18) 0.4302(2) 0.0399(12) Uani 1 1 d . . . . .
O9 O 0.3991(4) 0.22730(18) 0.2788(2) 0.0357(11) Uani 1 1 d . . . . .
O10 O 0.2833(4) 0.3085(2) 0.3153(2) 0.0433(12) Uani 1 1 d . . . . .
O11 O 0.3787(4) 0.33649(18) 0.4547(2) 0.0355(11) Uani 1 1 d . . . . .
O12 O 0.4507(4) 0.38575(18) 0.3960(2) 0.0368(11) Uani 1 1 d . . . . .
O13 O 0.3925(5) 0.4227(2) 0.4730(3) 0.0614(17) Uani 1 1 d . . . . .
N1 N 0.7880(4) 0.05349(19) 0.7561(3) 0.0260(11) Uani 1 1 d . . . . .
N2 N 0.8297(4) 0.13433(19) 0.6855(2) 0.0252(11) Uani 1 1 d . . . . .
N3 N 0.6906(16) 0.0464(10) 0.6094(11) 0.033(5) Uani 0.558(19) 1 d . U P A 1
N3A N 0.6713(18) 0.0466(10) 0.5992(12) 0.017(4) Uani 0.442(19) 1 d . U P A 2
N4 N 0.5869(4) 0.14002(19) 0.5985(2) 0.0255(11) Uani 1 1 d . . . . .
N5 N 0.5490(4) 0.06599(19) 0.6994(2) 0.0262(11) Uani 1 1 d . . . . .
N6 N 0.6547(4) 0.15256(19) 0.7557(2) 0.0241(11) Uani 1 1 d . . . . .
N7 N 0.8495(4) 0.4222(2) 0.7184(3) 0.0277(11) Uani 1 1 d . . . . .
N8 N 0.8650(4) 0.32731(19) 0.6652(3) 0.0256(11) Uani 1 1 d . . . . .
N9 N 0.7557(4) 0.4089(2) 0.5642(3) 0.0283(11) Uani 1 1 d . . . . .
N10 N 0.6261(4) 0.33097(18) 0.5759(2) 0.0214(10) Uani 1 1 d . . . . .
N11 N 0.6082(4) 0.42777(19) 0.6523(2) 0.0241(10) Uani 1 1 d . . . . .
N12 N 0.6860(4) 0.34486(18) 0.7323(2) 0.0212(10) Uani 1 1 d . . . . .
N13 N 0.9445(6) -0.0003(3) 0.8538(3) 0.0559(19) Uani 1 1 d . . . . .
N14 N 0.6847(13) -0.0094(5) 0.4894(6) 0.048(4) Uani 0.558(19) 1 d D U P A 1
N14A N 0.6290(19) -0.0228(8) 0.4935(10) 0.065(6) Uani 0.442(19) 1 d . U P A 2
N15 N 0.3587(5) 0.0379(2) 0.7191(3) 0.0379(14) Uani 1 1 d . . . . .
N16 N 1.0202(5) 0.4700(3) 0.8129(4) 0.0504(17) Uani 1 1 d . . . . .
N17 N 0.7904(5) 0.4294(3) 0.4408(3) 0.0452(16) Uani 1 1 d . . . . .
N18 N 0.4142(5) 0.4739(2) 0.6486(3) 0.0402(14) Uani 1 1 d . . . . .
N19 N 0.4062(5) 0.3827(2) 0.4426(3) 0.0370(14) Uani 1 1 d . . . . .
C1 C 0.7680(6) 0.0107(3) 0.7881(3) 0.0357(16) Uani 1 1 d . . . . .
H1 H 0.6988 -0.0019 0.7771 0.043 Uiso 1 1 calc R . . . .
C2 C 0.8447(7) -0.0151(3) 0.8361(4) 0.0466(19) Uani 1 1 d . . . . .
H2 H 0.8263 -0.0445 0.8577 0.056 Uiso 1 1 calc R . . . .
C3 C 0.9655(6) 0.0438(3) 0.8226(4) 0.0467(19) Uani 1 1 d . . . . .
H3 H 1.0342 0.0573 0.8355 0.056 Uiso 1 1 calc R . . . .
C4 C 0.8888(5) 0.0692(2) 0.7725(3) 0.0310(14) Uani 1 1 d . . . . .
C5 C 0.9119(6) 0.1155(3) 0.7322(3) 0.0341(15) Uani 1 1 d . . . . .
C6 C 0.8442(5) 0.1784(2) 0.6467(3) 0.0257(13) Uani 1 1 d . . . . .
C7 C 0.8387(5) 0.1725(3) 0.5790(3) 0.0303(14) Uani 1 1 d . . . . .
H7 H 0.8296 0.1386 0.5592 0.036 Uiso 1 1 calc R . . . .
C8 C 0.8466(6) 0.2162(3) 0.5414(3) 0.0338(15) Uani 1 1 d . . . . .
H8 H 0.8442 0.2117 0.4964 0.041 Uiso 1 1 calc R . . . .
C9 C 0.8582(5) 0.2679(3) 0.5697(3) 0.0304(14) Uani 1 1 d . . . . .
H9 H 0.8621 0.2976 0.5434 0.037 Uiso 1 1 calc R . . . .
C10 C 0.8640(5) 0.2744(2) 0.6377(3) 0.0270(13) Uani 1 1 d . . . . .
C11 C 0.8595(5) 0.2303(2) 0.6759(3) 0.0250(13) Uani 1 1 d . . . . .
H11 H 0.8665 0.2345 0.7217 0.030 Uiso 1 1 calc R . . . .
C12 C 0.9536(5) 0.3436(3) 0.7096(3) 0.0324(15) Uani 1 1 d . . . . .
C13 C 0.9446(5) 0.3979(3) 0.7389(3) 0.0302(14) Uani 1 1 d . . . . .
C14 C 1.0279(6) 0.4228(3) 0.7866(4) 0.0453(19) Uani 1 1 d . . . . .
H14 H 1.0927 0.4052 0.8008 0.054 Uiso 1 1 calc R . . . .
C15 C 0.9277(6) 0.4934(3) 0.7923(4) 0.0447(18) Uani 1 1 d . . . . .
H15 H 0.9196 0.5269 0.8102 0.054 Uiso 1 1 calc R . . . .
C16 C 0.8404(6) 0.4700(3) 0.7444(3) 0.0343(15) Uani 1 1 d . . . . .
H16 H 0.7759 0.4880 0.7308 0.041 Uiso 1 1 calc R . . . .
C17 C 0.7411(19) 0.0003(11) 0.6089(12) 0.043(7) Uani 0.558(19) 1 d D U P A 1
H17 H 0.7813 -0.0142 0.6502 0.052 Uiso 0.558(19) 1 calc R . P A 1
C17A C 0.720(2) -0.0016(10) 0.6085(12) 0.021(5) Uani 0.442(19) 1 d . U P A 2
H17A H 0.7640 -0.0120 0.6509 0.025 Uiso 0.442(19) 1 calc R . P A 2
C18 C 0.7367(16) -0.0274(8) 0.5491(7) 0.052(5) Uani 0.558(19) 1 d D U P A 1
H18 H 0.7725 -0.0599 0.5524 0.062 Uiso 0.558(19) 1 calc R . P A 1
C18A C 0.7006(17) -0.0350(7) 0.5522(7) 0.038(5) Uani 0.442(19) 1 d D U P A 2
H18A H 0.7390 -0.0667 0.5558 0.046 Uiso 0.442(19) 1 calc R . P A 2
C19 C 0.6334(13) 0.0388(5) 0.4853(7) 0.036(3) Uani 0.558(19) 1 d D U P A 1
H19 H 0.5946 0.0527 0.4433 0.043 Uiso 0.558(19) 1 calc R . P A 1
C19A C 0.5850(19) 0.0281(8) 0.4905(10) 0.049(5) Uani 0.442(19) 1 d . U P A 2
H19A H 0.5368 0.0392 0.4498 0.058 Uiso 0.442(19) 1 calc R . P A 2
C20 C 0.6402(15) 0.0667(7) 0.5448(9) 0.034(4) Uani 0.558(19) 1 d D U P A 1
C20A C 0.6081(15) 0.0613(8) 0.5426(10) 0.022(4) Uani 0.442(19) 1 d . U P A 2
C21 C 0.5823(15) 0.1178(8) 0.5402(10) 0.031(4) Uani 0.558(19) 1 d D U P A 1
C21A C 0.5526(17) 0.1153(9) 0.5397(11) 0.022(4) Uani 0.442(19) 1 d . U P A 2
C22 C 0.5437(5) 0.1923(2) 0.5982(3) 0.0260(13) Uani 1 1 d . . . . .
C23 C 0.5990(5) 0.2358(2) 0.5835(3) 0.0241(12) Uani 1 1 d . . . . .
H23 H 0.6602 0.2299 0.5717 0.029 Uiso 1 1 calc R . . . .
C24 C 0.5635(4) 0.2876(2) 0.5864(3) 0.0202(11) Uani 1 1 d . . . . .
C25 C 0.4706(5) 0.2967(2) 0.6017(3) 0.0252(13) Uani 1 1 d . . . . .
H25 H 0.4458 0.3315 0.6029 0.030 Uiso 1 1 calc R . . . .
C26 C 0.4148(5) 0.2534(2) 0.6153(3) 0.0251(12) Uani 1 1 d . . . . .
H26 H 0.3524 0.2594 0.6257 0.030 Uiso 1 1 calc R . . . .
C27 C 0.4507(5) 0.2008(2) 0.6136(3) 0.0283(14) Uani 1 1 d . . . . .
H27 H 0.4127 0.1720 0.6228 0.034 Uiso 1 1 calc R . . . .
C28 C 0.6368(5) 0.3354(2) 0.5162(3) 0.0243(12) Uani 1 1 d . . . . .
C29 C 0.7086(5) 0.3803(2) 0.5091(3) 0.0266(13) Uani 1 1 d . . . . .
C30 C 0.7248(6) 0.3903(3) 0.4476(3) 0.0356(16) Uani 1 1 d . . . . .
H30 H 0.6896 0.3696 0.4101 0.043 Uiso 1 1 calc R . . . .
C31 C 0.8378(7) 0.4572(3) 0.4958(4) 0.051(2) Uani 1 1 d . . . . .
H31 H 0.8848 0.4841 0.4930 0.061 Uiso 1 1 calc R . . . .
C32 C 0.8207(6) 0.4481(3) 0.5578(4) 0.0430(18) Uani 1 1 d . . . . .
H32 H 0.8546 0.4694 0.5950 0.052 Uiso 1 1 calc R . . . .
C33 C 0.4970(6) 0.0221(2) 0.6722(3) 0.0343(15) Uani 1 1 d . . . . .
H33 H 0.5249 0.0000 0.6458 0.041 Uiso 1 1 calc R . . . .
C34 C 0.4024(6) 0.0084(3) 0.6823(3) 0.0363(16) Uani 1 1 d . . . . .
H34 H 0.3683 -0.0228 0.6624 0.044 Uiso 1 1 calc R . . . .
C35 C 0.4115(5) 0.0822(3) 0.7464(3) 0.0333(15) Uani 1 1 d . . . . .
H35 H 0.3831 0.1045 0.7724 0.040 Uiso 1 1 calc R . . . .
C36 C 0.5056(5) 0.0959(2) 0.7373(3) 0.0223(12) Uani 1 1 d . . . . .
C37 C 0.5679(5) 0.1456(2) 0.7690(3) 0.0229(12) Uani 1 1 d . . . . .
C38 C 0.7103(5) 0.2013(2) 0.7806(3) 0.0234(12) Uani 1 1 d . . . . .
C39 C 0.8074(5) 0.2004(2) 0.8323(3) 0.0256(13) Uani 1 1 d . . . . .
H39 H 0.8358 0.1683 0.8530 0.031 Uiso 1 1 calc R . . . .
C40 C 0.8607(5) 0.2491(3) 0.8521(3) 0.0289(14) Uani 1 1 d . . . . .
H40 H 0.9246 0.2490 0.8870 0.035 Uiso 1 1 calc R . . . .
C41 C 0.8217(5) 0.2971(2) 0.8217(3) 0.0254(13) Uani 1 1 d . . . . .
H41 H 0.8587 0.3289 0.8357 0.030 Uiso 1 1 calc R . . . .
C42 C 0.7259(5) 0.2972(2) 0.7695(3) 0.0219(12) Uani 1 1 d . . . . .
C43 C 0.6698(5) 0.2495(2) 0.7511(3) 0.0204(11) Uani 1 1 d . . . . .
H43 H 0.6037 0.2501 0.7183 0.025 Uiso 1 1 calc R . . . .
C44 C 0.6007(5) 0.3648(2) 0.7399(3) 0.0236(12) Uani 1 1 d . . . . .
C45 C 0.5529(5) 0.4109(2) 0.6930(3) 0.0229(12) Uani 1 1 d . . . . .
C46 C 0.4575(5) 0.4326(3) 0.6899(3) 0.0320(14) Uani 1 1 d . . . . .
H46 H 0.4206 0.4184 0.7174 0.038 Uiso 1 1 calc R . . . .
C47 C 0.4720(6) 0.4919(3) 0.6096(3) 0.0347(15) Uani 1 1 d . . . . .
H47 H 0.4463 0.5205 0.5803 0.042 Uiso 1 1 calc R . . . .
C48 C 0.5690(5) 0.4691(2) 0.6117(3) 0.0294(14) Uani 1 1 d . . . . .
H48 H 0.6066 0.4830 0.5843 0.035 Uiso 1 1 calc R . . . .
O19A O 0.0935(15) 0.2642(8) 0.2983(10) 0.062(6) Uiso 0.319(12) 1 d . . P B 2
O19 O 0.1177(6) 0.2835(3) 0.2067(4) 0.047(2) Uiso 0.681(12) 1 d . . P B 1
O14 O 0.1657(15) 0.3540(7) 0.5676(9) 0.116(6) Uiso 0.5 1 d D . P . .
C49 C 0.0638(18) 0.3616(13) 0.5489(13) 0.123(10) Uiso 0.5 1 d D . P . .
H49A H 0.0435 0.3980 0.5562 0.148 Uiso 0.5 1 calc R . P . .
H49B H 0.0262 0.3356 0.5677 0.148 Uiso 0.5 1 calc R . P . .
C50 C 0.058(2) 0.3502(11) 0.4767(14) 0.139(11) Uiso 0.5 1 d D . P . .
H50A H -0.0139 0.3541 0.4467 0.167 Uiso 0.5 1 calc R . P . .
H50B H 0.0825 0.3141 0.4721 0.167 Uiso 0.5 1 calc R . P . .
C51 C 0.1305(11) 0.3919(6) 0.4607(7) 0.044(4) Uiso 0.5 1 d D . P . .
H51A H 0.1619 0.3806 0.4264 0.053 Uiso 0.5 1 calc R . P . .
H51B H 0.0989 0.4273 0.4506 0.053 Uiso 0.5 1 calc R . P . .
C52 C 0.1983(13) 0.3862(7) 0.5281(8) 0.059(5) Uiso 0.5 1 d D . P . .
H52A H 0.2663 0.3733 0.5263 0.071 Uiso 0.5 1 calc R . P . .
H52B H 0.2097 0.4215 0.5490 0.071 Uiso 0.5 1 calc R . P . .
O18 O 0.1772(8) 0.1878(4) 0.3851(5) 0.042(2) Uiso 0.5 1 d . . P . .
O15 O 0.0814(12) 0.1482(6) 0.4777(8) 0.089(4) Uiso 0.5 1 d . . P . .
C53 C 0.1402(19) 0.1702(9) 0.5480(11) 0.083(6) Uiso 0.5 1 d . . P . .
H53A H 0.2064 0.1871 0.5488 0.100 Uiso 0.5 1 calc R . P . .
H53B H 0.0972 0.1957 0.5633 0.100 Uiso 0.5 1 calc R . P . .
C54 C 0.1587(19) 0.1197(9) 0.5899(12) 0.091(7) Uiso 0.5 1 d . . P . .
H54A H 0.2280 0.1049 0.5940 0.109 Uiso 0.5 1 calc R . P . .
H54B H 0.1548 0.1271 0.6350 0.109 Uiso 0.5 1 calc R . P . .
C55 C 0.076(2) 0.0816(11) 0.5545(13) 0.104(8) Uiso 0.5 1 d . . P . .
H55A H 0.0244 0.0777 0.5790 0.125 Uiso 0.5 1 calc R . P . .
H55B H 0.1061 0.0467 0.5516 0.125 Uiso 0.5 1 calc R . P . .
C56 C 0.0174(15) 0.1057(7) 0.4777(9) 0.060(5) Uiso 0.5 1 d . . P . .
H56A H 0.0177 0.0798 0.4428 0.072 Uiso 0.5 1 calc R . P . .
H56B H -0.0547 0.1169 0.4722 0.072 Uiso 0.5 1 calc R . P . .
O20 O 0.1939(9) 0.4005(5) 0.3379(6) 0.058(3) Uiso 0.5 1 d . . P . .
O16 O 0.4157(8) 0.0974(3) 0.3481(4) 0.025(2) Uiso 0.558(19) 1 d . . P A 1
O16A O 0.4604(18) 0.0953(7) 0.3612(9) 0.068(5) Uiso 0.442(19) 1 d . . P A 2
O17 O 0.2483(6) 0.1487(3) 0.2429(4) 0.080(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.251(4) . ?
Tb1 O5 2.231(4) 4_565 ?
Tb1 O7 2.429(4) . ?
Tb1 O8 2.357(4) . ?
Tb1 O9 2.422(4) . ?
Tb1 O10 2.314(5) . ?
Tb1 O11 2.503(4) . ?
Tb1 O12 2.513(4) . ?
Tb1 N19 2.938(6) . ?
Ni1 N1 2.078(5) . ?
Ni1 N2 2.084(5) . ?
Ni1 N3 2.07(2) . ?
Ni1 N3A 2.17(2) . ?
Ni1 N4 2.066(5) . ?
Ni1 N5 2.120(5) . ?
Ni1 N6 2.100(5) . ?
Ni2 N7 2.077(5) . ?
Ni2 N8 2.088(5) . ?
Ni2 N9 2.118(5) . ?
Ni2 N10 2.090(5) . ?
Ni2 N11 2.091(5) . ?
Ni2 N12 2.077(4) . ?
O1 C5 1.263(8) . ?
O2 C12 1.240(8) . ?
O3 C21 1.31(2) . ?
O3A C21A 1.18(2) . ?
O4 C28 1.249(7) . ?
O5 Tb1 2.231(4) 4_566 ?
O5 C37 1.252(7) . ?
O6 C44 1.275(7) . ?
O11 N19 1.255(7) . ?
O12 N19 1.280(7) . ?
O13 N19 1.220(7) . ?
N1 C1 1.324(8) . ?
N1 C4 1.334(8) . ?
N2 C5 1.303(8) . ?
N2 C6 1.408(7) . ?
N3 C17 1.33(3) . ?
N3 C20 1.39(3) . ?
N3A C17A 1.35(3) . ?
N3A C20A 1.27(3) . ?
N4 C21 1.31(2) . ?
N4 C21A 1.31(2) . ?
N4 C22 1.421(7) . ?
N5 C33 1.322(8) . ?
N5 C36 1.336(7) . ?
N6 C37 1.275(7) . ?
N6 C38 1.432(7) . ?
N7 C13 1.344(8) . ?
N7 C16 1.329(8) . ?
N8 C10 1.434(7) . ?
N8 C12 1.314(8) . ?
N9 C29 1.327(8) . ?
N9 C32 1.336(8) . ?
N10 C24 1.420(7) . ?
N10 C28 1.292(7) . ?
N11 C45 1.344(7) . ?
N11 C48 1.329(7) . ?
N12 C42 1.424(7) . ?
N12 C44 1.291(7) . ?
N13 C2 1.314(10) . ?
N13 C3 1.347(10) . ?
N14 C18 1.30(2) . ?
N14 C19 1.369(14) . ?
N14A C18A 1.33(2) . ?
N14A C19A 1.39(3) . ?
N15 C34 1.313(9) . ?
N15 C35 1.336(8) . ?
N16 C14 1.312(9) . ?
N16 C15 1.307(10) . ?
N17 C30 1.343(9) . ?
N17 C31 1.314(10) . ?
N18 C46 1.347(8) . ?
N18 C47 1.350(9) . ?
C1 C2 1.348(10) . ?
C3 C4 1.365(9) . ?
C4 C5 1.509(9) . ?
C6 C7 1.390(8) . ?
C6 C11 1.416(8) . ?
C7 C8 1.358(9) . ?
C8 C9 1.403(9) . ?
C9 C10 1.397(8) . ?
C10 C11 1.364(8) . ?
C12 C13 1.501(9) . ?
C13 C14 1.382(10) . ?
C15 C16 1.399(10) . ?
C17 C18 1.40(2) . ?
C17A C18A 1.39(3) . ?
C19 C20 1.394(19) . ?
C19A C20A 1.32(3) . ?
C20 C21 1.47(3) . ?
C20A C21A 1.53(3) . ?
C22 C23 1.395(8) . ?
C22 C27 1.384(9) . ?
C23 C24 1.380(8) . ?
C24 C25 1.385(8) . ?
C25 C26 1.385(8) . ?
C26 C27 1.397(8) . ?
C28 C29 1.506(8) . ?
C29 C30 1.378(8) . ?
C31 C32 1.391(10) . ?
C33 C34 1.379(9) . ?
C35 C36 1.364(9) . ?
C36 C37 1.521(8) . ?
C38 C39 1.400(9) . ?
C38 C43 1.376(8) . ?
C39 C40 1.400(9) . ?
C40 C41 1.375(8) . ?
C41 C42 1.393(9) . ?
C42 C43 1.393(8) . ?
C44 C45 1.510(8) . ?
C45 C46 1.361(9) . ?
C47 C48 1.396(9) . ?
O14 C49 1.302(17) . ?
O14 C52 1.309(15) . ?
C49 C50 1.500(18) . ?
C50 C51 1.520(17) . ?
C51 C52 1.416(15) . ?
O15 C53 1.52(2) . ?
O15 C56 1.36(2) . ?
C53 C54 1.50(3) . ?
C54 C55 1.47(3) . ?
C55 C56 1.65(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O7 70.64(16) . . ?
O4 Tb1 O8 96.78(17) . . ?
O4 Tb1 O9 141.63(16) . . ?
O4 Tb1 O10 146.30(17) . . ?
O4 Tb1 O11 76.36(16) . . ?
O4 Tb1 O12 72.87(16) . . ?
O4 Tb1 N19 71.76(16) . . ?
O5 Tb1 O4 90.95(16) 4_565 . ?
O5 Tb1 O7 87.04(16) 4_565 . ?
O5 Tb1 O8 160.22(16) 4_565 . ?
O5 Tb1 O9 78.78(16) 4_565 . ?
O5 Tb1 O10 95.35(17) 4_565 . ?
O5 Tb1 O11 123.72(16) 4_565 . ?
O5 Tb1 O12 73.08(15) 4_565 . ?
O5 Tb1 N19 98.76(16) 4_565 . ?
O7 Tb1 O11 134.99(15) . . ?
O7 Tb1 O12 137.83(16) . . ?
O7 Tb1 N19 142.03(16) . . ?
O8 Tb1 O7 78.48(16) . . ?
O8 Tb1 O9 83.92(16) . . ?
O8 Tb1 O11 75.92(16) . . ?
O8 Tb1 O12 126.61(15) . . ?
O8 Tb1 N19 100.96(17) . . ?
O9 Tb1 O7 71.97(16) . . ?
O9 Tb1 O11 139.47(16) . . ?
O9 Tb1 O12 135.77(15) . . ?
O9 Tb1 N19 146.00(16) . . ?
O10 Tb1 O7 142.61(17) . . ?
O10 Tb1 O8 88.28(19) . . ?
O10 Tb1 O9 71.96(17) . . ?
O10 Tb1 O11 72.64(16) . . ?
O10 Tb1 O12 77.42(17) . . ?
O10 Tb1 N19 74.57(17) . . ?
O11 Tb1 O12 50.69(14) . . ?
O11 Tb1 N19 25.07(15) . . ?
O12 Tb1 N19 25.67(15) . . ?
N1 Ni1 N2 78.9(2) . . ?
N1 Ni1 N3A 95.3(6) . . ?
N1 Ni1 N5 92.9(2) . . ?
N1 Ni1 N6 93.21(19) . . ?
N2 Ni1 N3A 96.4(6) . . ?
N2 Ni1 N5 169.9(2) . . ?
N2 Ni1 N6 96.96(19) . . ?
N3 Ni1 N1 89.3(6) . . ?
N3 Ni1 N2 91.7(6) . . ?
N3 Ni1 N5 94.1(6) . . ?
N3 Ni1 N6 171.3(6) . . ?
N4 Ni1 N1 170.04(19) . . ?
N4 Ni1 N2 99.8(2) . . ?
N4 Ni1 N3 80.8(6) . . ?
N4 Ni1 N3A 74.9(6) . . ?
N4 Ni1 N5 89.3(2) . . ?
N4 Ni1 N6 96.75(18) . . ?
N5 Ni1 N3A 90.2(7) . . ?
N6 Ni1 N3A 165.3(6) . . ?
N6 Ni1 N5 77.44(19) . . ?
N7 Ni2 N8 78.7(2) . . ?
N7 Ni2 N9 93.9(2) . . ?
N7 Ni2 N10 171.37(19) . . ?
N7 Ni2 N11 95.1(2) . . ?
N7 Ni2 N12 91.79(19) . . ?
N8 Ni2 N9 89.3(2) . . ?
N8 Ni2 N10 97.53(19) . . ?
N8 Ni2 N11 172.8(2) . . ?
N10 Ni2 N9 78.21(19) . . ?
N10 Ni2 N11 89.09(19) . . ?
N11 Ni2 N9 94.7(2) . . ?
N12 Ni2 N8 97.53(19) . . ?
N12 Ni2 N9 171.9(2) . . ?
N12 Ni2 N10 96.42(19) . . ?
N12 Ni2 N11 78.93(19) . . ?
C28 O4 Tb1 147.5(4) . . ?
C37 O5 Tb1 172.1(4) . 4_566 ?
N19 O11 Tb1 97.2(3) . . ?
N19 O12 Tb1 96.0(3) . . ?
C1 N1 Ni1 129.4(5) . . ?
C1 N1 C4 116.7(6) . . ?
C4 N1 Ni1 113.9(4) . . ?
C5 N2 Ni1 115.7(4) . . ?
C5 N2 C6 118.2(5) . . ?
C6 N2 Ni1 125.6(4) . . ?
C17 N3 Ni1 135.3(17) . . ?
C17 N3 C20 114(2) . . ?
C20 N3 Ni1 110.6(15) . . ?
C17A N3A Ni1 121.8(17) . . ?
C20A N3A Ni1 115.1(17) . . ?
C20A N3A C17A 123(2) . . ?
C21 N4 Ni1 115.0(9) . . ?
C21 N4 C22 118.5(10) . . ?
C21A N4 Ni1 121.0(10) . . ?
C21A N4 C22 113.6(10) . . ?
C22 N4 Ni1 125.2(4) . . ?
C33 N5 Ni1 129.2(4) . . ?
C33 N5 C36 116.7(5) . . ?
C36 N5 Ni1 113.7(4) . . ?
C37 N6 Ni1 117.0(4) . . ?
C37 N6 C38 116.0(5) . . ?
C38 N6 Ni1 125.6(4) . . ?
C13 N7 Ni2 113.6(4) . . ?
C16 N7 Ni2 128.4(5) . . ?
C16 N7 C13 118.0(6) . . ?
C10 N8 Ni2 125.3(4) . . ?
C12 N8 Ni2 116.7(4) . . ?
C12 N8 C10 117.3(5) . . ?
C29 N9 Ni2 112.2(4) . . ?
C29 N9 C32 117.0(6) . . ?
C32 N9 Ni2 130.0(5) . . ?
C24 N10 Ni2 125.3(4) . . ?
C28 N10 Ni2 115.8(4) . . ?
C28 N10 C24 116.9(5) . . ?
C45 N11 Ni2 112.6(4) . . ?
C48 N11 Ni2 129.4(4) . . ?
C48 N11 C45 117.2(5) . . ?
C42 N12 Ni2 125.9(4) . . ?
C44 N12 Ni2 116.0(4) . . ?
C44 N12 C42 116.7(5) . . ?
C2 N13 C3 115.8(7) . . ?
C18 N14 C19 118.1(12) . . ?
C18A N14A C19A 115.0(18) . . ?
C34 N15 C35 116.0(6) . . ?
C15 N16 C14 116.8(7) . . ?
C31 N17 C30 116.3(6) . . ?
C46 N18 C47 114.9(6) . . ?
O11 N19 Tb1 57.7(3) . . ?
O11 N19 O12 115.8(5) . . ?
O12 N19 Tb1 58.3(3) . . ?
O13 N19 Tb1 175.7(5) . . ?
O13 N19 O11 123.1(6) . . ?
O13 N19 O12 121.1(6) . . ?
N1 C1 C2 122.0(7) . . ?
N13 C2 C1 122.8(7) . . ?
N13 C3 C4 121.7(7) . . ?
N1 C4 C3 120.9(6) . . ?
N1 C4 C5 116.3(6) . . ?
C3 C4 C5 122.8(7) . . ?
O1 C5 N2 127.0(6) . . ?
O1 C5 C4 118.3(6) . . ?
N2 C5 C4 114.7(6) . . ?
N2 C6 C11 119.7(5) . . ?
C7 C6 N2 121.4(5) . . ?
C7 C6 C11 118.9(6) . . ?
C8 C7 C6 120.3(6) . . ?
C7 C8 C9 120.9(6) . . ?
C10 C9 C8 119.5(6) . . ?
C9 C10 N8 119.9(6) . . ?
C11 C10 N8 120.4(5) . . ?
C11 C10 C9 119.5(6) . . ?
C10 C11 C6 120.9(6) . . ?
O2 C12 N8 128.9(6) . . ?
O2 C12 C13 117.8(6) . . ?
N8 C12 C13 113.3(6) . . ?
N7 C13 C12 117.5(6) . . ?
N7 C13 C14 119.4(6) . . ?
C14 C13 C12 123.1(6) . . ?
N16 C14 C13 123.4(7) . . ?
N16 C15 C16 122.3(7) . . ?
N7 C16 C15 120.1(7) . . ?
N3 C17 C18 123(2) . . ?
N3A C17A C18A 117(2) . . ?
N14 C18 C17 122.4(19) . . ?
N14A C18A C17A 122(2) . . ?
N14 C19 C20 119.2(13) . . ?
C20A C19A N14A 123.2(19) . . ?
N3 C20 C19 123.3(17) . . ?
N3 C20 C21 117.5(17) . . ?
C19 C20 C21 118.9(15) . . ?
N3A C20A C19A 120(2) . . ?
N3A C20A C21A 117.7(19) . . ?
C19A C20A C21A 122.3(18) . . ?
O3 C21 N4 125.7(16) . . ?
O3 C21 C20 118.9(17) . . ?
N4 C21 C20 115.4(15) . . ?
O3A C21A N4 132(2) . . ?
O3A C21A C20A 117.1(19) . . ?
N4 C21A C20A 110.6(16) . . ?
C23 C22 N4 118.2(5) . . ?
C27 C22 N4 121.9(6) . . ?
C27 C22 C23 119.8(6) . . ?
C24 C23 C22 120.5(6) . . ?
C23 C24 N10 118.7(5) . . ?
C23 C24 C25 120.2(5) . . ?
C25 C24 N10 121.1(5) . . ?
C26 C25 C24 119.3(6) . . ?
C25 C26 C27 121.0(6) . . ?
C22 C27 C26 119.1(6) . . ?
O4 C28 N10 128.1(6) . . ?
O4 C28 C29 117.2(5) . . ?
N10 C28 C29 114.6(5) . . ?
N9 C29 C28 117.4(5) . . ?
N9 C29 C30 122.1(6) . . ?
C30 C29 C28 120.6(6) . . ?
N17 C30 C29 121.3(6) . . ?
N17 C31 C32 122.9(7) . . ?
N9 C32 C31 120.4(7) . . ?
N5 C33 C34 121.3(6) . . ?
N15 C34 C33 122.5(6) . . ?
N15 C35 C36 122.1(6) . . ?
N5 C36 C35 121.4(6) . . ?
N5 C36 C37 115.6(5) . . ?
C35 C36 C37 123.0(5) . . ?
O5 C37 N6 128.4(6) . . ?
O5 C37 C36 116.4(5) . . ?
N6 C37 C36 115.1(5) . . ?
C39 C38 N6 120.8(5) . . ?
C43 C38 N6 119.4(5) . . ?
C43 C38 C39 119.7(5) . . ?
C38 C39 C40 118.2(6) . . ?
C41 C40 C39 122.3(6) . . ?
C40 C41 C42 118.8(6) . . ?
C41 C42 N12 121.4(5) . . ?
C41 C42 C43 119.6(5) . . ?
C43 C42 N12 119.0(5) . . ?
C38 C43 C42 121.3(5) . . ?
O6 C44 N12 127.8(5) . . ?
O6 C44 C45 117.1(5) . . ?
N12 C44 C45 115.1(5) . . ?
N11 C45 C44 116.1(5) . . ?
N11 C45 C46 121.7(6) . . ?
C46 C45 C44 122.2(5) . . ?
N18 C46 C45 122.9(6) . . ?
N18 C47 C48 122.5(6) . . ?
N11 C48 C47 120.7(6) . . ?
C49 O14 C52 104(2) . . ?
O14 C49 C50 90(2) . . ?
C49 C50 C51 104(2) . . ?
C52 C51 C50 88.3(15) . . ?
O14 C52 C51 116.4(16) . . ?
C56 O15 C53 114.5(16) . . ?
C54 C53 O15 101.2(17) . . ?
C55 C54 C53 107(2) . . ?
C54 C55 C56 108(2) . . ?
O15 C56 C55 100.2(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
