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

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

data_fuls_a
_database_code_depnum_ccdc_archive 'CCDC 1443379'
_audit_update_record             
;
2016-05-09 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_fuls_a              
;
PROBLEM: Short Inter D-H..H-D       H00F   ..  H011    ..       1.48 Ang.
RESPONSE: The structure features hydrogen bonding networks which includes water/solvents and anions (nitrates)
;
_vrf_PLAT355_fuls_a              
;
PROBLEM: Long    O-H (X0.82,N0.98A)  O888   -   H88A   ..       1.10 Ang.
RESPONSE: The structure features hydrogen bonding networks which includes water/solvents and anions (nitrates)
;
# Added during the CSD deposition process: Monday 09 May 2016 10:05 PM
# end Validation Reply Form

_audit_creation_date             2016-02-09
_audit_creation_method           
;
Olex2 1.2
(compiled Sep 16 2015 11:44:03 for OlexSys, GUI svn.r5103)
;
_chemical_formula_moiety         'C15 H30 Cu3 N9 O6, 3(N O3), H2 O'
_chemical_formula_sum            'C15 H32 Cu3 N12 O16'
_chemical_formula_weight         827.13
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cu 0.34125 1.28947 13.33800 7.16760 5.61580 1.67350 3.58280 0.24700 11.39660
64.81260 1.19099998474
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

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

_symmetry_Int_Tables_number      2
_cell_length_a                   12.6421(9)
_cell_length_b                   14.2612(10)
_cell_length_c                   17.0125(11)
_cell_angle_alpha                90.192(3)
_cell_angle_beta                 96.380(3)
_cell_angle_gamma                113.941(3)
_cell_volume                     2782.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      1.56
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0625 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.7825.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.9747
_exptl_crystal_description       block
_exptl_crystal_F_000             1688.9139
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50230
_diffrn_reflns_theta_full        30.5000
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.56
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9937
_diffrn_measured_fraction_theta_max 0.9937
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                11639
_reflns_number_total             13844
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.1713
_refine_diff_density_min         -0.9269
_refine_diff_density_rms         0.1084
_refine_ls_d_res_high            0.7478
_refine_ls_d_res_low             13.0157
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0620
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    83
_refine_ls_number_parameters     903
_refine_ls_number_reflns         13844
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.0617
_refine_ls_shift/su_max          3.5255
_refine_ls_shift/su_mean         0.0292
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+2.1466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0710
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O888-H88b
 0.95 with sigma of 0.02
 O010-H88b
 2 with sigma of 0.02
 O888-H88a
 1 with sigma of 0.02
 O00Q-H88a
 2.06 with sigma of 0.02
 O00M-H00k
 0.992 with sigma of 0.02
 O224-H00k
 1.75 with sigma of 0.02
 C02M-H02u
 0.99 with sigma of 0.02
 C02L-H02s
 0.99 with sigma of 0.02
3. Others
 Sof(H02i)=Sof(H02j)=Sof(H02q)=Sof(H02r)=Sof(C02M)=Sof(H02u)=Sof(H02v)=1-FVAR(1)
 Sof(H02g)=Sof(H02h)=Sof(H02o)=Sof(H02p)=Sof(C02L)=Sof(H02s)=Sof(H02t)=FVAR(1)
4.a Rotating group:
 O00D(H00e,H00f), O00E(H00a,H00b), O00G(H00g,H00h), O00H(H00i,H00j), O00I(H00c,
 H00d), O999(H99a,H99b)
4.b Rotating group with stretchable bonds:
 C02M(H00k,H00l)
4.c Secondary CH2 refined with riding coordinates:
 C01X(H01a,H01b), C021(H02w,H02x), C024(H02y,H), C026(H02z,Ha), C027(H02a,
 H02b), C028(H02,Hb), C029(H02c,H02d), C02A(H02e,H02f), C02B(H0aa,Hc),
 C02C(H1aa,Hd), C02D(H2aa,He), C02E(H3aa,Hf), C02F(H02g,H02h), C02F(H02i,H02j),
 C02G(H02k,H02l), C02H(H02m,H02n), C02I(H02o,H02p), C02I(H02q,H02r), C02J(H4aa,
 Hg), C02L(H02s,H02t), C02M(H02u,H02v)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
_atom_site_disorder_group
Cu01 Cu 0.28107(2) -0.257119(18) 0.718311(13) 0.00851(6) Uani 1.000000 . .
Cu02 Cu 0.52686(2) -0.096127(18) 0.868476(13) 0.00868(6) Uani 1.000000 . .
Cu03 Cu 0.46411(2) 0.588822(18) 0.622463(13) 0.00845(6) Uani 1.000000 . .
Cu04 Cu 0.45009(2) 0.587684(18) 0.840889(13) 0.00890(6) Uani 1.000000 . .
Cu05 Cu 0.72185(2) 0.759320(18) 0.760819(13) 0.00881(6) Uani 1.000000 . .
Cu06 Cu 0.55124(2) -0.076774(18) 0.647419(13) 0.00872(6) Uani 1.000000 . .
O007 O 0.61100(11) 0.70865(11) 0.66100(8) 0.0101(3) Uani 1.000000 . .
O008 O 0.60384(12) 0.70290(11) 0.83648(7) 0.0104(3) Uani 1.000000 . .
O009 O 0.59548(12) -0.06294(11) 0.76637(8) 0.0108(3) Uani 1.000000 . .
O00A O 0.40709(12) -0.20199(11) 0.64768(7) 0.0097(3) Uani 1.000000 . .
O00B O 0.37930(12) -0.20923(11) 0.82250(8) 0.0105(3) Uani 1.000000 . .
O00C O 0.39858(11) 0.56843(11) 0.72486(8) 0.0110(3) Uani 1.000000 . .
O00D O 0.45929(12) 0.03603(11) 0.87120(8) 0.0138(3) Uani 1.000000 . .
H00e H 0.4877(13) 0.0781(8) 0.8357(7) 0.0207(4) Uiso 1.000000 GR .
H00f H 0.4810(13) 0.0680(9) 0.9166(3) 0.0207(4) Uiso 1.000000 GR .
O00E O 0.74933(12) 0.61258(11) 0.75117(8) 0.0146(3) Uani 1.000000 . .
H00a H 0.7619(16) 0.5921(8) 0.79789(9) 0.0219(5) Uiso 1.000000 GR .
H00b H 0.8088(10) 0.6223(4) 0.7262(9) 0.0219(5) Uiso 1.000000 GR .
O00F O 0.94906(13) 0.57373(11) 0.56181(8) 0.0156(3) Uani 1.000000 . .
O00G O 0.45356(13) 0.02592(11) 0.64723(8) 0.0143(3) Uani 1.000000 . .
H00g H 0.4888(8) 0.0782(7) 0.6823(7) 0.0215(4) Uiso 1.000000 GR .
H00h H 0.3820(5) -0.0084(3) 0.6590(10) 0.0215(4) Uiso 1.000000 GR .
O00H O 0.24795(13) -0.11154(11) 0.70752(8) 0.0146(3) Uani 1.000000 . .
H00i H 0.2107(14) -0.1055(7) 0.7456(6) 0.0219(5) Uiso 1.000000 GR .
H00j H 0.2066(13) -0.1139(6) 0.6629(5) 0.0219(5) Uiso 1.000000 GR .
O00I O 0.55212(13) 0.47217(11) 0.64809(8) 0.0135(3) Uani 1.000000 . .
H00c H 0.5086(7) 0.4207(7) 0.6738(9) 0.0202(4) Uiso 1.000000 GR .
H00d H 0.6195(7) 0.5029(3) 0.6767(9) 0.0202(4) Uiso 1.000000 GR .
O00J O 0.79867(13) 0.60574(13) 0.57779(9) 0.0189(3) Uani 1.000000 . .
O00K O 0.06958(13) -0.06754(12) 0.93016(9) 0.0185(3) Uani 1.000000 . .
O00L O 0.23594(13) -0.07027(12) 0.91186(9) 0.0178(3) Uani 1.000000 . .
O00M O 0.56617(14) 0.17617(12) 0.76547(9) 0.0205(3) Uani 1.000000 D .
O00N O 0.43815(14) 0.29467(12) 0.74038(9) 0.0217(3) Uani 1.000000 . .
O999 O 0.52626(14) 0.46681(12) 0.85032(9) 0.0197(3) Uani 1.000000 . .
H99a H 0.60155(19) 0.49622(13) 0.8599(11) 0.0295(5) Uiso 1.000000 GR .
H99b H 0.5077(14) 0.4299(10) 0.8063(4) 0.0295(5) Uiso 1.000000 GR .
O00P O 0.93880(14) 0.63912(14) 0.67406(9) 0.0244(4) Uani 1.000000 . .
O00Q O 0.08882(14) -0.14829(14) 0.57577(9) 0.0263(4) Uani 1.000000 D .
N00R N 0.36015(14) -0.23833(13) 0.56943(9) 0.0087(3) Uani 1.000000 . .
O113 O 0.84856(15) 0.63025(12) 0.91365(9) 0.0221(4) Uani 1.000000 . .
O224 O 0.80021(15) 0.29742(13) 0.78901(10) 0.0253(4) Uani 1.000000 D .
N97 N 0.65839(14) 0.73566(13) 0.91385(9) 0.0096(3) Uani 1.000000 . .
O112 O 0.87501(14) 0.60580(14) 1.03863(9) 0.0256(4) Uani 1.000000 . .
N85 N 0.67096(14) 0.75119(13) 0.59636(9) 0.0092(3) Uani 1.000000 . .
N00X N 0.19232(16) -0.32509(13) 0.61989(10) 0.0107(3) Uani 1.000000 . .
N00Y N 0.51961(15) -0.10933(13) 0.53322(10) 0.0112(3) Uani 1.000000 . .
N00Z N 0.30705(15) 0.49326(14) 0.58376(10) 0.0107(3) Uani 1.000000 . .
O010 O 0.30115(15) 0.14116(13) 0.75059(11) 0.0294(4) Uani 1.000000 D .
N011 N 0.46258(15) -0.14415(14) 0.96636(10) 0.0111(3) Uani 1.000000 . .
N012 N 0.82022(15) 0.82646(13) 0.85756(10) 0.0104(3) Uani 1.000000 . .
N45 N 0.28084(14) 0.49955(13) 0.71209(9) 0.0096(3) Uani 1.000000 . .
N014 N 0.16360(16) -0.33059(14) 0.78581(10) 0.0118(3) Uani 1.000000 . .
N015 N 0.49222(15) 0.62223(14) 0.95297(10) 0.0124(3) Uani 1.000000 . .
N55 N 0.31109(14) -0.25437(13) 0.88328(9) 0.0093(3) Uani 1.000000 . .
N44 N 0.71208(14) 0.00703(13) 0.78288(9) 0.0099(3) Uani 1.000000 . .
N018 N 0.28869(15) 0.50016(13) 0.84496(10) 0.0110(3) Uani 1.000000 . .
N019 N 0.52241(15) 0.62624(14) 0.52138(10) 0.0107(3) Uani 1.000000 . .
O01A O 0.24716(14) -0.08601(13) 0.51968(10) 0.0264(4) Uani 1.000000 . .
N37 N 0.71025(15) 0.02121(13) 0.65093(10) 0.0112(3) Uani 1.000000 . .
N76 N 0.82397(16) 0.84117(14) 0.68685(10) 0.0138(4) Uani 1.000000 . .
N111 N 0.81182(16) 0.58253(14) 0.97247(10) 0.0151(4) Uani 1.000000 . .
O111 O 0.71231(15) 0.51377(15) 0.96882(10) 0.0335(4) Uani 1.000000 . .
N88 N 0.68405(15) -0.00474(14) 0.91172(10) 0.0113(3) Uani 1.000000 . .
N333 N 0.13927(16) -0.12359(14) 0.51446(10) 0.0152(4) Uani 1.000000 . .
O01H O 0.25698(16) 0.27162(15) 0.73550(11) 0.0334(4) Uani 1.000000 . .
O01I O 0.07986(16) -0.14010(15) 0.44845(10) 0.0331(4) Uani 1.000000 . .
N487 N 0.89508(15) 0.60628(13) 0.60475(10) 0.0134(4) Uani 1.000000 . .
O01K O 0.09713(16) -0.10564(18) 0.81435(10) 0.0407(5) Uani 1.000000 . .
N765 N 0.13377(15) -0.08158(13) 0.88512(10) 0.0144(4) Uani 1.000000 . .
O223 O 0.71205(16) 0.39833(15) 0.80100(13) 0.0376(5) Uani 1.000000 . .
O888 O 0.06399(17) 0.01335(15) 0.67484(12) 0.0364(5) Uani 1.000000 D .
N567 N 0.33004(18) 0.23566(15) 0.74208(11) 0.0209(4) Uani 1.000000 . .
O222 O 0.90013(17) 0.46253(16) 0.81214(14) 0.0473(6) Uani 1.000000 . .
N222 N 0.80533(18) 0.38823(16) 0.80115(11) 0.0214(4) Uani 1.000000 . .
C01R C 0.23675(17) 0.46104(15) 0.63651(11) 0.0100(4) Uani 1.000000 . .
C01S C 0.19621(17) -0.31731(15) 0.86060(11) 0.0098(4) Uani 1.000000 . .
C01T C 0.24366(17) -0.30144(15) 0.55782(11) 0.0093(4) Uani 1.000000 . .
C01U C 0.35985(18) -0.21593(15) 0.95877(11) 0.0103(4) Uani 1.000000 . .
C01V C 0.22591(17) 0.46628(15) 0.77848(11) 0.0097(4) Uani 1.000000 . .
C01W C 0.77444(17) 0.80036(15) 0.92163(11) 0.0098(4) Uani 1.000000 . .
C01X C 0.09989(17) 0.39442(16) 0.76660(11) 0.0124(4) Uani 1.000000 . .
H01a H 0.09260(17) 0.32323(16) 0.77347(11) 0.0149(5) Uiso 1.000000 R .
H01b H 0.05927(17) 0.41124(16) 0.80736(11) 0.0149(5) Uiso 1.000000 R .
C01Y C 0.76987(17) 0.04839(15) 0.71919(11) 0.0096(4) Uani 1.000000 . .
C01Z C 0.75507(17) 0.03589(15) 0.86081(11) 0.0099(4) Uani 1.000000 . .
C020 C 0.42399(17) -0.18674(15) 0.51068(11) 0.0098(4) Uani 1.000000 . .
C021 C 0.89580(17) 0.12144(16) 0.73528(12) 0.0127(4) Uani 1.000000 . .
H02w H 0.93843(17) 0.11114(16) 0.69296(12) 0.0153(5) Uiso 1.000000 R .
H02x H 0.90195(17) 0.19286(16) 0.73409(12) 0.0153(5) Uiso 1.000000 R .
C022 C 0.78293(17) 0.82294(15) 0.61339(12) 0.0114(4) Uani 1.000000 . .
C023 C 0.62038(17) 0.70391(15) 0.52363(11) 0.0102(4) Uani 1.000000 . .
C024 C 0.27792(18) -0.33310(16) 0.42024(11) 0.0128(4) Uani 1.000000 . .
H02y H 0.30952(18) -0.38431(16) 0.43611(11) 0.0153(5) Uiso 1.000000 R .
H H 0.24050(18) -0.35059(16) 0.36476(11) 0.0153(5) Uiso 1.000000 R .
C025 C 0.59469(17) 0.68996(15) 0.97403(11) 0.0102(4) Uani 1.000000 . .
C026 C 0.18827(17) -0.33561(16) 0.47422(11) 0.0118(4) Uani 1.000000 . .
H02z H 0.12708(17) -0.40637(16) 0.47313(11) 0.0142(5) Uiso 1.000000 R .
Ha H 0.15057(17) -0.29011(16) 0.45425(11) 0.0142(5) Uiso 1.000000 R .
C027 C 0.75042(18) 0.82964(16) 1.06259(11) 0.0132(4) Uani 1.000000 . .
H02a H 0.79174(18) 0.84580(16) 1.11714(11) 0.0158(5) Uiso 1.000000 R .
H02b H 0.71877(18) 0.88167(16) 1.04993(11) 0.0158(5) Uiso 1.000000 R .
C028 C 0.37582(18) -0.22646(16) 0.42662(11) 0.0120(4) Uani 1.000000 . .
H02 H 0.34657(18) -0.17850(16) 0.39999(11) 0.0144(5) Uiso 1.000000 R .
Hb H 0.43959(18) -0.22785(16) 0.39837(11) 0.0144(5) Uiso 1.000000 R .
C029 C 0.04170(17) 0.40077(16) 0.68488(12) 0.0129(4) Uani 1.000000 . .
H02c H -0.03904(17) 0.34717(16) 0.67670(12) 0.0155(5) Uiso 1.000000 R .
H02d H 0.03837(17) 0.46872(16) 0.68020(12) 0.0155(5) Uiso 1.000000 R .
C02A C 0.83528(17) 0.83312(16) 1.00441(11) 0.0121(4) Uani 1.000000 . .
H02e H 0.87402(17) 0.78729(16) 1.02141(11) 0.0145(5) Uiso 1.000000 R .
H02f H 0.89624(17) 0.90391(16) 1.00501(11) 0.0145(5) Uiso 1.000000 R .
C02B C 0.95238(17) 0.10624(17) 0.81527(12) 0.0136(4) Uani 1.000000 . .
H0aa H 0.95669(17) 0.03846(17) 0.81462(12) 0.0163(5) Uiso 1.000000 R .
Hc H 1.03261(17) 0.16017(17) 0.82664(12) 0.0163(5) Uiso 1.000000 R .
C02C C 0.87901(17) 0.11230(16) 0.87883(12) 0.0140(4) Uani 1.000000 . .
H1aa H 0.88123(17) 0.18239(16) 0.88238(12) 0.0168(5) Uiso 1.000000 R .
Hd H 0.91258(17) 0.09902(16) 0.93078(12) 0.0168(5) Uiso 1.000000 R .
C02D C 0.15847(18) -0.29874(17) 0.99997(12) 0.0156(4) Uani 1.000000 . .
H2aa H 0.14056(18) -0.23784(17) 0.99137(12) 0.0188(5) Uiso 1.000000 R .
He H 0.11461(18) -0.33727(17) 1.04260(12) 0.0188(5) Uiso 1.000000 R .
C02E C 0.12137(18) -0.36673(16) 0.92410(12) 0.0138(4) Uani 1.000000 . .
H3aa H 0.03913(18) -0.38131(16) 0.90481(12) 0.0165(5) Uiso 1.000000 R .
Hf H 0.12628(18) -0.43296(16) 0.93553(12) 0.0165(5) Uiso 1.000000 R .
C02F C 0.68336(19) 0.74741(17) 0.45360(12) 0.0152(4) Uani 1.000000 . .
H02g H 0.72599(19) 0.70593(17) 0.43992(12) 0.0183(5) Uiso 0.596(6) R 1
H02h H 0.62550(19) 0.74207(17) 0.40762(12) 0.0183(5) Uiso 0.596(6) R 1
H02i H 0.66627(19) 0.69071(17) 0.41384(12) 0.0183(5) Uiso 0.404(6) R 2
H02j H 0.65261(19) 0.79564(17) 0.42916(12) 0.0183(5) Uiso 0.404(6) R 2
C02G C 0.65164(18) 0.72371(16) 1.05743(11) 0.0138(4) Uani 1.000000 . .
H02k H 0.59256(18) 0.72418(16) 1.09088(11) 0.0166(5) Uiso 1.000000 R .
H02l H 0.68226(18) 0.67374(16) 1.07843(11) 0.0166(5) Uiso 1.000000 R .
C02H C 0.11196(17) 0.38517(16) 0.62237(12) 0.0143(4) Uani 1.000000 . .
H02m H 0.07722(17) 0.39327(16) 0.56913(12) 0.0171(5) Uiso 1.000000 R .
H02n H 0.10835(17) 0.31455(16) 0.62388(12) 0.0171(5) Uiso 1.000000 R .
C02I C 0.84575(19) 0.87306(17) 0.54478(12) 0.0183(5) Uani 1.000000 . .
H02o H 0.88752(19) 0.94782(17) 0.55778(12) 0.0220(6) Uiso 0.596(6) R 1
H02p H 0.90482(19) 0.84586(17) 0.53733(12) 0.0220(6) Uiso 0.596(6) R 1
H02q H 0.82737(19) 0.93269(17) 0.53120(12) 0.0220(6) Uiso 0.404(6) R 2
H02r H 0.93082(19) 0.89926(17) 0.56111(12) 0.0220(6) Uiso 0.404(6) R 2
C02J C 0.28920(18) -0.26428(17) 1.02470(12) 0.0148(4) Uani 1.000000 . .
H4aa H 0.30464(18) -0.32442(17) 1.04146(12) 0.0178(5) Uiso 1.000000 R .
Hg H 0.31404(18) -0.21420(17) 1.07067(12) 0.0178(5) Uiso 1.000000 R .
C02L C 0.7671(3) 0.8565(3) 0.4685(2) 0.0157(10) Uani 0.596(6) D 1
H02s H 0.8151(3) 0.8776(3) 0.4242(2) 0.0188(12) Uiso 0.596(6) DR 1
H02t H 0.7234(3) 0.9002(3) 0.4702(2) 0.0188(12) Uiso 0.596(6) R 1
C02M C 0.8153(4) 0.8036(4) 0.4736(3) 0.0153(14) Uani 0.404(6) D 2
H02u H 0.8497(4) 0.7528(4) 0.4827(3) 0.0183(17) Uiso 0.404(6) DR 2
H02v H 0.8485(4) 0.8439(4) 0.4283(3) 0.0183(17) Uiso 0.404(6) R 2
H00k H 0.6484(4) 0.2275(4) 0.7732(3) 0.000(5) Uiso 1.000000 DGR .
H00l H 0.5280(4) 0.2098(4) 0.7589(3) 0.004(5) Uiso 1.000000 GR .
H37 H 0.747(2) 0.0467(19) 0.6146(15) 0.019(7) Uiso 1.000000 . .
H88 H 0.709(2) 0.013(2) 0.9569(15) 0.019(7) Uiso 1.000000 . .
H012 H 0.890(2) 0.859(2) 0.8635(15) 0.025(7) Uiso 1.000000 . .
H00Y H 0.557(2) -0.077(2) 0.4985(16) 0.024(7) Uiso 1.000000 . .
H015 H 0.458(2) 0.593(2) 0.9873(16) 0.026(7) Uiso 1.000000 . .
H00Z H 0.280(2) 0.470(2) 0.5425(16) 0.022(7) Uiso 1.000000 . .
H00X H 0.125(2) -0.3578(19) 0.6111(14) 0.012(6) Uiso 1.000000 . .
H76 H 0.887(2) 0.883(2) 0.6941(15) 0.022(7) Uiso 1.000000 . .
H019 H 0.495(2) 0.601(2) 0.4784(16) 0.022(7) Uiso 1.000000 . .
H014 H 0.096(2) -0.366(2) 0.7736(16) 0.027(8) Uiso 1.000000 . .
H011 H 0.485(2) -0.127(2) 1.0060(16) 0.022(8) Uiso 1.000000 . .
H018 H 0.252(2) 0.478(2) 0.8833(16) 0.028(7) Uiso 1.000000 . .
H88a H 0.123(19) -0.011(4) 0.643(8) 1.0(2) Uiso 1.000000 D .
H88b H 0.1367(15) 0.066(2) 0.7105(16) 0.047(9) Uiso 1.000000 D .


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
Cu01 O00A 2.0039(13) . ?
Cu01 O00B 1.9912(13) . ?
Cu01 O00H 2.2826(14) . ?
Cu01 N00X 1.9212(18) . ?
Cu01 N014 1.9355(17) . ?
Cu02 O009 2.0004(13) . ?
Cu02 O00B 1.9796(14) . ?
Cu02 O00D 2.3662(15) . ?
Cu02 N011 1.9389(17) . ?
Cu02 N88 1.9379(17) . ?
Cu03 O007 1.9862(14) . ?
Cu03 O00C 1.9835(13) . ?
Cu03 O00I 2.3654(14) . ?
Cu03 N00Z 1.9341(18) . ?
Cu03 N019 1.9375(17) . ?
Cu04 O008 1.9811(13) . ?
Cu04 O00C 1.9903(13) . ?
Cu04 O999 2.2889(15) . ?
Cu04 N015 1.9281(17) . ?
Cu04 N018 1.9212(17) . ?
Cu05 O007 2.0027(14) . ?
Cu05 O008 1.9974(13) . ?
Cu05 O00E 2.2644(14) . ?
Cu05 N012 1.9339(17) . ?
Cu05 N76 1.9392(18) . ?
Cu06 O009 2.0255(13) . ?
Cu06 O00A 1.9674(14) . ?
Cu06 O00G 2.2664(14) . ?
Cu06 N00Y 1.9546(17) . ?
Cu06 N37 1.9210(17) . ?
O007 N85 1.4030(19) . ?
O008 N97 1.400(2) . ?
O009 N44 1.400(2) . ?
O00A N00R 1.401(2) . ?
O00B N55 1.4067(19) . ?
O00C N45 1.403(2) . ?
O00D H00e 0.8542 . ?
O00D H00f 0.8539 . ?
O00E H00a 0.8681 . ?
O00E H00b 0.8674 . ?
O00F N487 1.257(2) . ?
O00G H00g 0.8829 . ?
O00G H00h 0.8829 . ?
O00H H00i 0.8662 . ?
O00H H00j 0.8652 . ?
O00I H00c 0.8719 . ?
O00I H00d 0.8708 . ?
O00J N487 1.251(2) . ?
O00K N765 1.247(2) . ?
O00L N765 1.265(2) . ?
O00M H00k 0.993(5) . ?
O00M H00l 0.807(5) . ?
O00N N567 1.285(2) . ?
O999 H99a 0.8658 . ?
O999 H99b 0.8659 . ?
O00P N487 1.248(2) . ?
O00Q N333 1.260(2) . ?
N00R C01T 1.370(2) . ?
N00R C020 1.376(2) . ?
O113 N111 1.237(2) . ?
O224 N222 1.285(2) . ?
N97 C01W 1.371(2) . ?
N97 C025 1.372(2) . ?
O112 N111 1.264(2) . ?
N85 C022 1.366(3) . ?
N85 C023 1.365(3) . ?
N00X C01T 1.276(2) . ?
N00X H00X 0.78(2) . ?
N00Y C020 1.280(3) . ?
N00Y H00Y 0.82(3) . ?
N00Z C01R 1.286(3) . ?
N00Z H00Z 0.76(3) . ?
O010 N567 1.259(2) . ?
N011 C01U 1.278(3) . ?
N011 H011 0.70(3) . ?
N012 C01W 1.277(2) . ?
N012 H012 0.80(3) . ?
N45 C01R 1.361(2) . ?
N45 C01V 1.376(2) . ?
N014 C01S 1.282(3) . ?
N014 H014 0.80(3) . ?
N015 C025 1.272(3) . ?
N015 H015 0.78(3) . ?
N55 C01S 1.371(2) . ?
N55 C01U 1.369(2) . ?
N44 C01Y 1.373(2) . ?
N44 C01Z 1.370(2) . ?
N018 C01V 1.276(3) . ?
N018 H018 0.83(3) . ?
N019 C023 1.280(3) . ?
N019 H019 0.79(3) . ?
O01A N333 1.239(2) . ?
N37 C01Y 1.278(3) . ?
N37 H37 0.81(3) . ?
N76 C022 1.282(3) . ?
N76 H76 0.77(3) . ?
N111 O111 1.237(2) . ?
N88 C01Z 1.283(3) . ?
N88 H88 0.80(3) . ?
N333 O01I 1.244(2) . ?
O01H N567 1.221(3) . ?
O01K N765 1.235(2) . ?
O223 N222 1.244(2) . ?
O888 H88a 1.13(10) . ?
O888 H88b 1.044(14) . ?
O222 N222 1.230(3) . ?
C01R C02H 1.499(3) . ?
C01S C02E 1.500(3) . ?
C01T C026 1.499(3) . ?
C01U C02J 1.503(3) . ?
C01V C01X 1.494(3) . ?
C01W C02A 1.502(3) . ?
C01X H01a 0.9900 . ?
C01X H01b 0.9900 . ?
C01X C029 1.520(3) . ?
C01Y C021 1.500(3) . ?
C01Z C02C 1.497(3) . ?
C020 C028 1.503(3) . ?
C021 H02w 0.9900 . ?
C021 H02x 0.9900 . ?
C021 C02B 1.524(3) . ?
C022 C02I 1.502(3) . ?
C023 C02F 1.501(3) . ?
C024 H02y 0.9900 . ?
C024 H 0.9900 . ?
C024 C026 1.526(3) . ?
C024 C028 1.516(3) . ?
C025 C02G 1.500(3) . ?
C026 H02z 0.9900 . ?
C026 Ha 0.9900 . ?
C027 H02a 0.9900 . ?
C027 H02b 0.9900 . ?
C027 C02A 1.525(3) . ?
C027 C02G 1.514(3) . ?
C028 H02 0.9900 . ?
C028 Hb 0.9900 . ?
C029 H02c 0.9900 . ?
C029 H02d 0.9900 . ?
C029 C02H 1.529(3) . ?
C02A H02e 0.9900 . ?
C02A H02f 0.9900 . ?
C02B H0aa 0.9900 . ?
C02B Hc 0.9900 . ?
C02B C02C 1.525(3) . ?
C02C H1aa 0.9900 . ?
C02C Hd 0.9900 . ?
C02D H2aa 0.9900 . ?
C02D He 0.9900 . ?
C02D C02E 1.521(3) . ?
C02D C02J 1.528(3) . ?
C02E H3aa 0.9900 . ?
C02E Hf 0.9900 . ?
C02F H02g 0.9900 . ?
C02F H02h 0.9900 . ?
C02F H02i 0.9900 . ?
C02F H02j 0.9900 . ?
C02F C02L 1.485(4) . ?
C02F C02M 1.525(5) . ?
C02G H02k 0.9900 . ?
C02G H02l 0.9900 . ?
C02H H02m 0.9900 . ?
C02H H02n 0.9900 . ?
C02I H02o 0.9900 . ?
C02I H02p 0.9900 . ?
C02I H02q 0.9900 . ?
C02I H02r 0.9900 . ?
C02I C02L 1.500(4) . ?
C02I C02M 1.475(5) . ?
C02J H4aa 0.9900 . ?
C02J Hg 0.9900 . ?
C02L H02s 0.9900 . ?
C02L H02t 0.9900 . ?
C02M H02u 0.9900 . ?
C02M H02v 0.9900 . ?

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
O00B Cu01 O00A 98.68(5) . . ?
O00H Cu01 O00A 90.47(5) . . ?
O00H Cu01 O00B 93.30(6) . . ?
N00X Cu01 O00A 81.12(6) . . ?
N00X Cu01 O00B 169.56(7) . . ?
N00X Cu01 O00H 97.14(6) . . ?
N014 Cu01 O00A 170.68(7) . . ?
N014 Cu01 O00B 81.75(6) . . ?
N014 Cu01 O00H 98.81(6) . . ?
N014 Cu01 N00X 96.76(7) . . ?
O00B Cu02 O009 95.65(5) . . ?
O00D Cu02 O009 97.13(5) . . ?
O00D Cu02 O00B 98.28(5) . . ?
N011 Cu02 O009 172.91(7) . . ?
N011 Cu02 O00B 81.76(7) . . ?
N011 Cu02 O00D 89.79(6) . . ?
N88 Cu02 O009 81.97(6) . . ?
N88 Cu02 O00B 168.93(7) . . ?
N88 Cu02 O00D 92.76(6) . . ?
N88 Cu02 N011 99.30(7) . . ?
O00C Cu03 O007 95.95(5) . . ?
O00I Cu03 O007 92.18(5) . . ?
O00I Cu03 O00C 93.32(5) . . ?
N00Z Cu03 O007 167.94(7) . . ?
N00Z Cu03 O00C 82.02(6) . . ?
N00Z Cu03 O00I 99.79(6) . . ?
N019 Cu03 O007 81.78(6) . . ?
N019 Cu03 O00C 171.51(7) . . ?
N019 Cu03 O00I 94.94(6) . . ?
N019 Cu03 N00Z 98.49(7) . . ?
O00C Cu04 O008 97.09(5) . . ?
O999 Cu04 O008 93.58(6) . . ?
O999 Cu04 O00C 97.66(6) . . ?
N015 Cu04 O008 81.87(6) . . ?
N015 Cu04 O00C 171.64(7) . . ?
N015 Cu04 O999 90.69(7) . . ?
N018 Cu04 O008 167.08(7) . . ?
N018 Cu04 O00C 82.08(6) . . ?
N018 Cu04 O999 99.31(7) . . ?
N018 Cu04 N015 97.07(7) . . ?
O008 Cu05 O007 97.06(5) . . ?
O00E Cu05 O007 86.92(5) . . ?
O00E Cu05 O008 93.39(5) . . ?
N012 Cu05 O007 170.50(7) . . ?
N012 Cu05 O008 81.46(6) . . ?
N012 Cu05 O00E 102.52(6) . . ?
N76 Cu05 O007 81.44(7) . . ?
N76 Cu05 O008 166.01(7) . . ?
N76 Cu05 O00E 100.39(7) . . ?
N76 Cu05 N012 97.71(7) . . ?
O00A Cu06 O009 95.61(5) . . ?
O00G Cu06 O009 94.67(5) . . ?
O00G Cu06 O00A 92.27(5) . . ?
N00Y Cu06 O009 169.60(7) . . ?
N00Y Cu06 O00A 82.36(6) . . ?
N00Y Cu06 O00G 95.60(6) . . ?
N37 Cu06 O009 81.46(6) . . ?
N37 Cu06 O00A 165.38(7) . . ?
N37 Cu06 O00G 102.22(6) . . ?
N37 Cu06 N00Y 97.92(7) . . ?
Cu05 O007 Cu03 138.31(7) . . ?
N85 O007 Cu03 109.22(10) . . ?
N85 O007 Cu05 108.83(10) . . ?
Cu05 O008 Cu04 139.01(7) . . ?
N97 O008 Cu04 108.84(10) . . ?
N97 O008 Cu05 109.18(10) . . ?
Cu06 O009 Cu02 142.23(7) . . ?
N44 O009 Cu02 108.56(10) . . ?
N44 O009 Cu06 108.28(10) . . ?
Cu06 O00A Cu01 135.84(7) . . ?
N00R O00A Cu01 109.32(10) . . ?
N00R O00A Cu06 109.28(10) . . ?
Cu02 O00B Cu01 139.29(7) . . ?
N55 O00B Cu01 109.05(10) . . ?
N55 O00B Cu02 109.51(10) . . ?
Cu04 O00C Cu03 140.46(7) . . ?
N45 O00C Cu03 109.05(10) . . ?
N45 O00C Cu04 108.67(10) . . ?
H00e O00D Cu02 109.5 . . ?
H00f O00D Cu02 109.5 . . ?
H00f O00D H00e 109.3 . . ?
H00a O00E Cu05 110.6 . . ?
H00b O00E Cu05 110.4 . . ?
H00b O00E H00a 108.5 . . ?
H00g O00G Cu06 111.4 . . ?
H00h O00G Cu06 111.0 . . ?
H00h O00G H00g 107.6 . . ?
H00i O00H Cu01 110.3 . . ?
H00j O00H Cu01 110.2 . . ?
H00j O00H H00i 108.6 . . ?
H00c O00I Cu03 110.9 . . ?
H00d O00I Cu03 110.2 . . ?
H00d O00I H00c 108.2 . . ?
H00l O00M H00k 104.8(5) . . ?
H99a O999 Cu04 110.3 . . ?
H99b O999 Cu04 110.1 . . ?
H99b O999 H99a 108.6 . . ?
C01T N00R O00A 116.01(14) . . ?
C020 N00R O00A 116.90(15) . . ?
C020 N00R C01T 124.48(16) . . ?
C01W N97 O008 116.36(15) . . ?
C025 N97 O008 116.71(15) . . ?
C025 N97 C01W 126.38(16) . . ?
C022 N85 O007 116.78(15) . . ?
C023 N85 O007 116.61(15) . . ?
C023 N85 C022 125.42(16) . . ?
C01T N00X Cu01 116.92(15) . . ?
H00X N00X Cu01 128.1(17) . . ?
H00X N00X C01T 113.8(17) . . ?
C020 N00Y Cu06 114.77(13) . . ?
H00Y N00Y Cu06 128.1(19) . . ?
H00Y N00Y C020 116.9(19) . . ?
C01R N00Z Cu03 115.58(14) . . ?
H00Z N00Z Cu03 131(2) . . ?
H00Z N00Z C01R 113(2) . . ?
C01U N011 Cu02 115.76(14) . . ?
H011 N011 Cu02 131(2) . . ?
H011 N011 C01U 113(2) . . ?
C01W N012 Cu05 116.05(14) . . ?
H012 N012 Cu05 127.5(19) . . ?
H012 N012 C01W 114.8(19) . . ?
C01R N45 O00C 116.90(15) . . ?
C01V N45 O00C 116.60(15) . . ?
C01V N45 C01R 125.80(17) . . ?
C01S N014 Cu01 116.34(14) . . ?
H014 N014 Cu01 128.7(19) . . ?
H014 N014 C01S 114.8(19) . . ?
C025 N015 Cu04 116.08(14) . . ?
H015 N015 Cu04 127(2) . . ?
H015 N015 C025 116(2) . . ?
C01S N55 O00B 116.82(15) . . ?
C01U N55 O00B 116.16(15) . . ?
C01U N55 C01S 125.76(16) . . ?
C01Y N44 O009 116.91(15) . . ?
C01Z N44 O009 117.28(15) . . ?
C01Z N44 C01Y 125.48(17) . . ?
C01V N018 Cu04 116.33(14) . . ?
H018 N018 Cu04 130.7(19) . . ?
H018 N018 C01V 112.9(19) . . ?
C023 N019 Cu03 115.78(14) . . ?
H019 N019 Cu03 129.9(19) . . ?
H019 N019 C023 114.4(19) . . ?
C01Y N37 Cu06 116.96(14) . . ?
H37 N37 Cu06 129.1(18) . . ?
H37 N37 C01Y 113.9(18) . . ?
C022 N76 Cu05 116.06(15) . . ?
H76 N76 Cu05 130.5(19) . . ?
H76 N76 C022 113.4(19) . . ?
O112 N111 O113 120.05(19) . . ?
O111 N111 O113 121.39(18) . . ?
O111 N111 O112 118.52(17) . . ?
C01Z N88 Cu02 115.75(14) . . ?
H88 N88 Cu02 127.9(18) . . ?
H88 N88 C01Z 116.3(19) . . ?
O01A N333 O00Q 120.24(18) . . ?
O01I N333 O00Q 119.46(19) . . ?
O01I N333 O01A 120.27(18) . . ?
O00J N487 O00F 119.97(16) . . ?
O00P N487 O00F 119.35(17) . . ?
O00P N487 O00J 120.68(17) . . ?
O00L N765 O00K 119.99(17) . . ?
O01K N765 O00K 119.49(18) . . ?
O01K N765 O00L 120.52(17) . . ?
H88b O888 H88a 89(10) . . ?
O010 N567 O00N 119.19(19) . . ?
O01H N567 O00N 119.9(2) . . ?
O01H N567 O010 120.9(2) . . ?
O223 N222 O224 118.1(2) . . ?
O222 N222 O224 120.4(2) . . ?
O222 N222 O223 121.5(2) . . ?
N45 C01R N00Z 116.45(18) . . ?
C02H C01R N00Z 126.08(18) . . ?
C02H C01R N45 117.48(17) . . ?
N55 C01S N014 116.02(17) . . ?
C02E C01S N014 125.92(18) . . ?
C02E C01S N55 118.03(17) . . ?
N00X C01T N00R 116.28(18) . . ?
C026 C01T N00R 117.59(16) . . ?
C026 C01T N00X 126.13(18) . . ?
N55 C01U N011 116.60(17) . . ?
C02J C01U N011 126.37(18) . . ?
C02J C01U N55 117.01(17) . . ?
N018 C01V N45 116.14(18) . . ?
C01X C01V N45 117.73(17) . . ?
C01X C01V N018 126.13(18) . . ?
N012 C01W N97 116.56(18) . . ?
C02A C01W N97 116.98(16) . . ?
C02A C01W N012 126.45(18) . . ?
H01a C01X C01V 109.24(11) . . ?
H01b C01X C01V 109.24(11) . . ?
H01b C01X H01a 107.9 . . ?
C029 C01X C01V 111.87(16) . . ?
C029 C01X H01a 109.24(12) . . ?
C029 C01X H01b 109.24(11) . . ?
N37 C01Y N44 116.35(18) . . ?
C021 C01Y N44 117.90(17) . . ?
C021 C01Y N37 125.76(17) . . ?
N88 C01Z N44 116.38(18) . . ?
C02C C01Z N44 117.59(16) . . ?
C02C C01Z N88 126.03(18) . . ?
N00Y C020 N00R 116.46(17) . . ?
C028 C020 N00R 117.37(17) . . ?
C028 C020 N00Y 126.17(17) . . ?
H02w C021 C01Y 109.21(11) . . ?
H02x C021 C01Y 109.21(11) . . ?
H02x C021 H02w 107.9 . . ?
C02B C021 C01Y 111.99(16) . . ?
C02B C021 H02w 109.21(11) . . ?
C02B C021 H02x 109.21(12) . . ?
N76 C022 N85 116.45(17) . . ?
C02I C022 N85 117.22(18) . . ?
C02I C022 N76 126.33(19) . . ?
N019 C023 N85 116.60(17) . . ?
C02F C023 N85 117.63(18) . . ?
C02F C023 N019 125.77(18) . . ?
H C024 H02y 108.3 . . ?
C026 C024 H02y 109.86(11) . . ?
C026 C024 H 109.86(10) . . ?
C028 C024 H02y 109.86(11) . . ?
C028 C024 H 109.86(10) . . ?
C028 C024 C026 109.12(16) . . ?
N015 C025 N97 116.01(17) . . ?
C02G C025 N97 117.59(17) . . ?
C02G C025 N015 126.40(18) . . ?
C024 C026 C01T 111.43(16) . . ?
H02z C026 C01T 109.34(11) . . ?
H02z C026 C024 109.34(11) . . ?
Ha C026 C01T 109.34(11) . . ?
Ha C026 C024 109.34(11) . . ?
Ha C026 H02z 108.0 . . ?
H02b C027 H02a 108.2 . . ?
C02A C027 H02a 109.74(11) . . ?
C02A C027 H02b 109.74(11) . . ?
C02G C027 H02a 109.74(10) . . ?
C02G C027 H02b 109.74(11) . . ?
C02G C027 C02A 109.66(17) . . ?
C024 C028 C020 113.24(16) . . ?
H02 C028 C020 108.93(11) . . ?
H02 C028 C024 108.93(11) . . ?
Hb C028 C020 108.93(11) . . ?
Hb C028 C024 108.93(11) . . ?
Hb C028 H02 107.7 . . ?
H02c C029 C01X 109.89(11) . . ?
H02d C029 C01X 109.89(12) . . ?
H02d C029 H02c 108.3 . . ?
C02H C029 C01X 108.97(16) . . ?
C02H C029 H02c 109.89(11) . . ?
C02H C029 H02d 109.89(11) . . ?
C027 C02A C01W 111.68(16) . . ?
H02e C02A C01W 109.28(11) . . ?
H02e C02A C027 109.28(11) . . ?
H02f C02A C01W 109.28(11) . . ?
H02f C02A C027 109.28(11) . . ?
H02f C02A H02e 107.9 . . ?
H0aa C02B C021 109.99(12) . . ?
Hc C02B C021 109.99(11) . . ?
Hc C02B H0aa 108.4 . . ?
C02C C02B C021 108.51(16) . . ?
C02C C02B H0aa 109.99(11) . . ?
C02C C02B Hc 109.99(11) . . ?
C02B C02C C01Z 111.41(17) . . ?
H1aa C02C C01Z 109.35(11) . . ?
H1aa C02C C02B 109.35(11) . . ?
Hd C02C C01Z 109.35(11) . . ?
Hd C02C C02B 109.35(11) . . ?
Hd C02C H1aa 108.0 . . ?
He C02D H2aa 108.2 . . ?
C02E C02D H2aa 109.70(12) . . ?
C02E C02D He 109.70(11) . . ?
C02J C02D H2aa 109.70(12) . . ?
C02J C02D He 109.70(10) . . ?
C02J C02D C02E 109.82(17) . . ?
C02D C02E C01S 111.94(17) . . ?
H3aa C02E C01S 109.23(11) . . ?
H3aa C02E C02D 109.23(11) . . ?
Hf C02E C01S 109.23(11) . . ?
Hf C02E C02D 109.23(11) . . ?
Hf C02E H3aa 107.9 . . ?
H02h C02F H02g 107.8 . . ?
H02j C02F H02i 107.6 . . ?
C02L C02F H02g 109.04(16) . . ?
C02L C02F H02h 109.04(16) . . ?
C02M C02F H02i 108.7(2) . . ?
C02M C02F H02j 108.7(2) . . ?
C027 C02G C025 112.09(16) . . ?
H02k C02G C025 109.19(11) . . ?
H02k C02G C027 109.19(11) . . ?
H02l C02G C025 109.19(11) . . ?
H02l C02G C027 109.19(11) . . ?
H02l C02G H02k 107.9 . . ?
C029 C02H C01R 111.07(17) . . ?
H02m C02H C01R 109.42(11) . . ?
H02m C02H C029 109.42(11) . . ?
H02n C02H C01R 109.42(11) . . ?
H02n C02H C029 109.42(11) . . ?
H02n C02H H02m 108.0 . . ?
H02p C02I H02o 107.7 . . ?
H02r C02I H02q 107.7 . . ?
C02L C02I H02o 108.79(16) . . ?
C02L C02I H02p 108.79(16) . . ?
C02M C02I H02q 108.8(2) . . ?
C02M C02I H02r 108.8(2) . . ?
C02D C02J C01U 112.20(17) . . ?
H4aa C02J C01U 109.17(11) . . ?
H4aa C02J C02D 109.17(12) . . ?
Hg C02J C01U 109.17(11) . . ?
Hg C02J C02D 109.17(11) . . ?
Hg C02J H4aa 107.9 . . ?
C02I C02L C02F 111.9(2) . . ?
H02t C02L H02s 107.9 . . ?
C02I C02M C02F 111.1(3) . . ?
H02v C02M H02u 108.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O00M H00k 1 0.9920 0.0200 -0.0006
O00Q H88a 1 2.0600 0.0200 -0.0695
O224 H00k 1 1.7500 0.0200 -0.0051
O010 H88b 1 2.0000 0.0200 0.0484
O888 H88a 1 1.0000 0.0200 -0.1260
O888 H88b 1 0.9500 0.0200 -0.0943
C02L H02s 1 0.9900 0.0200 -0.0000
C02M H02u 1 0.9900 0.0200 0.0000

####################################################################### 
# 
# 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_fuls
_database_code_depnum_ccdc_archive 'CCDC 1454629'
_audit_update_record             
;
2016-02-18 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_vrf_PLAT417_                    
;
PROBLEM: _A Note: Short Inter D-H..H-D     H5A     H14A        1.18 Ang. 
PROBLEM: _A Note: Short Inter D-H..H-D     H0AB    H0AB      1.27 Ang.
PROBLEM: _A Note: Short Inter D-H..H-D     H33A   H1AC       1.18 Ang.
RESPONSE: This due to a disordered water molecule.  
;

_audit_creation_date             2016-02-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C15 H36 N9 Ni3 O9, 3(Cl), 4(H2 O)'
_chemical_formula_sum            'C15 H44 Cl3 N9 Ni3 O13'
_chemical_formula_weight         841.07
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   17.1605(12)
_cell_length_b                   13.4761(10)
_cell_length_c                   14.8097(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.774(4)
_cell_angle_gamma                90.00
_cell_volume                     3180.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.342
_cell_measurement_theta_min      2.556
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0827 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.8595.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32907
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.98
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Bruker-APEXII-CCD
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                7035
_reflns_number_total             7953
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7953
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0330P)²+5.2250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0765
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1AB-H1AD
 0.84 with sigma of 0.01
 O1AB-H1AC
 0.84 with sigma of 0.01
 O1AA-H1AA
 0.84 with sigma of 0.01
 O1AB-O33
 2.909 with sigma of 0.01
 H1AD-H30A
 2.289 with sigma of 0.01
 H1AD-H1AA
 0.543 with sigma of 0.01
 H1AD-H1AC
 1.34 with sigma of 0.02
3. Others
 Sof(O1AB)=Sof(H1AC)=Sof(H1AD)=1-FVAR(1)
 Sof(O1AA)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(H38C)=Sof(H38D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H38A)=Sof(H38B)=FVAR(2)
4.a Free rotating group:
 O19(H19A,H19B), O33(H33A,H33B), O0AA(H0AA,H0AB), O1AA(H1AA,H1AB), O1AB(H1AC,
 H1AD)
4.b Rotating group:
 O2(H2A,H2B), O4(H4A,H4B), O5(H5A,H5B), O7(H7A,H7B), O12(H12A,H12B), O14(H14A,
 H14B)
4.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C32(H32C,H32D), C34(H34A,H34B), C36(H36A,H36B),
 C38(H38A,H38B), C38(H38C,H38D), C36A(H36C,H36D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Ni1 Ni 0.329439(16) 0.308295(18) 0.183270(18) 0.00849(6) Uani 1 d . . .
Ni2 Ni 0.192425(16) 0.171147(19) 0.289210(18) 0.00940(6) Uani 1 d . . .
Ni3 Ni 0.173618(16) 0.451683(19) 0.258144(18) 0.00952(6) Uani 1 d . . .
Cl6 Cl -0.09607(4) 0.40156(5) 0.05924(4) 0.02647(13) Uani 1 d . . .
O1 O 0.29071(9) 0.19788(10) 0.24899(10) 0.0099(3) Uani 1 d . . .
O2 O 0.12619(9) 0.13873(11) 0.13669(11) 0.0144(3) Uani 1 d . . .
H2A H 0.0735 0.1388 0.1240 0.022 Uiso 1 d . . GR
H2B H 0.1408 0.0820 0.1232 0.022 Uiso 1 d . . GR
O3 O 0.27220(9) 0.42641(10) 0.21776(10) 0.0107(3) Uani 1 d . . .
O4 O 0.25681(9) 0.43485(11) 0.40614(10) 0.0143(3) Uani 1 d . . .
H4A H 0.2354 0.4624 0.4434 0.021 Uiso 1 d . . GR
H4B H 0.3035 0.4621 0.4141 0.021 Uiso 1 d . . GR
O5 O 0.20338(9) 0.28778(11) 0.06827(10) 0.0122(3) Uani 1 d . . .
H5A H 0.2070 0.2934 0.0128 0.018 Uiso 1 d . . GR
H5B H 0.1702 0.3321 0.0744 0.018 Uiso 1 d . . GR
N6 N 0.09659(11) 0.14399(14) 0.33096(13) 0.0132(3) Uani 1 d . . .
O7 O 0.09901(10) 0.44223(11) 0.10141(10) 0.0146(3) Uani 1 d . . .
H7A H 0.1023 0.4969 0.0744 0.022 Uiso 1 d . . GR
H7B H 0.0481 0.4307 0.0927 0.022 Uiso 1 d . . GR
N8 N 0.07339(11) 0.47549(14) 0.29261(13) 0.0135(3) Uani 1 d . . .
N9 N 0.38574(12) 0.19139(13) 0.14963(13) 0.0140(3) Uani 1 d . . .
O10 O 0.13373(9) 0.30779(10) 0.26327(10) 0.0108(3) Uani 1 d . . .
N11 N 0.21031(11) 0.59109(13) 0.24703(13) 0.0133(3) Uani 1 d . . .
O12 O 0.43399(9) 0.33362(11) 0.31174(10) 0.0134(3) Uani 1 d . . .
H12A H 0.4399 0.2856 0.3512 0.020 Uiso 1 d . . GR
H12B H 0.4263 0.3871 0.3378 0.020 Uiso 1 d . . GR
N13 N 0.36009(11) 0.41568(13) 0.10973(13) 0.0128(3) Uani 1 d . . .
O14 O 0.26904(9) 0.23183(11) 0.42610(10) 0.0122(3) Uani 1 d . . .
H14A H 0.2529 0.2097 0.4701 0.018 Uiso 1 d . . GR
H14B H 0.2646 0.2947 0.4236 0.018 Uiso 1 d . . GR
C15 C 0.30991(14) 0.02822(16) 0.28670(15) 0.0150(4) Uani 1 d A . .
N16 N 0.24961(12) 0.03880(14) 0.31729(13) 0.0150(4) Uani 1 d . . .
N18 N 0.29117(11) 0.51300(13) 0.17952(12) 0.0109(3) Uani 1 d . . .
O19 O -0.03916(11) 0.16786(14) 0.09678(13) 0.0251(4) Uani 1 d . . .
H19A H -0.0568 0.2274 0.0870 0.038 Uiso 1 d . . G
H19B H -0.0754 0.1296 0.0576 0.038 Uiso 1 d . . G
N20 N 0.07165(11) 0.30814(13) 0.30281(13) 0.0125(3) Uani 1 d . . .
N21 N 0.33111(11) 0.10979(12) 0.24559(12) 0.0113(3) Uani 1 d . . .
C22 C 0.05353(13) 0.21951(17) 0.33644(14) 0.0139(4) Uani 1 d . . .
C23 C 0.33787(13) 0.50349(16) 0.12178(14) 0.0123(4) Uani 1 d . . .
C24 C 0.25998(13) 0.59931(15) 0.20050(15) 0.0125(4) Uani 1 d . . .
C25 C 0.03996(13) 0.39885(16) 0.31391(15) 0.0136(4) Uani 1 d . . .
C26 C 0.28404(16) 0.69427(16) 0.16560(18) 0.0208(5) Uani 1 d . . .
H26A H 0.2913 0.7464 0.2152 0.025 Uiso 1 calc . . R
H26B H 0.2380 0.7153 0.1052 0.025 Uiso 1 calc . . R
C27 C 0.38153(13) 0.10976(16) 0.19224(15) 0.0135(4) Uani 1 d A . .
C28 C 0.36508(16) 0.68508(17) 0.14563(19) 0.0233(5) Uani 1 d . . .
H28A H 0.3744 0.7464 0.1142 0.028 Uiso 1 calc . . R
H28B H 0.4134 0.6758 0.2075 0.028 Uiso 1 calc . . R
C29 C -0.02989(15) 0.40096(19) 0.35186(19) 0.0224(5) Uani 1 d . . .
H29A H -0.0701 0.4539 0.3181 0.027 Uiso 1 calc . . R
H29B H -0.0065 0.4171 0.4221 0.027 Uiso 1 calc . . R
C30 C 0.35746(15) 0.59672(17) 0.07936(17) 0.0191(4) Uani 1 d . . .
H30A H 0.3125 0.6095 0.0154 0.023 Uiso 1 calc . . DR
H30B H 0.4108 0.5880 0.0689 0.023 Uiso 1 calc . . R
C31 C -0.07596(16) 0.30256(19) 0.3372(2) 0.0260(5) Uani 1 d . . .
H31A H -0.1167 0.3040 0.3700 0.031 Uiso 1 calc . . R
H31B H -0.1073 0.2911 0.2669 0.031 Uiso 1 calc . . R
C32 C 0.42788(17) 0.01589(18) 0.19091(19) 0.0244(5) Uani 1 d . . .
H32A H 0.4846 0.0325 0.1925 0.029 Uiso 0.694(10) calc A 1 R
H32B H 0.3978 -0.0204 0.1297 0.029 Uiso 0.694(10) calc A 1 R
H32C H 0.4262 0.0058 0.1240 0.029 Uiso 0.306(10) calc A 2 R
H32D H 0.4874 0.0253 0.2336 0.029 Uiso 0.306(10) calc A 2 R
C34 C -0.01371(15) 0.21982(19) 0.37856(18) 0.0225(5) Uani 1 d . . .
H34A H 0.0125 0.2275 0.4500 0.027 Uiso 1 calc . . R
H34B H -0.0436 0.1554 0.3647 0.027 Uiso 1 calc . . R
C36 C 0.4359(3) -0.0498(3) 0.2759(3) 0.0226(11) Uani 0.694(10) d A 1 .
H36A H 0.4575 -0.1153 0.2658 0.027 Uiso 0.694(10) calc A 1 R
H36B H 0.4776 -0.0204 0.3355 0.027 Uiso 0.694(10) calc A 1 R
C38 C 0.3581(2) -0.06433(19) 0.2908(2) 0.0339(7) Uani 1 d . . .
H38A H 0.3708 -0.0959 0.3550 0.041 Uiso 0.694(10) calc A 1 R
H38B H 0.3225 -0.1108 0.2407 0.041 Uiso 0.694(10) calc A 1 R
H38C H 0.4021 -0.0696 0.3567 0.041 Uiso 0.306(10) calc A 2 R
H38D H 0.3197 -0.1213 0.2824 0.041 Uiso 0.306(10) calc A 2 R
Cl4 Cl 0.54271(3) 0.67669(4) 0.02295(4) 0.01858(11) Uani 1 d . . .
Cl5 Cl 0.18555(4) 0.54122(5) 0.54403(4) 0.02500(13) Uani 1 d . . .
O33 O 0.38308(17) 0.79787(19) -0.0981(2) 0.0600(8) Uani 1 d . . D
H33A H 0.3651 0.7816 -0.0539 0.090 Uiso 1 d . . G
H33B H 0.4345 0.7814 -0.0808 0.090 Uiso 1 d . . G
H6 H 0.0833(19) 0.093(2) 0.353(2) 0.028(8) Uiso 1 d . . .
H16 H 0.2374(19) -0.014(2) 0.341(2) 0.029(8) Uiso 1 d . . .
H13 H 0.3871(16) 0.410(2) 0.0729(19) 0.015(6) Uiso 1 d . . .
H9 H 0.419(2) 0.187(2) 0.115(2) 0.031(8) Uiso 1 d . . .
H11 H 0.1968(18) 0.646(2) 0.264(2) 0.019(7) Uiso 1 d . . .
O0AA O 0.41977(10) 0.99710(12) -0.07778(11) 0.0156(3) Uani 1 d . . .
H0AA H 0.4053 0.9376 -0.0947 0.023 Uiso 1 d . . G
H0AB H 0.4606 0.9974 -0.0232 0.023 Uiso 1 d . . G
O1AA O 0.2306(2) 0.7724(2) -0.0823(2) 0.0297(9) Uani 0.598(6) d B 1 D
H1AA H 0.1963 0.7241 -0.0961 0.045 Uiso 0.598(6) d B 1 DG
H1AB H 0.2158 0.8155 -0.0499 0.045 Uiso 0.598(6) d B 1 G
O1AB O 0.2240(3) 0.6957(4) -0.1391(4) 0.0333(14) Uani 0.402(6) d B 2 D
H1AC H 0.2657 0.7337 -0.1117 0.050 Uiso 0.402(6) d B 2 DG
H1AD H 0.1988 0.6845 -0.1005 0.050 Uiso 0.402(6) d B 2 DG
H8 H 0.0535(19) 0.529(2) 0.301(2) 0.024(7) Uiso 1 d . . .
C36A C 0.3980(6) -0.0741(6) 0.2209(7) 0.019(2) Uani 0.306(10) d A 2 .
H36C H 0.3576 -0.1063 0.1620 0.023 Uiso 0.306(10) calc A 2 R
H36D H 0.4462 -0.1198 0.2484 0.023 Uiso 0.306(10) calc A 2 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
Ni1 O1 2.0206(14) . ?
Ni1 O3 2.0326(14) . ?
Ni1 O5 2.2188(15) . ?
Ni1 N9 2.0052(18) . ?
Ni1 O12 2.1031(15) . ?
Ni1 N13 1.9954(17) . ?
Ni2 O1 2.0186(14) . ?
Ni2 O2 2.1634(15) . ?
Ni2 N6 1.9938(17) . ?
Ni2 O10 2.0654(14) . ?
Ni2 O14 2.1283(14) . ?
Ni2 N16 2.0035(19) . ?
Ni3 O3 2.0215(14) . ?
Ni3 O4 2.1383(15) . ?
Ni3 O7 2.1996(15) . ?
Ni3 N8 1.9931(18) . ?
Ni3 O10 2.0672(14) . ?
Ni3 N11 2.0074(18) . ?
O1 N21 1.385(2) . ?
O2 H2A 0.8523 . ?
O2 H2B 0.8509 . ?
O3 N18 1.387(2) . ?
O4 H4A 0.8524 . ?
O4 H4B 0.8498 . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8533 . ?
N6 C22 1.278(3) . ?
N6 H6 0.83(3) . ?
O7 H7A 0.8502 . ?
O7 H7B 0.8494 . ?
N8 C25 1.277(3) . ?
N8 H8 0.83(3) . ?
N9 C27 1.284(3) . ?
N9 H9 0.90(3) . ?
O10 N20 1.393(2) . ?
N11 C24 1.284(3) . ?
N11 H11 0.84(3) . ?
O12 H12A 0.8518 . ?
O12 H12B 0.8505 . ?
N13 C23 1.276(3) . ?
N13 H13 0.84(3) . ?
O14 H14A 0.8504 . ?
O14 H14B 0.8503 . ?
C15 N16 1.282(3) . ?
C15 N21 1.370(3) . ?
C15 C38 1.486(3) . ?
N16 H16 0.86(3) . ?
N18 C23 1.378(2) . ?
N18 C24 1.364(3) . ?
O19 H19A 0.8508 . ?
O19 H19B 0.8497 . ?
N20 C22 1.373(3) . ?
N20 C25 1.372(3) . ?
N21 C27 1.371(2) . ?
C22 C34 1.501(3) . ?
C23 C30 1.498(3) . ?
C24 C26 1.494(3) . ?
C25 C29 1.501(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C28 1.530(3) . ?
C27 C32 1.498(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C30 1.517(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C31 1.518(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C34 1.508(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 H32C 0.9900 . ?
C32 H32D 0.9900 . ?
C32 C36 1.503(4) . ?
C32 C36A 1.450(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C38 1.444(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 H38C 0.9900 . ?
C38 H38D 0.9900 . ?
C38 C36A 1.442(8) . ?
O33 H33A 0.8502 . ?
O33 H33B 0.8510 . ?
O0AA H0AA 0.8496 . ?
O0AA H0AB 0.8511 . ?
O1AA H1AA 0.8505 . ?
O1AA H1AB 0.8505 . ?
O1AA H1AC 1.0098 . ?
O1AA H1AD 1.2903 . ?
O1AB H1AA 1.0014 . ?
O1AB H1AC 0.8504 . ?
O1AB H1AD 0.8485 . ?
C36A H36C 0.9900 . ?
C36A H36D 0.9900 . ?

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 Ni1 O3 100.35(5) . . ?
O1 Ni1 O5 82.92(6) . . ?
O1 Ni1 O12 90.37(6) . . ?
O3 Ni1 O5 82.30(6) . . ?
O3 Ni1 O12 88.58(6) . . ?
N9 Ni1 O1 79.39(6) . . ?
N9 Ni1 O3 179.75(7) . . ?
N9 Ni1 O5 97.69(7) . . ?
N9 Ni1 O12 91.39(7) . . ?
O12 Ni1 O5 167.50(5) . . ?
N13 Ni1 O1 175.79(7) . . ?
N13 Ni1 O3 79.57(6) . . ?
N13 Ni1 O5 92.91(6) . . ?
N13 Ni1 N9 100.68(7) . . ?
N13 Ni1 O12 93.84(7) . . ?
O1 Ni2 O2 84.31(6) . . ?
O1 Ni2 O10 100.91(5) . . ?
O1 Ni2 O14 85.64(6) . . ?
N6 Ni2 O1 179.10(7) . . ?
N6 Ni2 O2 96.45(6) . . ?
N6 Ni2 O10 79.62(7) . . ?
N6 Ni2 O14 93.69(6) . . ?
N6 Ni2 N16 99.73(8) . . ?
O10 Ni2 O2 87.41(6) . . ?
O10 Ni2 O14 85.46(6) . . ?
O14 Ni2 O2 166.36(6) . . ?
N16 Ni2 O1 79.72(7) . . ?
N16 Ni2 O2 93.68(7) . . ?
N16 Ni2 O10 178.80(6) . . ?
N16 Ni2 O14 93.58(7) . . ?
O3 Ni3 O4 88.37(6) . . ?
O3 Ni3 O7 84.34(6) . . ?
O3 Ni3 O10 100.24(5) . . ?
O4 Ni3 O7 168.95(6) . . ?
N8 Ni3 O3 177.74(7) . . ?
N8 Ni3 O4 93.78(7) . . ?
N8 Ni3 O7 93.43(7) . . ?
N8 Ni3 O10 79.20(7) . . ?
N8 Ni3 N11 101.36(8) . . ?
O10 Ni3 O4 88.11(6) . . ?
O10 Ni3 O7 85.03(6) . . ?
N11 Ni3 O3 79.11(7) . . ?
N11 Ni3 O4 94.18(7) . . ?
N11 Ni3 O7 92.59(7) . . ?
N11 Ni3 O10 177.59(7) . . ?
Ni2 O1 Ni1 137.19(7) . . ?
N21 O1 Ni1 110.81(10) . . ?
N21 O1 Ni2 110.00(10) . . ?
Ni2 O2 H2A 109.4 . . ?
Ni2 O2 H2B 109.8 . . ?
H2A O2 H2B 109.4 . . ?
Ni3 O3 Ni1 137.88(7) . . ?
N18 O3 Ni1 110.34(10) . . ?
N18 O3 Ni3 109.14(11) . . ?
Ni3 O4 H4A 109.5 . . ?
Ni3 O4 H4B 109.4 . . ?
H4A O4 H4B 109.4 . . ?
Ni1 O5 H5A 109.4 . . ?
Ni1 O5 H5B 109.2 . . ?
H5A O5 H5B 109.4 . . ?
Ni2 N6 H6 131(2) . . ?
C22 N6 Ni2 115.88(15) . . ?
C22 N6 H6 112(2) . . ?
Ni3 O7 H7A 109.3 . . ?
Ni3 O7 H7B 109.5 . . ?
H7A O7 H7B 109.4 . . ?
Ni3 N8 H8 128(2) . . ?
C25 N8 Ni3 116.28(15) . . ?
C25 N8 H8 115(2) . . ?
Ni1 N9 H9 131.0(19) . . ?
C27 N9 Ni1 115.54(14) . . ?
C27 N9 H9 113.1(19) . . ?
Ni2 O10 Ni3 134.25(7) . . ?
N20 O10 Ni2 108.73(11) . . ?
N20 O10 Ni3 109.12(11) . . ?
Ni3 N11 H11 131.7(19) . . ?
C24 N11 Ni3 114.55(15) . . ?
C24 N11 H11 113.6(19) . . ?
Ni1 O12 H12A 110.0 . . ?
Ni1 O12 H12B 108.9 . . ?
H12A O12 H12B 109.3 . . ?
Ni1 N13 H13 127.3(18) . . ?
C23 N13 Ni1 116.32(13) . . ?
C23 N13 H13 116.3(18) . . ?
Ni2 O14 H14A 109.5 . . ?
Ni2 O14 H14B 109.1 . . ?
H14A O14 H14B 109.5 . . ?
N16 C15 N21 116.75(19) . . ?
N16 C15 C38 126.1(2) . . ?
N21 C15 C38 117.13(19) . . ?
Ni2 N16 H16 131(2) . . ?
C15 N16 Ni2 115.02(15) . . ?
C15 N16 H16 114(2) . . ?
C23 N18 O3 116.98(16) . . ?
C24 N18 O3 116.94(15) . . ?
C24 N18 C23 126.06(17) . . ?
H19A O19 H19B 109.4 . . ?
C22 N20 O10 117.44(16) . . ?
C25 N20 O10 116.89(16) . . ?
C25 N20 C22 125.31(17) . . ?
C15 N21 O1 116.91(16) . . ?
C15 N21 C27 125.76(18) . . ?
C27 N21 O1 116.91(16) . . ?
N6 C22 N20 117.10(18) . . ?
N6 C22 C34 125.5(2) . . ?
N20 C22 C34 117.42(19) . . ?
N13 C23 N18 116.48(18) . . ?
N13 C23 C30 126.46(18) . . ?
N18 C23 C30 117.06(18) . . ?
N11 C24 N18 116.32(18) . . ?
N11 C24 C26 125.6(2) . . ?
N18 C24 C26 118.00(18) . . ?
N8 C25 N20 117.16(18) . . ?
N8 C25 C29 124.9(2) . . ?
N20 C25 C29 117.95(19) . . ?
C24 C26 H26A 109.1 . . ?
C24 C26 H26B 109.1 . . ?
C24 C26 C28 112.64(19) . . ?
H26A C26 H26B 107.8 . . ?
C28 C26 H26A 109.1 . . ?
C28 C26 H26B 109.1 . . ?
N9 C27 N21 116.46(18) . . ?
N9 C27 C32 126.17(19) . . ?
N21 C27 C32 117.35(19) . . ?
C26 C28 H28A 109.9 . . ?
C26 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
C30 C28 C26 108.79(19) . . ?
C30 C28 H28A 109.9 . . ?
C30 C28 H28B 109.9 . . ?
C25 C29 H29A 109.2 . . ?
C25 C29 H29B 109.2 . . ?
C25 C29 C31 112.07(19) . . ?
H29A C29 H29B 107.9 . . ?
C31 C29 H29A 109.2 . . ?
C31 C29 H29B 109.2 . . ?
C23 C30 C28 111.47(18) . . ?
C23 C30 H30A 109.3 . . ?
C23 C30 H30B 109.3 . . ?
C28 C30 H30A 109.3 . . ?
C28 C30 H30B 109.3 . . ?
H30A C30 H30B 108.0 . . ?
C29 C31 H31A 109.8 . . ?
C29 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
C34 C31 C29 109.6(2) . . ?
C34 C31 H31A 109.8 . . ?
C34 C31 H31B 109.8 . . ?
C27 C32 H32A 109.3 . . ?
C27 C32 H32B 109.3 . . ?
C27 C32 H32C 108.1 . . ?
C27 C32 H32D 108.1 . . ?
C27 C32 C36 111.8(2) . . ?
H32A C32 H32B 107.9 . . ?
H32A C32 H32C 73.6 . . ?
H32A C32 H32D 35.3 . . ?
H32B C32 H32C 37.3 . . ?
H32B C32 H32D 135.4 . . ?
H32C C32 H32D 107.3 . . ?
C36 C32 H32A 109.3 . . ?
C36 C32 H32B 109.3 . . ?
C36 C32 H32C 135.8 . . ?
C36 C32 H32D 77.8 . . ?
C36A C32 C27 116.9(3) . . ?
C36A C32 H32A 129.7 . . ?
C36A C32 H32B 75.1 . . ?
C36A C32 H32C 108.1 . . ?
C36A C32 H32D 108.1 . . ?
C36A C32 C36 35.2(4) . . ?
C22 C34 C31 111.77(19) . . ?
C22 C34 H34A 109.3 . . ?
C22 C34 H34B 109.3 . . ?
C31 C34 H34A 109.3 . . ?
C31 C34 H34B 109.3 . . ?
H34A C34 H34B 107.9 . . ?
C32 C36 H36A 108.8 . . ?
C32 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
C38 C36 C32 113.9(3) . . ?
C38 C36 H36A 108.8 . . ?
C38 C36 H36B 108.8 . . ?
C15 C38 H38A 108.7 . . ?
C15 C38 H38B 108.7 . . ?
C15 C38 H38C 108.1 . . ?
C15 C38 H38D 108.1 . . ?
C36 C38 C15 114.4(2) . . ?
C36 C38 H38A 108.7 . . ?
C36 C38 H38B 108.7 . . ?
C36 C38 H38C 75.6 . . ?
C36 C38 H38D 134.2 . . ?
H38A C38 H38B 107.6 . . ?
H38A C38 H38C 37.5 . . ?
H38A C38 H38D 71.7 . . ?
H38B C38 H38C 136.6 . . ?
H38B C38 H38D 38.5 . . ?
H38C C38 H38D 107.3 . . ?
C36A C38 C15 116.9(4) . . ?
C36A C38 C36 36.1(4) . . ?
C36A C38 H38A 131.1 . . ?
C36A C38 H38B 74.3 . . ?
C36A C38 H38C 108.1 . . ?
C36A C38 H38D 108.1 . . ?
H33A O33 H33B 109.4 . . ?
H0AA O0AA H0AB 109.4 . . ?
H1AC O1AA H1AD 73.1 . . ?
H1AC O1AB H1AD 109.6 . . ?
C32 C36A H36C 108.0 . . ?
C32 C36A H36D 108.0 . . ?
C38 C36A C32 117.3(6) . . ?
C38 C36A H36C 108.0 . . ?
C38 C36A H36D 108.0 . . ?
H36C C36A H36D 107.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 N21 C15 -179.26(14) . . . . ?
Ni1 O1 N21 C27 -6.2(2) . . . . ?
Ni1 O3 N18 C23 4.5(2) . . . . ?
Ni1 O3 N18 C24 -177.20(14) . . . . ?
Ni1 N9 C27 N21 7.6(3) . . . . ?
Ni1 N9 C27 C32 -170.91(19) . . . . ?
Ni1 N13 C23 N18 -3.7(2) . . . . ?
Ni1 N13 C23 C30 176.39(17) . . . . ?
Ni2 O1 N21 C15 -12.5(2) . . . . ?
Ni2 O1 N21 C27 160.55(14) . . . . ?
Ni2 N6 C22 N20 7.2(2) . . . . ?
Ni2 N6 C22 C34 -171.36(17) . . . . ?
Ni2 O10 N20 C22 -8.9(2) . . . . ?
Ni2 O10 N20 C25 164.57(14) . . . . ?
Ni3 O3 N18 C23 -160.54(14) . . . . ?
Ni3 O3 N18 C24 17.8(2) . . . . ?
Ni3 N8 C25 N20 -5.5(3) . . . . ?
Ni3 N8 C25 C29 173.25(17) . . . . ?
Ni3 O10 N20 C22 -162.74(14) . . . . ?
Ni3 O10 N20 C25 10.7(2) . . . . ?
Ni3 N11 C24 N18 -10.2(2) . . . . ?
Ni3 N11 C24 C26 167.95(18) . . . . ?
O1 Ni1 O3 Ni3 -21.79(12) . . . . ?
O1 Ni1 O3 N18 179.55(11) . . . . ?
O1 Ni1 N9 C27 -8.50(16) . . . . ?
O1 Ni1 N13 C23 94.1(9) . . . . ?
O1 Ni2 N6 C22 117(4) . . . . ?
O1 Ni2 O10 Ni3 -25.52(11) . . . . ?
O1 Ni2 O10 N20 -169.94(11) . . . . ?
O1 Ni2 N16 C15 -8.81(16) . . . . ?
O1 N21 C27 N9 -0.7(3) . . . . ?
O1 N21 C27 C32 177.93(19) . . . . ?
O2 Ni2 O1 Ni1 77.87(11) . . . . ?
O2 Ni2 O1 N21 -83.81(12) . . . . ?
O2 Ni2 N6 C22 -95.51(16) . . . . ?
O2 Ni2 O10 Ni3 -109.22(10) . . . . ?
O2 Ni2 O10 N20 106.36(12) . . . . ?
O2 Ni2 N16 C15 74.72(17) . . . . ?
O3 Ni1 O1 Ni2 26.00(12) . . . . ?
O3 Ni1 O1 N21 -172.43(12) . . . . ?
O3 Ni1 N9 C27 -2(21) . . . . ?
O3 Ni1 N13 C23 4.77(16) . . . . ?
O3 Ni3 N8 C25 84.5(18) . . . . ?
O3 Ni3 O10 Ni2 27.86(11) . . . . ?
O3 Ni3 O10 N20 172.18(11) . . . . ?
O3 Ni3 N11 C24 15.54(15) . . . . ?
O3 N18 C23 N13 -0.7(3) . . . . ?
O3 N18 C23 C30 179.22(17) . . . . ?
O3 N18 C24 N11 -5.5(3) . . . . ?
O3 N18 C24 C26 176.13(18) . . . . ?
O4 Ni3 O3 Ni1 89.52(11) . . . . ?
O4 Ni3 O3 N18 -111.65(12) . . . . ?
O4 Ni3 N8 C25 -78.52(16) . . . . ?
O4 Ni3 O10 Ni2 -60.15(10) . . . . ?
O4 Ni3 O10 N20 84.18(12) . . . . ?
O4 Ni3 N11 C24 103.08(16) . . . . ?
O5 Ni1 O1 Ni2 -54.80(11) . . . . ?
O5 Ni1 O1 N21 106.77(12) . . . . ?
O5 Ni1 O3 Ni3 59.52(11) . . . . ?
O5 Ni1 O3 N18 -99.14(12) . . . . ?
O5 Ni1 N9 C27 -89.77(16) . . . . ?
O5 Ni1 N13 C23 86.39(16) . . . . ?
N6 Ni2 O1 Ni1 -135(4) . . . . ?
N6 Ni2 O1 N21 64(5) . . . . ?
N6 Ni2 O10 Ni3 153.74(11) . . . . ?
N6 Ni2 O10 N20 9.32(12) . . . . ?
N6 Ni2 N16 C15 171.92(16) . . . . ?
N6 C22 C34 C31 -155.3(2) . . . . ?
O7 Ni3 O3 Ni1 -82.16(11) . . . . ?
O7 Ni3 O3 N18 76.66(12) . . . . ?
O7 Ni3 N8 C25 93.10(16) . . . . ?
O7 Ni3 O10 Ni2 111.18(10) . . . . ?
O7 Ni3 O10 N20 -104.49(12) . . . . ?
O7 Ni3 N11 C24 -68.19(16) . . . . ?
N8 Ni3 O3 Ni1 -73.6(18) . . . . ?
N8 Ni3 O3 N18 85.3(18) . . . . ?
N8 Ni3 O10 Ni2 -154.36(11) . . . . ?
N8 Ni3 O10 N20 -10.04(12) . . . . ?
N8 Ni3 N11 C24 -162.21(16) . . . . ?
N8 C25 C29 C31 160.0(2) . . . . ?
N9 Ni1 O1 Ni2 -154.03(12) . . . . ?
N9 Ni1 O1 N21 7.54(12) . . . . ?
N9 Ni1 O3 Ni3 -28(21) . . . . ?
N9 Ni1 O3 N18 173(100) . . . . ?
N9 Ni1 N13 C23 -175.23(16) . . . . ?
N9 C27 C32 C36 157.7(3) . . . . ?
N9 C27 C32 C36A -163.9(5) . . . . ?
O10 Ni2 O1 Ni1 -8.38(12) . . . . ?
O10 Ni2 O1 N21 -170.05(11) . . . . ?
O10 Ni2 N6 C22 -9.35(15) . . . . ?
O10 Ni2 N16 C15 -131(3) . . . . ?
O10 Ni3 O3 Ni1 1.74(12) . . . . ?
O10 Ni3 O3 N18 160.56(11) . . . . ?
O10 Ni3 N8 C25 8.83(15) . . . . ?
O10 Ni3 N11 C24 -59.0(16) . . . . ?
O10 N20 C22 N6 1.7(3) . . . . ?
O10 N20 C22 C34 -179.68(18) . . . . ?
O10 N20 C25 N8 -4.1(3) . . . . ?
O10 N20 C25 C29 177.12(18) . . . . ?
N11 Ni3 O3 Ni1 -175.90(13) . . . . ?
N11 Ni3 O3 N18 -17.08(12) . . . . ?
N11 Ni3 N8 C25 -173.56(16) . . . . ?
N11 Ni3 O10 Ni2 101.9(15) . . . . ?
N11 Ni3 O10 N20 -113.7(15) . . . . ?
N11 C24 C26 C28 159.8(2) . . . . ?
O12 Ni1 O1 Ni2 114.62(11) . . . . ?
O12 Ni1 O1 N21 -83.81(12) . . . . ?
O12 Ni1 O3 Ni3 -111.90(11) . . . . ?
O12 Ni1 O3 N18 89.44(12) . . . . ?
O12 Ni1 N9 C27 81.61(17) . . . . ?
O12 Ni1 N13 C23 -83.08(16) . . . . ?
N13 Ni1 O1 Ni2 -62.6(9) . . . . ?
N13 Ni1 O1 N21 99.0(9) . . . . ?
N13 Ni1 O3 Ni3 153.93(13) . . . . ?
N13 Ni1 O3 N18 -4.73(12) . . . . ?
N13 Ni1 N9 C27 175.79(16) . . . . ?
N13 C23 C30 C28 -149.1(2) . . . . ?
O14 Ni2 O1 Ni1 -92.90(11) . . . . ?
O14 Ni2 O1 N21 105.43(12) . . . . ?
O14 Ni2 N6 C22 75.35(16) . . . . ?
O14 Ni2 O10 Ni3 59.14(10) . . . . ?
O14 Ni2 O10 N20 -85.28(11) . . . . ?
O14 Ni2 N16 C15 -93.72(16) . . . . ?
C15 N21 C27 N9 171.6(2) . . . . ?
C15 N21 C27 C32 -9.7(3) . . . . ?
C15 C38 C36A C32 32.6(9) . . . . ?
N16 Ni2 O1 Ni1 172.66(12) . . . . ?
N16 Ni2 O1 N21 10.99(12) . . . . ?
N16 Ni2 N6 C22 169.62(16) . . . . ?
N16 Ni2 O10 Ni3 96(3) . . . . ?
N16 Ni2 O10 N20 -48(3) . . . . ?
N16 C15 N21 O1 5.7(3) . . . . ?
N16 C15 N21 C27 -166.7(2) . . . . ?
N16 C15 C38 C36 -164.2(3) . . . . ?
N16 C15 C38 C36A 155.6(5) . . . . ?
N18 C23 C30 C28 31.0(3) . . . . ?
N18 C24 C26 C28 -22.0(3) . . . . ?
N20 C22 C34 C31 26.2(3) . . . . ?
N20 C25 C29 C31 -21.3(3) . . . . ?
N21 C15 N16 Ni2 4.5(3) . . . . ?
N21 C15 C38 C36 16.4(4) . . . . ?
N21 C15 C38 C36A -23.7(6) . . . . ?
N21 C27 C32 C36 -20.8(4) . . . . ?
N21 C27 C32 C36A 17.6(6) . . . . ?
C22 N20 C25 N8 168.8(2) . . . . ?
C22 N20 C25 C29 -10.0(3) . . . . ?
C23 N18 C24 N11 172.6(2) . . . . ?
C23 N18 C24 C26 -5.7(3) . . . . ?
C24 N18 C23 N13 -178.9(2) . . . . ?
C24 N18 C23 C30 1.1(3) . . . . ?
C24 C26 C28 C30 51.8(3) . . . . ?
C25 N20 C22 N6 -171.2(2) . . . . ?
C25 N20 C22 C34 7.4(3) . . . . ?
C25 C29 C31 C34 52.5(3) . . . . ?
C26 C28 C30 C23 -56.0(3) . . . . ?
C27 C32 C36 C38 48.5(4) . . . . ?
C27 C32 C36A C38 -29.5(9) . . . . ?
C29 C31 C34 C22 -55.0(3) . . . . ?
C32 C36 C38 C15 -46.6(5) . . . . ?
C32 C36 C38 C36A 56.3(6) . . . . ?
C36 C32 C36A C38 60.6(7) . . . . ?
C36 C38 C36A C32 -62.5(7) . . . . ?
C38 C15 N16 Ni2 -174.9(2) . . . . ?
C38 C15 N21 O1 -174.9(2) . . . . ?
C38 C15 N21 C27 12.7(3) . . . . ?
C36A C32 C36 C38 -57.7(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Vapour Deposition'
####################################################################### 
# 
# 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_zck2a
_database_code_depnum_ccdc_archive 'CCDC 1454630'
_audit_update_record             
;
2016-02-19 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H32 N8 O14 U2'
_chemical_formula_weight         1060.57

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.3529(4)
_cell_length_b                   21.2854(8)
_cell_length_c                   8.9198(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.8841(15)
_cell_angle_gamma                90
_cell_volume                     1471.61(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    568(2)
_cell_measurement_reflns_used    9696
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      28.52

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.242
_exptl_absorpt_coefficient_mu    11.068
_shelx_estimated_absorpt_T_min   0.073
_shelx_estimated_absorpt_T_max   0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3818
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62272
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.010
_diffrn_reflns_theta_max         28.572
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3673
_reflns_number_gt                3457
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0283P)²+8.3735P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3673
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.210
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.06851(2) -0.07977(2) 0.15488(2) 0.02546(7) Uani 1 1 d . . . . .
N1 N 0.3216(6) 0.0402(2) 0.1257(6) 0.0294(10) Uani 1 1 d . . . . .
N2 N 0.3769(6) -0.0469(3) 0.2757(7) 0.0382(12) Uani 1 1 d . . . . .
H2 H 0.4473 -0.0709 0.3480 0.046 Uiso 1 1 calc R U . . .
N3 N -0.2270(7) -0.1240(3) 0.0351(8) 0.0481(16) Uani 1 1 d . . . . .
H3 H -0.2446 -0.1604 0.0675 0.058 Uiso 1 1 calc R U . . .
N4 N 0.1590(8) -0.1889(3) 0.3785(8) 0.0463(14) Uani 1 1 d . . . . .
O1 O 0.0149(6) -0.0389(2) 0.3021(6) 0.0404(10) Uani 1 1 d . . . . .
O2 O 0.1252(6) -0.1227(2) 0.0136(6) 0.0411(10) Uani 1 1 d . . . . .
O3 O 0.1512(5) 0.01952(18) 0.0612(5) 0.0303(8) Uani 1 1 d . . . . .
O4 O 0.2631(7) -0.1452(3) 0.3866(7) 0.0600(15) Uani 1 1 d . . . . .
O5 O 0.0135(6) -0.1843(2) 0.2659(7) 0.0507(13) Uani 1 1 d . . . . .
O6 O 0.1978(8) -0.2327(3) 0.4727(8) 0.0714(18) Uani 1 1 d . . . . .
C1 C 0.4365(7) 0.0023(3) 0.2381(7) 0.0305(11) Uani 1 1 d . . . . .
C2 C 0.6210(8) 0.0236(4) 0.3081(9) 0.0469(17) Uani 1 1 d . . . . .
H2C H 0.6409 0.0454 0.4090 0.056 Uiso 0.5 1 calc R U P A 1
H2D H 0.6956 -0.0130 0.3321 0.056 Uiso 0.5 1 calc R U P A 1
H2A H 0.6522 0.0314 0.4227 0.056 Uiso 0.5 1 calc R U P B 2
H2B H 0.6940 -0.0101 0.2969 0.056 Uiso 0.5 1 calc R U P B 2
C3 C 0.6684(13) 0.0663(5) 0.1974(14) 0.019(2) Uiso 0.5 1 d . . P C 1
H3A H 0.6651 0.0434 0.1022 0.022 Uiso 0.5 1 calc R U P C 1
H3B H 0.7841 0.0826 0.2520 0.022 Uiso 0.5 1 calc R U P C 1
C3A C 0.656(2) 0.0809(8) 0.232(2) 0.044(4) Uiso 0.5 1 d . . P C 2
H3AA H 0.7407 0.1049 0.3175 0.052 Uiso 0.5 1 calc R U P C 2
H3AB H 0.7133 0.0671 0.1607 0.052 Uiso 0.5 1 calc R U P C 2
C4 C 0.5358(9) 0.1210(4) 0.1482(11) 0.059(2) Uani 1 1 d . . . . .
H4C H 0.5462 0.1455 0.2432 0.071 Uiso 0.5 1 calc R U P C 1
H4D H 0.5608 0.1485 0.0729 0.071 Uiso 0.5 1 calc R U P C 1
H4A H 0.5691 0.1385 0.0635 0.071 Uiso 0.5 1 calc R U P C 2
H4B H 0.5348 0.1554 0.2193 0.071 Uiso 0.5 1 calc R U P C 2
C5 C 0.3543(8) 0.0964(3) 0.0710(8) 0.0365(13) Uani 1 1 d . . . . .
O7 O 0.3450(14) 0.1272(5) 0.4932(13) 0.049(2) Uiso 0.5 1 d . . P D 1
C6 C 0.365(3) 0.1974(11) 0.521(3) 0.081(6) Uiso 0.5 1 d . . P D 1
H6A H 0.3727 0.2073 0.6294 0.097 Uiso 0.5 1 calc R U P D 1
H6B H 0.4709 0.2115 0.5098 0.097 Uiso 0.5 1 calc R U P D 1
C7 C 0.246(4) 0.2233(16) 0.426(4) 0.111(10) Uiso 0.5 1 d . . P D 1
H7A H 0.2851 0.2503 0.3586 0.133 Uiso 0.5 1 calc R U P D 1
H7B H 0.1909 0.2494 0.4816 0.133 Uiso 0.5 1 calc R U P D 1
C8 C 0.133(4) 0.1812(15) 0.333(4) 0.090(9) Uiso 0.5 1 d . . P D 1
H8A H 0.1321 0.1829 0.2243 0.108 Uiso 0.5 1 calc R U P D 1
H8B H 0.0185 0.1914 0.3290 0.108 Uiso 0.5 1 calc R U P D 1
C9 C 0.177(3) 0.1220(10) 0.394(3) 0.058(5) Uiso 0.5 1 d . . P D 1
H9A H 0.1063 0.1088 0.4539 0.070 Uiso 0.5 1 calc R U P D 1
H9B H 0.1626 0.0920 0.3082 0.070 Uiso 0.5 1 calc R U P D 1
O7A O 0.3146(18) 0.1275(7) 0.5794(17) 0.071(3) Uiso 0.5 1 d . . P E 2
C6A C 0.346(3) 0.1889(9) 0.608(2) 0.065(4) Uiso 0.5 1 d . . P E 2
H6AA H 0.4588 0.1991 0.6076 0.077 Uiso 0.5 1 calc R U P E 2
H6AB H 0.3437 0.1996 0.7126 0.077 Uiso 0.5 1 calc R U P E 2
C7A C 0.209(3) 0.2261(9) 0.477(2) 0.059(4) Uiso 0.5 1 d . . P E 2
H7AA H 0.1429 0.2513 0.5245 0.071 Uiso 0.5 1 calc R U P E 2
H7AB H 0.2625 0.2540 0.4238 0.071 Uiso 0.5 1 calc R U P E 2
C8A C 0.093(3) 0.1806(10) 0.358(3) 0.058(5) Uiso 0.5 1 d . . P E 2
H8AA H -0.0269 0.1863 0.3458 0.069 Uiso 0.5 1 calc R U P E 2
H8AB H 0.1019 0.1845 0.2532 0.069 Uiso 0.5 1 calc R U P E 2
C9A C 0.162(2) 0.1188(9) 0.436(2) 0.045(4) Uiso 0.5 1 d . . P E 2
H9AA H 0.0739 0.0975 0.4636 0.055 Uiso 0.5 1 calc R U P E 2
H9AB H 0.1890 0.0926 0.3594 0.055 Uiso 0.5 1 calc R U P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.759(4) . ?
U1 O1 1.766(4) . ?
U1 O3 2.464(4) . ?
U1 O3 2.468(4) 3 ?
U1 N3 2.480(5) . ?
U1 N2 2.493(5) . ?
U1 O4 2.519(5) . ?
U1 O5 2.546(5) . ?
U1 N4 2.970(5) . ?
N1 C5 1.358(8) . ?
N1 C1 1.363(7) . ?
N1 O3 1.393(5) . ?
N2 C1 1.259(8) . ?
N3 C5 1.273(8) 3 ?
N4 O6 1.216(7) . ?
N4 O4 1.256(8) . ?
N4 O5 1.259(8) . ?
O3 U1 2.468(4) 3 ?
C1 C2 1.501(8) . ?
C2 C3A 1.479(17) . ?
C2 C3 1.500(13) . ?
C3 C4 1.554(14) . ?
C3A C4 1.318(18) . ?
C4 C5 1.507(8) . ?
C5 N3 1.273(8) 3 ?
O7 C9 1.36(2) . ?
O7 C6 1.51(2) . ?
C6 C7 1.18(4) . ?
C7 C8 1.34(4) . ?
C8 C9 1.37(4) . ?
O7A C6A 1.34(2) . ?
O7A C9A 1.45(2) . ?
C6A C7A 1.52(3) . ?
C7A C8A 1.50(3) . ?
C8A C9A 1.50(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
O2 U1 O1 177.9(2) . . ?
O2 U1 O3 91.07(18) . . ?
O1 U1 O3 90.59(18) . . ?
O2 U1 O3 91.76(19) . 3 ?
O1 U1 O3 90.23(19) . 3 ?
O3 U1 O3 60.67(14) . 3 ?
O2 U1 N3 89.1(2) . . ?
O1 U1 N3 91.1(2) . . ?
O3 U1 N3 122.61(15) . . ?
O3 U1 N3 61.96(15) 3 . ?
O2 U1 N2 86.8(2) . . ?
O1 U1 N2 92.7(2) . . ?
O3 U1 N2 62.04(15) . . ?
O3 U1 N2 122.65(14) 3 . ?
N3 U1 N2 173.94(19) . . ?
O2 U1 O4 92.1(2) . . ?
O1 U1 O4 85.8(2) . . ?
O3 U1 O4 125.14(15) . . ?
O3 U1 O4 172.93(16) 3 . ?
N3 U1 O4 112.19(18) . . ?
N2 U1 O4 63.50(17) . . ?
O2 U1 O5 87.7(2) . . ?
O1 U1 O5 90.5(2) . . ?
O3 U1 O5 174.57(14) . . ?
O3 U1 O5 124.64(14) 3 . ?
N3 U1 O5 62.68(17) . . ?
N2 U1 O5 112.60(16) . . ?
O4 U1 O5 49.66(17) . . ?
O2 U1 N4 90.3(2) . . ?
O1 U1 N4 87.6(2) . . ?
O3 U1 N4 149.90(15) . . ?
O3 U1 N4 149.32(15) 3 . ?
N3 U1 N4 87.48(17) . . ?
N2 U1 N4 88.03(17) . . ?
O4 U1 N4 24.76(17) . . ?
O5 U1 N4 24.91(16) . . ?
C5 N1 C1 127.1(5) . . ?
C5 N1 O3 116.2(4) . . ?
C1 N1 O3 116.7(4) . . ?
C1 N2 U1 124.5(4) . . ?
C5 N3 U1 124.5(4) 3 . ?
O6 N4 O4 121.8(6) . . ?
O6 N4 O5 122.7(6) . . ?
O4 N4 O5 115.5(5) . . ?
O6 N4 U1 178.6(6) . . ?
O4 N4 U1 57.1(3) . . ?
O5 N4 U1 58.3(3) . . ?
N1 O3 U1 120.2(3) . . ?
N1 O3 U1 120.4(3) . 3 ?
U1 O3 U1 119.33(14) . 3 ?
N4 O4 U1 98.1(4) . . ?
N4 O5 U1 96.7(4) . . ?
N2 C1 N1 116.6(5) . . ?
N2 C1 C2 126.0(6) . . ?
N1 C1 C2 117.4(5) . . ?
C3A C2 C1 114.0(8) . . ?
C3 C2 C1 113.0(6) . . ?
C2 C3 C4 107.8(8) . . ?
C4 C3A C2 123.6(13) . . ?
C3A C4 C5 117.3(9) . . ?
C5 C4 C3 110.9(7) . . ?
N3 C5 N1 116.7(5) 3 . ?
N3 C5 C4 126.8(6) 3 . ?
N1 C5 C4 116.5(6) . . ?
C9 O7 C6 102.3(15) . . ?
C7 C6 O7 109(2) . . ?
C6 C7 C8 110(3) . . ?
C7 C8 C9 111(3) . . ?
O7 C9 C8 104(2) . . ?
C6A O7A C9A 109.7(15) . . ?
O7A C6A C7A 109.2(16) . . ?
C8A C7A C6A 108.1(17) . . ?
C9A C8A C7A 101.8(17) . . ?
O7A C9A C8A 111.0(16) . . ?

_refine_diff_density_max         0.961
_refine_diff_density_min         -2.657
_refine_diff_density_rms         0.187


_exptl_crystal_recrystallization_method 'Vapour Deposition'
