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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1401604'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C53 H76 N12 Ni2 O12,17(H2 O)'
_chemical_formula_sum            'C53 H110 N12 Ni2 O29'
_chemical_formula_weight         1496.94

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   37.526(8)
_cell_length_b                   8.8468(18)
_cell_length_c                   29.720(6)
_cell_angle_alpha                90
_cell_angle_beta                 127.61(3)
_cell_angle_gamma                90
_cell_volume                     7816(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    12734
_cell_measurement_theta_min      2.4020
_cell_measurement_theta_max      31.4816

_exptl_crystal_description       Prism
_exptl_crystal_colour            Violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_F_000             3200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4700
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1400
_exptl_absorpt_coefficient_mu    0.563
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            27283
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.407
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6861
_reflns_number_gt                6161
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_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)+(0.1057P)²+21.0245P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6861
_refine_ls_number_parameters     452
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1966
_refine_ls_wR_factor_gt          0.1905
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.170
_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
O6W O 0.34748(16) 0.3690(5) 0.93730(18) 0.0750(12) Uani 1 1 d . . . . .
Ni1 Ni 0.2500 1.7500 0.0000 0.0234(2) Uani 1 2 d S . P . .
Ni2 Ni 0.5000 0.0000 0.0000 0.0234(2) Uani 1 2 d S . P . .
N2 N 0.25887(11) 1.7609(4) -0.06196(13) 0.0306(7) Uani 1 1 d . . . . .
H2N H 0.2796 1.6797 -0.0546 0.037 Uiso 1 1 calc R U . . .
N1 N 0.20350(11) 1.5772(4) -0.03946(14) 0.0359(8) Uani 1 1 d . . . . .
H1N H 0.2198 1.4820 -0.0312 0.043 Uiso 1 1 calc R U . . .
N3 N 0.19239(12) 1.6044(4) -0.12945(14) 0.0411(9) Uani 1 1 d . . . . .
C13 C 0.21710(14) 1.7413(5) -0.12054(17) 0.0376(10) Uani 1 1 d . . . . .
H13A H 0.1976 1.8274 -0.1301 0.045 Uiso 1 1 calc R U . . .
H13B H 0.2247 1.7412 -0.1464 0.045 Uiso 1 1 calc R U . . .
C11 C 0.17129(15) 1.5950(6) -0.10197(18) 0.0453(11) Uani 1 1 d . . . . .
H11A H 0.1507 1.5099 -0.1177 0.054 Uiso 1 1 calc R U . . .
H11B H 0.1537 1.6859 -0.1106 0.054 Uiso 1 1 calc R U . . .
C14 C 0.28185(16) 1.9067(5) -0.05300(19) 0.0432(10) Uani 1 1 d . . . . .
H14A H 0.2604 1.9892 -0.0678 0.052 Uiso 1 1 calc R U . . .
H14B H 0.2951 1.9062 -0.0726 0.052 Uiso 1 1 calc R U . . .
C10 C 0.18154(16) 1.5732(6) -0.0108(2) 0.0476(11) Uani 1 1 d . . . . .
H10A H 0.1663 1.4774 -0.0183 0.057 Uiso 1 1 calc R U . . .
H10B H 0.1595 1.6537 -0.0253 0.057 Uiso 1 1 calc R U . . .
C12 C 0.21569(19) 1.4648(6) -0.1250(2) 0.0586(14) Uani 1 1 d . . . . .
H12A H 0.2408 1.4474 -0.0860 0.088 Uiso 1 1 calc R U . . .
H12B H 0.2263 1.4749 -0.1472 0.088 Uiso 1 1 calc R U . . .
H12C H 0.1952 1.3811 -0.1390 0.088 Uiso 1 1 calc R U . . .
N4 N 0.56865(11) -0.0317(4) 0.04884(13) 0.0294(7) Uani 1 1 d . . . . .
H5N H 0.5829 0.0568 0.0736 0.035 Uiso 1 1 calc R U . . .
N5 N 0.49785(11) 0.1423(4) -0.05659(13) 0.0328(7) Uani 1 1 d . . . . .
H4N H 0.5074 0.2429 -0.0392 0.039 Uiso 1 1 calc R U . . .
N6 N 0.57524(13) 0.0808(4) -0.02152(16) 0.0417(9) Uani 1 1 d . . . . .
C23 C 0.44976(15) 0.1523(5) -0.10652(18) 0.0423(10) Uani 1 1 d . . . . .
H23A H 0.4412 0.0633 -0.1302 0.051 Uiso 1 1 calc R U . . .
H23B H 0.4449 0.2405 -0.1290 0.051 Uiso 1 1 calc R U . . .
C24 C 0.52873(16) 0.0947(5) -0.07020(18) 0.0424(10) Uani 1 1 d . . . . .
H24A H 0.5185 -0.0018 -0.0897 0.051 Uiso 1 1 calc R U . . .
H24B H 0.5265 0.1679 -0.0961 0.051 Uiso 1 1 calc R U . . .
C27 C 0.57849(15) -0.1635(5) 0.08578(19) 0.0415(10) Uani 1 1 d . . . . .
H27A H 0.6102 -0.1647 0.1180 0.050 Uiso 1 1 calc R U . . .
H27B H 0.5715 -0.2565 0.0646 0.050 Uiso 1 1 calc R U . . .
C26 C 0.58657(15) -0.0449(5) 0.0158(2) 0.0413(10) Uani 1 1 d . . . . .
H26A H 0.6191 -0.0539 0.0422 0.050 Uiso 1 1 calc R U . . .
H26B H 0.5749 -0.1368 -0.0066 0.050 Uiso 1 1 calc R U . . .
C25 C 0.59670(17) 0.2241(6) 0.0067(2) 0.0521(12) Uani 1 1 d . . . . .
H25A H 0.5824 0.2661 0.0218 0.078 Uiso 1 1 calc R U . . .
H25B H 0.5938 0.2933 -0.0203 0.078 Uiso 1 1 calc R U . . .
H25C H 0.6280 0.2072 0.0370 0.078 Uiso 1 1 calc R U . . .
O2 O 0.49527(9) 0.6881(3) 0.19101(12) 0.0326(6) Uani 1 1 d . . . . .
C1 C 0.5000 0.8792(5) 0.2500 0.0195(9) Uani 1 2 d S T P . .
C15 C 0.52778(12) 0.7784(4) 0.23971(15) 0.0233(7) Uani 1 1 d . . . . .
H15A H 0.5451 0.8394 0.2322 0.028 Uiso 1 1 calc R U . . .
H15B H 0.5482 0.7148 0.2725 0.028 Uiso 1 1 calc R U . . .
O5 O 0.50766(9) 0.1943(3) 0.04795(11) 0.0348(6) Uani 1 1 d . . . . .
O6 O 0.58124(9) 0.2372(3) 0.11302(12) 0.0341(6) Uani 1 1 d . . . . .
O4 O 0.30148(9) 1.5836(3) 0.04808(11) 0.0351(6) Uani 1 1 d . . . . .
C19 C 0.52963(13) 0.3729(4) 0.11982(16) 0.0291(8) Uani 1 1 d . . . . .
C2 C 0.46914(12) 0.9781(4) 0.19741(14) 0.0222(7) Uani 1 1 d . . . . .
H2A H 0.4868 1.0346 0.1894 0.027 Uiso 1 1 calc R U . . .
H2B H 0.4480 0.9152 0.1648 0.027 Uiso 1 1 calc R U . . .
C3 C 0.41771(12) 1.1839(4) 0.16621(15) 0.0246(7) Uani 1 1 d . . . . .
C5 C 0.38174(13) 1.2989(4) 0.07464(16) 0.0295(8) Uani 1 1 d . . . . .
H5 H 0.3778 1.3054 0.0406 0.035 Uiso 1 1 calc R U . . .
C6 C 0.35793(12) 1.3968(4) 0.08410(16) 0.0277(8) Uani 1 1 d . . . . .
C20 C 0.56357(13) 0.4420(4) 0.17067(16) 0.0288(8) Uani 1 1 d . . . . .
H20 H 0.5934 0.4168 0.1877 0.035 Uiso 1 1 calc R U . . .
C16 C 0.50953(13) 0.5833(4) 0.17138(16) 0.0277(8) Uani 1 1 d . . . . .
C21 C 0.55414(13) 0.5482(4) 0.19684(16) 0.0277(8) Uani 1 1 d . . . . .
H21 H 0.5773 0.5945 0.2306 0.033 Uiso 1 1 calc R U . . .
C4 C 0.41126(12) 1.1918(4) 0.11455(15) 0.0256(7) Uani 1 1 d . . . . .
H4 H 0.4265 1.1264 0.1071 0.031 Uiso 1 1 calc R U . . .
C22 C 0.54024(14) 0.2604(4) 0.09120(17) 0.0306(8) Uani 1 1 d . . . . .
O3 O 0.32640(12) 1.5310(4) -0.00190(14) 0.0582(10) Uani 1 1 d . . . . .
C8 C 0.39452(14) 1.2814(5) 0.17649(17) 0.0335(9) Uani 1 1 d . . . . .
H8 H 0.3990 1.2767 0.2109 0.040 Uiso 1 1 calc R U . . .
C7 C 0.36479(14) 1.3853(5) 0.13595(17) 0.0345(9) Uani 1 1 d . . . . .
H7 H 0.3490 1.4488 0.1431 0.041 Uiso 1 1 calc R U . . .
C18 C 0.48518(14) 0.4101(5) 0.09538(19) 0.0402(10) Uani 1 1 d . . . . .
H18 H 0.4620 0.3643 0.0615 0.048 Uiso 1 1 calc R U . . .
C9 C 0.32596(13) 1.5112(4) 0.03972(17) 0.0325(9) Uani 1 1 d . . . . .
C17 C 0.47499(14) 0.5133(5) 0.1204(2) 0.0414(11) Uani 1 1 d . . . . .
H17 H 0.4451 0.5368 0.1036 0.050 Uiso 1 1 calc R U . . .
O1 O 0.44539(9) 1.0797(3) 0.20785(10) 0.0287(6) Uani 1 1 d . . . . .
O1W O 0.62582(12) 0.8666(4) 0.25019(14) 0.0623(10) Uani 1 1 d . . . . .
H2W H 0.6414 0.8708 0.2853 0.093 Uiso 1 1 d R U . . .
H1W H 0.6287 0.9478 0.2391 0.093 Uiso 1 1 d R U . . .
O2W O 0.63794(17) 0.4730(5) 0.13168(19) 0.0817(14) Uani 1 1 d . . . . .
H3W H 0.6129 0.4304 0.1177 0.123 Uiso 1 1 d R U . . .
H4W H 0.6562 0.4478 0.1656 0.123 Uiso 1 1 d R U . . .
O4W O 0.64666(12) 0.1325(4) 0.22091(16) 0.0616(10) Uani 1 1 d . . . . .
H7W H 0.6570 0.1189 0.2024 0.092 Uiso 1 1 d R U . . .
H8W H 0.6291 0.1788 0.1895 0.092 Uiso 1 1 d R U . . .
O8W O 0.7199(4) 0.3314(18) 0.1719(6) 0.147(6) Uani 0.5 1 d . . P . .
O7W O 0.71760(17) 0.8224(7) 0.1464(2) 0.1071(18) Uani 1 1 d . . . . .
H14W H 0.7131 0.9161 0.1472 0.161 Uiso 1 1 d R U . . .
H13W H 0.7097 0.8069 0.1131 0.161 Uiso 1 1 d R U . . .
O5W O 0.66416(15) 0.6391(4) 0.22827(16) 0.0721(11) Uani 1 1 d . . . . .
H9W H 0.6651 0.7034 0.2502 0.108 Uiso 1 1 d R U . . .
H10W H 0.6727 0.5546 0.2454 0.108 Uiso 1 1 d R U . . .
O3W O 0.69066(14) 0.3816(5) 0.29818(17) 0.0682(10) Uani 1 1 d . . . . .
H6W H 0.7185 0.3618 0.3170 0.102 Uiso 1 1 d R U . . .
H5W H 0.6777 0.3069 0.2752 0.102 Uiso 1 1 d R U . . .
O10W O 0.2510(9) 0.258(3) 0.0209(10) 0.202(8) Uani 0.5 1 d . . P . .
H11W H 0.3356 0.4306 0.9099 0.303 Uiso 1 1 d R U . . .
H12W H 0.3415 0.4118 0.9585 0.303 Uiso 1 1 d R U . . .
O9W O 0.7079(4) -0.002(2) 0.2106(8) 0.218(8) Uani 0.5 1 d . U 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
Ni1 N1 2.064(3) . ?
Ni1 N1 2.064(3) 7_585 ?
Ni1 N2 2.064(3) . ?
Ni1 N2 2.064(3) 7_585 ?
Ni1 O4 2.138(3) . ?
Ni1 O4 2.138(3) 7_585 ?
Ni2 N5 2.063(3) 5_655 ?
Ni2 N5 2.063(3) . ?
Ni2 N4 2.063(3) . ?
Ni2 N4 2.064(3) 5_655 ?
Ni2 O5 2.137(3) 5_655 ?
Ni2 O5 2.137(3) . ?
N2 C13 1.479(5) . ?
N2 C14 1.482(5) . ?
N1 C11 1.482(5) . ?
N1 C10 1.503(5) . ?
N3 C11 1.446(6) . ?
N3 C13 1.448(6) . ?
N3 C12 1.472(6) . ?
C14 C10 1.529(7) 7_585 ?
C10 C14 1.529(7) 7_585 ?
N4 C27 1.485(5) . ?
N4 C26 1.495(5) . ?
N5 C23 1.483(6) . ?
N5 C24 1.502(5) . ?
N6 C26 1.439(6) . ?
N6 C24 1.440(6) . ?
N6 C25 1.461(6) . ?
C23 C27 1.520(7) 5_655 ?
C27 C23 1.520(6) 5_655 ?
O2 C16 1.367(4) . ?
O2 C15 1.437(4) . ?
C1 C2 1.530(4) 2_655 ?
C1 C2 1.530(4) . ?
C1 C15 1.538(4) . ?
C1 C15 1.538(4) 2_655 ?
O5 C22 1.254(5) . ?
O6 C22 1.270(5) . ?
O4 C9 1.263(5) . ?
C19 C20 1.389(5) . ?
C19 C18 1.393(6) . ?
C19 C22 1.512(5) . ?
C2 O1 1.427(4) . ?
C3 O1 1.375(4) . ?
C3 C8 1.385(5) . ?
C3 C4 1.403(5) . ?
C5 C4 1.388(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.402(5) . ?
C6 C9 1.507(5) . ?
C20 C21 1.396(5) . ?
C16 C21 1.387(5) . ?
C16 C17 1.400(6) . ?
O3 C9 1.259(5) . ?
C8 C7 1.379(6) . ?
C18 C17 1.372(6) . ?
O10W O10W 1.21(3) 7 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 . 7_585 ?
N1 Ni1 N2 93.93(14) . . ?
N1 Ni1 N2 86.07(14) 7_585 . ?
N1 Ni1 N2 86.07(14) . 7_585 ?
N1 Ni1 N2 93.93(14) 7_585 7_585 ?
N2 Ni1 N2 180.0 . 7_585 ?
N1 Ni1 O4 88.60(13) . . ?
N1 Ni1 O4 91.39(13) 7_585 . ?
N2 Ni1 O4 93.25(11) . . ?
N2 Ni1 O4 86.75(11) 7_585 . ?
N1 Ni1 O4 91.39(13) . 7_585 ?
N1 Ni1 O4 88.61(13) 7_585 7_585 ?
N2 Ni1 O4 86.75(11) . 7_585 ?
N2 Ni1 O4 93.25(11) 7_585 7_585 ?
O4 Ni1 O4 180.00(16) . 7_585 ?
N5 Ni2 N5 180.0 5_655 . ?
N5 Ni2 N4 86.14(13) 5_655 . ?
N5 Ni2 N4 93.86(13) . . ?
N5 Ni2 N4 93.86(13) 5_655 5_655 ?
N5 Ni2 N4 86.14(13) . 5_655 ?
N4 Ni2 N4 180.0(2) . 5_655 ?
N5 Ni2 O5 88.58(12) 5_655 5_655 ?
N5 Ni2 O5 91.42(12) . 5_655 ?
N4 Ni2 O5 87.82(12) . 5_655 ?
N4 Ni2 O5 92.18(12) 5_655 5_655 ?
N5 Ni2 O5 91.42(12) 5_655 . ?
N5 Ni2 O5 88.58(12) . . ?
N4 Ni2 O5 92.18(12) . . ?
N4 Ni2 O5 87.82(12) 5_655 . ?
O5 Ni2 O5 180.00(18) 5_655 . ?
C13 N2 C14 113.4(3) . . ?
C13 N2 Ni1 114.4(2) . . ?
C14 N2 Ni1 105.9(2) . . ?
C11 N1 C10 113.7(3) . . ?
C11 N1 Ni1 113.2(3) . . ?
C10 N1 Ni1 105.1(3) . . ?
C11 N3 C13 117.1(3) . . ?
C11 N3 C12 113.7(4) . . ?
C13 N3 C12 114.0(4) . . ?
N3 C13 N2 114.5(3) . . ?
N3 C11 N1 113.9(4) . . ?
N2 C14 C10 107.9(3) . 7_585 ?
N1 C10 C14 108.2(3) . 7_585 ?
C27 N4 C26 114.5(3) . . ?
C27 N4 Ni2 105.5(2) . . ?
C26 N4 Ni2 114.7(3) . . ?
C23 N5 C24 114.5(3) . . ?
C23 N5 Ni2 105.7(2) . . ?
C24 N5 Ni2 113.3(3) . . ?
C26 N6 C24 116.6(4) . . ?
C26 N6 C25 115.4(4) . . ?
C24 N6 C25 114.1(4) . . ?
N5 C23 C27 108.8(3) . 5_655 ?
N6 C24 N5 114.5(3) . . ?
N4 C27 C23 109.1(3) . 5_655 ?
N6 C26 N4 114.0(3) . . ?
C16 O2 C15 119.6(3) . . ?
C2 C1 C2 110.2(4) 2_655 . ?
C2 C1 C15 110.65(18) 2_655 . ?
C2 C1 C15 108.11(18) . . ?
C2 C1 C15 108.12(18) 2_655 2_655 ?
C2 C1 C15 110.65(18) . 2_655 ?
C15 C1 C15 109.1(4) . 2_655 ?
O2 C15 C1 105.1(2) . . ?
C22 O5 Ni2 135.2(3) . . ?
C9 O4 Ni1 133.4(2) . . ?
C20 C19 C18 118.3(3) . . ?
C20 C19 C22 121.3(3) . . ?
C18 C19 C22 120.3(4) . . ?
O1 C2 C1 108.8(2) . . ?
O1 C3 C8 116.7(3) . . ?
O1 C3 C4 123.4(3) . . ?
C8 C3 C4 119.9(3) . . ?
C4 C5 C6 121.9(3) . . ?
C5 C6 C7 117.9(3) . . ?
C5 C6 C9 120.5(3) . . ?
C7 C6 C9 121.6(3) . . ?
C19 C20 C21 121.8(4) . . ?
O2 C16 C21 125.1(3) . . ?
O2 C16 C17 114.6(3) . . ?
C21 C16 C17 120.3(3) . . ?
C16 C21 C20 118.6(3) . . ?
C5 C4 C3 119.0(3) . . ?
O5 C22 O6 124.6(3) . . ?
O5 C22 C19 117.2(3) . . ?
O6 C22 C19 118.2(3) . . ?
C7 C8 C3 120.3(4) . . ?
C8 C7 C6 121.1(4) . . ?
C17 C18 C19 121.1(4) . . ?
O3 C9 O4 124.7(4) . . ?
O3 C9 C6 118.2(3) . . ?
O4 C9 C6 117.1(3) . . ?
C18 C17 C16 120.0(4) . . ?
C3 O1 C2 117.1(3) . . ?

_refine_diff_density_max         1.467
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.103
# start Validation Reply Form

_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact  O10W   ..  O10W    ..       1.21 Ang.  
RESPONSE: Due to the disorder of O10w, the occupancies of O10wis set to be 0.5,
and thus the short contact should be acceptable.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1401605'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C57 H76 N12 Ni2 O12,17(H2 O)'
_chemical_formula_sum            'C57 H110 N12 Ni2 O29'
_chemical_formula_weight         1544.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   37.153(3)
_cell_length_b                   8.9381(8)
_cell_length_c                   29.414(3)
_cell_angle_alpha                90
_cell_angle_beta                 127.964(2)
_cell_angle_gamma                90
_cell_volume                     7700.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1984
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      23.50

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             3296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.574
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6637
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19425
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.390
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7729
_reflns_number_gt                4746
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_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)+(0.1124P)²+2.3333P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7729
_refine_ls_number_parameters     468
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.2088
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.008
_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
Ni1 Ni 0.0000 1.0000 0.0000 0.0196(2) Uani 1 2 d S . P . .
Ni2 Ni 0.2500 -0.7500 0.5000 0.0177(2) Uani 1 2 d S . P . .
O6 O 0.19939(10) -0.5773(3) 0.45408(12) 0.0229(7) Uani 1 1 d . . . . .
O5 O 0.17308(12) -0.5313(4) 0.50336(14) 0.0342(9) Uani 1 1 d . . . . .
O4 O 0.05683(10) -0.0715(3) 0.29470(12) 0.0231(7) Uani 1 1 d . . . . .
O1 O -0.00309(10) 0.3196(3) 0.19460(12) 0.0242(7) Uani 1 1 d . . . . .
O3 O 0.08402(11) 0.7727(4) 0.11962(14) 0.0320(8) Uani 1 1 d . . . . .
O2 O 0.01006(11) 0.8236(3) 0.05682(13) 0.0274(8) Uani 1 1 d . . . . .
N2 N 0.24105(12) -0.7632(4) 0.56145(14) 0.0216(8) Uani 1 1 d . . . . .
H2 H 0.2195 -0.6840 0.5529 0.026 Uiso 1 1 calc R U . . .
N1 N 0.19766(12) -0.9104(4) 0.45422(15) 0.0237(9) Uani 1 1 d . . . . .
N3 N 0.18819(13) -0.8824(5) 0.36933(16) 0.0313(10) Uani 1 1 d . . . . .
N4 N -0.00582(14) 0.8449(4) -0.05767(15) 0.0261(9) Uani 1 1 d . . . . .
N6 N 0.06819(13) 1.0234(4) 0.04391(16) 0.0257(9) Uani 1 1 d . . . . .
H6N H 0.0829 0.9440 0.0731 0.031 Uiso 1 1 calc R U . . .
N5 N 0.06642(15) 0.8883(5) -0.03136(17) 0.0329(10) Uani 1 1 d . . . . .
C25 C 0.01827(17) 0.9037(6) -0.0795(2) 0.0302(11) Uani 1 1 d . . . . .
H25A H 0.0105 0.8461 -0.1124 0.036 Uiso 1 1 calc R U . . .
H25B H 0.0104 1.0077 -0.0908 0.036 Uiso 1 1 calc R U . . .
C27 C 0.06836(19) 0.7400(6) -0.0072(2) 0.0400(13) Uani 1 1 d . . . . .
H27A H 0.0882 0.7441 0.0346 0.048 Uiso 1 1 calc R U . . .
H27B H 0.0800 0.6648 -0.0190 0.048 Uiso 1 1 calc R U . . .
C26 C 0.01870(18) 0.7017(5) -0.0313(2) 0.0325(12) Uani 1 1 d . . . . .
H26A H 0.0061 0.6226 -0.0598 0.039 Uiso 1 1 calc R U . . .
H26B H 0.0174 0.6715 -0.0006 0.039 Uiso 1 1 calc R U . . .
C29 C 0.08564(17) 1.0098(6) 0.0098(2) 0.0334(12) Uani 1 1 d . . . . .
H29A H 0.0795 1.1029 -0.0108 0.040 Uiso 1 1 calc R U . . .
H29B H 0.1185 0.9971 0.0364 0.040 Uiso 1 1 calc R U . . .
C28 C 0.07996(17) 1.1676(6) 0.0755(2) 0.0326(12) Uani 1 1 d . . . . .
H28A H 0.0702 1.2509 0.0492 0.039 Uiso 1 1 calc R U . . .
H28B H 0.1127 1.1747 0.1053 0.039 Uiso 1 1 calc R U . . .
C24 C -0.05580(17) 0.8272(6) -0.1024(2) 0.0321(12) Uani 1 1 d . . . . .
H24A H -0.0621 0.7324 -0.1221 0.039 Uiso 1 1 calc R U . . .
H24B H -0.0673 0.9066 -0.1307 0.039 Uiso 1 1 calc R U . . .
C14 C 0.16426(16) -0.8595(6) 0.39376(19) 0.0296(11) Uani 1 1 d . . . . .
H14A H 0.1365 -0.9186 0.3735 0.036 Uiso 1 1 calc R U . . .
H14B H 0.1566 -0.7549 0.3921 0.036 Uiso 1 1 calc R U . . .
C16 C 0.21074(17) -1.0563(5) 0.4441(2) 0.0309(12) Uani 1 1 d . . . . .
H16A H 0.1886 -1.1330 0.4345 0.037 Uiso 1 1 calc R U . . .
H16B H 0.2406 -1.0877 0.4780 0.037 Uiso 1 1 calc R U . . .
C15 C 0.21150(18) -1.0278(5) 0.3940(2) 0.0332(12) Uani 1 1 d . . . . .
H15A H 0.2427 -1.0231 0.4072 0.040 Uiso 1 1 calc R U . . .
H15B H 0.1955 -1.1067 0.3655 0.040 Uiso 1 1 calc R U . . .
C11 C 0.28215(16) -0.7414(6) 0.62209(18) 0.0292(11) Uani 1 1 d . . . . .
H11A H 0.2724 -0.7232 0.6456 0.035 Uiso 1 1 calc R U . . .
H11B H 0.2998 -0.8332 0.6357 0.035 Uiso 1 1 calc R U . . .
C12 C 0.21744(17) -0.9069(5) 0.5508(2) 0.0289(11) Uani 1 1 d . . . . .
H12A H 0.2053 -0.9106 0.5720 0.035 Uiso 1 1 calc R U . . .
H12B H 0.2387 -0.9893 0.5635 0.035 Uiso 1 1 calc R U . . .
C13 C 0.17906(17) -0.9198(6) 0.4869(2) 0.0326(12) Uani 1 1 d . . . . .
H13A H 0.1634 -1.0145 0.4788 0.039 Uiso 1 1 calc R U . . .
H13B H 0.1572 -0.8399 0.4747 0.039 Uiso 1 1 calc R U . . .
C10 C 0.17389(15) -0.5093(5) 0.46209(19) 0.0227(10) Uani 1 1 d . . . . .
C7 C 0.14194(14) -0.3947(5) 0.41726(17) 0.0196(9) Uani 1 1 d . . . . .
C6 C 0.13502(15) -0.3817(5) 0.36513(18) 0.0246(10) Uani 1 1 d . . . . .
H6 H 0.1504 -0.4462 0.3575 0.030 Uiso 1 1 calc R U . . .
C5 C 0.10628(16) -0.2765(5) 0.32502(19) 0.0254(11) Uani 1 1 d . . . . .
H5 H 0.1016 -0.2713 0.2902 0.030 Uiso 1 1 calc R U . . .
C4 C 0.08414(14) -0.1776(5) 0.33658(18) 0.0177(9) Uani 1 1 d . . . . .
C9 C 0.09054(14) -0.1854(5) 0.38817(17) 0.0187(9) Uani 1 1 d . . . . .
H9 H 0.0759 -0.1182 0.3961 0.022 Uiso 1 1 calc R U . . .
C8 C 0.11902(14) -0.2948(5) 0.42763(18) 0.0206(10) Uani 1 1 d . . . . .
H8 H 0.1230 -0.3017 0.4620 0.025 Uiso 1 1 calc R U . . .
C3 C 0.03084(14) 0.0240(5) 0.30333(17) 0.0170(9) Uani 1 1 d . . . . .
H3A H 0.0511 0.0864 0.3370 0.020 Uiso 1 1 calc R U . . .
H3B H 0.0125 -0.0355 0.3097 0.020 Uiso 1 1 calc R U . . .
C1 C 0.0000 0.1218(6) 0.2500 0.0136(12) Uani 1 2 d S T P . .
C2 C 0.02869(14) 0.2204(5) 0.24087(17) 0.0176(9) Uani 1 1 d . . . . .
H2A H 0.0511 0.2764 0.2756 0.021 Uiso 1 1 calc R U . . .
H2B H 0.0445 0.1600 0.2307 0.021 Uiso 1 1 calc R U . . .
C17 C 0.01217(16) 0.4280(5) 0.17746(18) 0.0219(10) Uani 1 1 d . . . . .
C21 C -0.02236(16) 0.5163(5) 0.1324(2) 0.0277(11) Uani 1 1 d . . . . .
H21 H -0.0524 0.5036 0.1184 0.033 Uiso 1 1 calc R U . . .
C22 C -0.01155(16) 0.6229(5) 0.1088(2) 0.0276(11) Uani 1 1 d . . . . .
H22 H -0.0347 0.6807 0.0782 0.033 Uiso 1 1 calc R U . . .
C20 C 0.03332(16) 0.6460(5) 0.12966(18) 0.0226(10) Uani 1 1 d . . . . .
C19 C 0.06717(16) 0.5617(5) 0.17609(18) 0.0237(10) Uani 1 1 d . . . . .
H19 H 0.0975 0.5790 0.1918 0.028 Uiso 1 1 calc R U . . .
C18 C 0.05702(16) 0.4505(5) 0.20024(18) 0.0240(10) Uani 1 1 d . . . . .
H18 H 0.0801 0.3931 0.2311 0.029 Uiso 1 1 calc R U . . .
C23 C 0.04341(16) 0.7562(5) 0.10026(19) 0.0229(10) Uani 1 1 d . . . . .
O1W O 0.1337(3) 0.5196(6) 0.1297(3) 0.127(3) Uani 1 1 d . . . . .
H1W H 0.1601 0.5535 0.1524 0.190 Uiso 1 1 d R U . . .
H2W H 0.1163 0.5804 0.1300 0.190 Uiso 1 1 d R U . . .
O6W O 0.21300(18) 0.1556(6) 0.1425(2) 0.0945(18) Uani 1 1 d . . . . .
H11W H 0.1950 0.2253 0.1180 0.142 Uiso 1 1 d R U . . .
H12W H 0.2305 0.1451 0.1321 0.142 Uiso 1 1 d R U . . .
O8WA O 0.2761(6) 0.143(2) 0.3250(9) 0.188(8) Uani 0.5 1 d . U P . .
O8WB O 0.2462(4) 0.2255(15) 0.2627(6) 0.104(4) Uani 0.5 1 d . . P . .
O9W O 0.2096(7) 0.965(3) 0.2052(11) 0.251(11) Uani 0.5 1 d . U P . .
O7W O 0.12700(14) 0.1267(5) 0.24779(15) 0.0589(12) Uani 1 1 d . . . . .
H14W H 0.1313 0.1150 0.2795 0.088 Uiso 1 1 d R U . . .
H13W H 0.1501 0.1685 0.2542 0.088 Uiso 1 1 d R U . . .
O5W O 0.1573(2) 0.3839(6) 0.0700(3) 0.113(2) Uani 1 1 d . . . . .
H9W H 0.1628 0.4132 0.0471 0.169 Uiso 1 1 d R U . . .
H10W H 0.1398 0.4369 0.0730 0.169 Uiso 1 1 d R U . . .
O4W O 0.16878(17) 0.3606(5) 0.23195(18) 0.0713(14) Uani 1 1 d . . . . .
H8W H 0.1481 0.4198 0.2048 0.107 Uiso 1 1 d R U . . .
H7W H 0.1973 0.3765 0.2434 0.107 Uiso 1 1 d R U . . .
O2W O 0.15238(15) 0.8580(5) 0.22971(18) 0.0708(14) Uani 1 1 d . . . . .
H3W H 0.1711 0.9226 0.2294 0.106 Uiso 1 1 d R U . . .
H4W H 0.1290 0.8328 0.1960 0.106 Uiso 1 1 d R U . . .
O3W O 0.19566(15) 0.6106(5) 0.30631(17) 0.0653(13) Uani 1 1 d . . . . .
H5W H 0.1823 0.6958 0.2904 0.098 Uiso 1 1 d R U . . .
H6W H 0.1712 0.5613 0.2826 0.098 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N6 2.026(4) . ?
Ni1 N6 2.026(4) 5_575 ?
Ni1 N4 2.096(4) 5_575 ?
Ni1 N4 2.096(4) . ?
Ni1 O2 2.156(3) . ?
Ni1 O2 2.156(3) 5_575 ?
Ni2 N2 2.032(3) 7_536 ?
Ni2 N2 2.032(3) . ?
Ni2 N1 2.104(4) 7_536 ?
Ni2 N1 2.104(4) . ?
Ni2 O6 2.149(3) 7_536 ?
Ni2 O6 2.149(3) . ?
O6 C10 1.264(5) . ?
O5 C10 1.248(5) . ?
O4 C4 1.382(5) . ?
O4 C3 1.424(5) . ?
O1 C17 1.365(5) . ?
O1 C2 1.434(5) . ?
O3 C23 1.251(5) . ?
O2 C23 1.258(5) . ?
N2 C12 1.476(6) . ?
N2 C11 1.483(5) . ?
N2 H2 0.9800 . ?
N1 C14 1.481(5) . ?
N1 C16 1.484(6) . ?
N1 C13 1.491(6) . ?
N3 C14 1.461(6) . ?
N3 C11 1.470(6) 7_536 ?
N3 C15 1.481(6) . ?
N4 C25 1.481(6) . ?
N4 C26 1.484(6) . ?
N4 C24 1.483(6) . ?
N6 C28 1.490(6) . ?
N6 C29 1.498(6) . ?
N6 H6N 0.9800 . ?
N5 C29 1.446(6) . ?
N5 C25 1.452(6) . ?
N5 C27 1.484(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C27 C26 1.554(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C28 C24 1.519(7) 5_575 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C24 C28 1.519(7) 5_575 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C15 1.513(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C11 N3 1.470(6) 7_536 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.511(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C10 C7 1.507(6) . ?
C7 C8 1.391(6) . ?
C7 C6 1.395(6) . ?
C6 C5 1.366(6) . ?
C6 H6 0.9300 . ?
C5 C4 1.385(6) . ?
C5 H5 0.9300 . ?
C4 C9 1.386(6) . ?
C9 C8 1.383(6) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C3 C1 1.525(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 C3 1.525(5) 2 ?
C1 C2 1.529(5) 2 ?
C1 C2 1.529(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C17 C18 1.376(6) . ?
C17 C21 1.391(6) . ?
C21 C22 1.377(6) . ?
C21 H21 0.9300 . ?
C22 C20 1.392(7) . ?
C22 H22 0.9300 . ?
C20 C19 1.379(6) . ?
C20 C23 1.502(6) . ?
C19 C18 1.402(6) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
O1W H1W 0.8329 . ?
O1W H2W 0.8477 . ?
O6W H11W 0.8733 . ?
O6W H12W 0.8755 . ?
O8WA O8WB 1.62(2) . ?
O7W H14W 0.8500 . ?
O7W H13W 0.8453 . ?
O5W H9W 0.8567 . ?
O5W H10W 0.8512 . ?
O4W H8W 0.8679 . ?
O4W H7W 0.9057 . ?
O2W H3W 0.9081 . ?
O2W H4W 0.8536 . ?
O3W H5W 0.8713 . ?
O3W H6W 0.8524 . ?

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
N6 Ni1 N6 180.0 . 5_575 ?
N6 Ni1 N4 87.13(15) . 5_575 ?
N6 Ni1 N4 92.87(15) 5_575 5_575 ?
N6 Ni1 N4 92.87(15) . . ?
N6 Ni1 N4 87.13(15) 5_575 . ?
N4 Ni1 N4 180.0 5_575 . ?
N6 Ni1 O2 91.64(13) . . ?
N6 Ni1 O2 88.36(13) 5_575 . ?
N4 Ni1 O2 88.50(13) 5_575 . ?
N4 Ni1 O2 91.51(13) . . ?
N6 Ni1 O2 88.36(13) . 5_575 ?
N6 Ni1 O2 91.64(13) 5_575 5_575 ?
N4 Ni1 O2 91.50(13) 5_575 5_575 ?
N4 Ni1 O2 88.49(13) . 5_575 ?
O2 Ni1 O2 180.0 . 5_575 ?
N2 Ni2 N2 180.0 7_536 . ?
N2 Ni2 N1 86.40(14) 7_536 7_536 ?
N2 Ni2 N1 93.60(14) . 7_536 ?
N2 Ni2 N1 93.60(14) 7_536 . ?
N2 Ni2 N1 86.40(14) . . ?
N1 Ni2 N1 180.0(2) 7_536 . ?
N2 Ni2 O6 92.42(13) 7_536 7_536 ?
N2 Ni2 O6 87.58(13) . 7_536 ?
N1 Ni2 O6 88.87(13) 7_536 7_536 ?
N1 Ni2 O6 91.12(13) . 7_536 ?
N2 Ni2 O6 87.58(13) 7_536 . ?
N2 Ni2 O6 92.42(13) . . ?
N1 Ni2 O6 91.13(13) 7_536 . ?
N1 Ni2 O6 88.87(13) . . ?
O6 Ni2 O6 180.00(10) 7_536 . ?
C10 O6 Ni2 134.0(3) . . ?
C4 O4 C3 117.3(3) . . ?
C17 O1 C2 120.2(3) . . ?
C23 O2 Ni1 136.9(3) . . ?
C12 N2 C11 114.0(3) . . ?
C12 N2 Ni2 105.2(3) . . ?
C11 N2 Ni2 116.8(3) . . ?
C12 N2 H2 106.7 . . ?
C11 N2 H2 106.7 . . ?
Ni2 N2 H2 106.7 . . ?
C14 N1 C16 99.5(3) . . ?
C14 N1 C13 114.4(4) . . ?
C16 N1 C13 114.7(4) . . ?
C14 N1 Ni2 108.7(3) . . ?
C16 N1 Ni2 116.1(3) . . ?
C13 N1 Ni2 103.8(3) . . ?
C14 N3 C11 115.4(4) . 7_536 ?
C14 N3 C15 103.3(4) . . ?
C11 N3 C15 115.2(4) 7_536 . ?
C25 N4 C26 101.1(4) . . ?
C25 N4 C24 114.4(3) . . ?
C26 N4 C24 113.8(4) . . ?
C25 N4 Ni1 109.1(3) . . ?
C26 N4 Ni1 115.0(3) . . ?
C24 N4 Ni1 103.8(3) . . ?
C28 N6 C29 114.0(4) . . ?
C28 N6 Ni1 105.0(3) . . ?
C29 N6 Ni1 116.8(3) . . ?
C28 N6 H6N 106.8 . . ?
C29 N6 H6N 106.8 . . ?
Ni1 N6 H6N 106.8 . . ?
C29 N5 C25 115.0(4) . . ?
C29 N5 C27 114.6(4) . . ?
C25 N5 C27 102.6(4) . . ?
N5 C25 N4 104.8(4) . . ?
N5 C25 H25A 110.8 . . ?
N4 C25 H25A 110.8 . . ?
N5 C25 H25B 110.8 . . ?
N4 C25 H25B 110.8 . . ?
H25A C25 H25B 108.9 . . ?
N5 C27 C26 106.5(4) . . ?
N5 C27 H27A 110.4 . . ?
C26 C27 H27A 110.4 . . ?
N5 C27 H27B 110.4 . . ?
C26 C27 H27B 110.4 . . ?
H27A C27 H27B 108.6 . . ?
N4 C26 C27 102.9(4) . . ?
N4 C26 H26A 111.2 . . ?
C27 C26 H26A 111.2 . . ?
N4 C26 H26B 111.2 . . ?
C27 C26 H26B 111.2 . . ?
H26A C26 H26B 109.1 . . ?
N5 C29 N6 115.3(4) . . ?
N5 C29 H29A 108.5 . . ?
N6 C29 H29A 108.5 . . ?
N5 C29 H29B 108.5 . . ?
N6 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
N6 C28 C24 108.1(4) . 5_575 ?
N6 C28 H28A 110.1 . . ?
C24 C28 H28A 110.1 5_575 . ?
N6 C28 H28B 110.1 . . ?
C24 C28 H28B 110.1 5_575 . ?
H28A C28 H28B 108.4 . . ?
N4 C24 C28 110.6(4) . 5_575 ?
N4 C24 H24A 109.5 . . ?
C28 C24 H24A 109.5 5_575 . ?
N4 C24 H24B 109.5 . . ?
C28 C24 H24B 109.5 5_575 . ?
H24A C24 H24B 108.1 . . ?
N3 C14 N1 103.5(4) . . ?
N3 C14 H14A 111.1 . . ?
N1 C14 H14A 111.1 . . ?
N3 C14 H14B 111.1 . . ?
N1 C14 H14B 111.1 . . ?
H14A C14 H14B 109.0 . . ?
N1 C16 C15 104.6(4) . . ?
N1 C16 H16A 110.8 . . ?
C15 C16 H16A 110.8 . . ?
N1 C16 H16B 110.8 . . ?
C15 C16 H16B 110.8 . . ?
H16A C16 H16B 108.9 . . ?
N3 C15 C16 105.7(4) . . ?
N3 C15 H15A 110.6 . . ?
C16 C15 H15A 110.6 . . ?
N3 C15 H15B 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.7 . . ?
N3 C11 N2 114.4(4) 7_536 . ?
N3 C11 H11A 108.7 7_536 . ?
N2 C11 H11A 108.7 . . ?
N3 C11 H11B 108.7 7_536 . ?
N2 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N2 C12 C13 108.3(4) . . ?
N2 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
N2 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N1 C13 C12 109.9(4) . . ?
N1 C13 H13A 109.7 . . ?
C12 C13 H13A 109.7 . . ?
N1 C13 H13B 109.7 . . ?
C12 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
O5 C10 O6 125.1(4) . . ?
O5 C10 C7 118.7(4) . . ?
O6 C10 C7 116.2(4) . . ?
C8 C7 C6 117.6(4) . . ?
C8 C7 C10 120.2(4) . . ?
C6 C7 C10 122.1(4) . . ?
C5 C6 C7 121.6(4) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
O4 C4 C5 116.1(4) . . ?
O4 C4 C9 123.2(4) . . ?
C5 C4 C9 120.6(4) . . ?
C8 C9 C4 118.8(4) . . ?
C8 C9 H9 120.6 . . ?
C4 C9 H9 120.6 . . ?
C9 C8 C7 121.7(4) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
O4 C3 C1 108.8(3) . . ?
O4 C3 H3A 109.9 . . ?
C1 C3 H3A 109.9 . . ?
O4 C3 H3B 109.9 . . ?
C1 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C3 C1 C3 110.1(5) . 2 ?
C3 C1 C2 108.3(2) . 2 ?
C3 C1 C2 110.3(2) 2 2 ?
C3 C1 C2 110.3(2) . . ?
C3 C1 C2 108.3(2) 2 . ?
C2 C1 C2 109.6(5) 2 . ?
O1 C2 C1 105.5(3) . . ?
O1 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
O1 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
O1 C17 C18 125.3(4) . . ?
O1 C17 C21 113.9(4) . . ?
C18 C17 C21 120.8(4) . . ?
C22 C21 C17 119.3(4) . . ?
C22 C21 H21 120.3 . . ?
C17 C21 H21 120.3 . . ?
C21 C22 C20 121.5(4) . . ?
C21 C22 H22 119.3 . . ?
C20 C22 H22 119.3 . . ?
C19 C20 C22 118.1(4) . . ?
C19 C20 C23 122.0(4) . . ?
C22 C20 C23 119.9(4) . . ?
C20 C19 C18 121.6(4) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C17 C18 C19 118.7(4) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
O3 C23 O2 124.3(4) . . ?
O3 C23 C20 118.2(4) . . ?
O2 C23 C20 117.4(4) . . ?
H1W O1W H2W 106.5 . . ?
H11W O6W H12W 98.3 . . ?
H14W O7W H13W 109.3 . . ?
H9W O5W H10W 118.6 . . ?
H8W O4W H7W 114.8 . . ?
H3W O2W H4W 113.3 . . ?
H5W O3W H6W 92.5 . . ?

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
C29 N5 C25 N4 -84.5(5) . . . . ?
C27 N5 C25 N4 40.7(4) . . . . ?
C26 N4 C25 N5 -48.1(4) . . . . ?
C24 N4 C25 N5 -170.8(4) . . . . ?
Ni1 N4 C25 N5 73.4(4) . . . . ?
C29 N5 C27 C26 107.7(5) . . . . ?
C25 N5 C27 C26 -17.7(5) . . . . ?
C25 N4 C26 C27 34.5(4) . . . . ?
C24 N4 C26 C27 157.7(4) . . . . ?
Ni1 N4 C26 C27 -82.8(4) . . . . ?
N5 C27 C26 N4 -10.9(5) . . . . ?
C25 N5 C29 N6 67.3(5) . . . . ?
C27 N5 C29 N6 -51.4(6) . . . . ?
C28 N6 C29 N5 -166.5(4) . . . . ?
Ni1 N6 C29 N5 -43.7(5) . . . . ?
C29 N6 C28 C24 173.8(4) . . . 5_575 ?
Ni1 N6 C28 C24 44.7(4) . . . 5_575 ?
C25 N4 C24 C28 -155.8(4) . . . 5_575 ?
C26 N4 C24 C28 88.7(5) . . . 5_575 ?
Ni1 N4 C24 C28 -37.0(4) . . . 5_575 ?
C11 N3 C14 N1 -86.0(4) 7_536 . . . ?
C15 N3 C14 N1 40.7(4) . . . . ?
C16 N1 C14 N3 -48.7(4) . . . . ?
C13 N1 C14 N3 -171.4(4) . . . . ?
Ni2 N1 C14 N3 73.1(4) . . . . ?
C14 N1 C16 C15 37.3(4) . . . . ?
C13 N1 C16 C15 159.9(4) . . . . ?
Ni2 N1 C16 C15 -79.0(4) . . . . ?
C14 N3 C15 C16 -16.2(5) . . . . ?
C11 N3 C15 C16 110.6(4) 7_536 . . . ?
N1 C16 C15 N3 -13.6(5) . . . . ?
C12 N2 C11 N3 166.3(4) . . . 7_536 ?
Ni2 N2 C11 N3 43.1(5) . . . 7_536 ?
C11 N2 C12 C13 -175.1(4) . . . . ?
Ni2 N2 C12 C13 -45.8(4) . . . . ?
C14 N1 C13 C12 -156.0(4) . . . . ?
C16 N1 C13 C12 90.0(5) . . . . ?
Ni2 N1 C13 C12 -37.7(4) . . . . ?
N2 C12 C13 N1 58.3(5) . . . . ?
Ni2 O6 C10 O5 0.3(7) . . . . ?
Ni2 O6 C10 C7 -178.9(3) . . . . ?
O5 C10 C7 C8 13.0(6) . . . . ?
O6 C10 C7 C8 -167.7(4) . . . . ?
O5 C10 C7 C6 -168.7(4) . . . . ?
O6 C10 C7 C6 10.6(6) . . . . ?
C8 C7 C6 C5 -1.0(7) . . . . ?
C10 C7 C6 C5 -179.4(4) . . . . ?
C7 C6 C5 C4 1.5(7) . . . . ?
C3 O4 C4 C5 175.2(4) . . . . ?
C3 O4 C4 C9 -6.3(6) . . . . ?
C6 C5 C4 O4 177.9(4) . . . . ?
C6 C5 C4 C9 -0.6(7) . . . . ?
O4 C4 C9 C8 -179.2(4) . . . . ?
C5 C4 C9 C8 -0.8(7) . . . . ?
C4 C9 C8 C7 1.3(7) . . . . ?
C6 C7 C8 C9 -0.4(7) . . . . ?
C10 C7 C8 C9 178.0(4) . . . . ?
C4 O4 C3 C1 -174.7(3) . . . . ?
O4 C3 C1 C3 57.7(2) . . . 2 ?
O4 C3 C1 C2 178.4(3) . . . 2 ?
O4 C3 C1 C2 -61.7(4) . . . . ?
C17 O1 C2 C1 177.0(3) . . . . ?
C3 C1 C2 O1 -173.0(3) . . . . ?
C3 C1 C2 O1 66.5(4) 2 . . . ?
C2 C1 C2 O1 -53.9(2) 2 . . . ?
C2 O1 C17 C18 1.7(6) . . . . ?
C2 O1 C17 C21 -179.7(4) . . . . ?
O1 C17 C21 C22 -175.7(4) . . . . ?
C18 C17 C21 C22 3.0(7) . . . . ?
C17 C21 C22 C20 -1.2(7) . . . . ?
C21 C22 C20 C19 -1.7(7) . . . . ?
C21 C22 C20 C23 176.0(4) . . . . ?
C22 C20 C19 C18 3.0(7) . . . . ?
C23 C20 C19 C18 -174.7(4) . . . . ?
O1 C17 C18 C19 176.7(4) . . . . ?
C21 C17 C18 C19 -1.7(7) . . . . ?
C20 C19 C18 C17 -1.3(7) . . . . ?
Ni1 O2 C23 O3 -7.1(7) . . . . ?
Ni1 O2 C23 C20 174.5(3) . . . . ?
C19 C20 C23 O3 -1.3(7) . . . . ?
C22 C20 C23 O3 -178.9(4) . . . . ?
C19 C20 C23 O2 177.2(4) . . . . ?
C22 C20 C23 O2 -0.4(6) . . . . ?

_refine_diff_density_max         1.546
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.107
# start Validation Reply Form
_vrf_PLAT430_2                   
;
PROBLEM: Short Inter D...A Contact  O8WB   ..  O9W     ..       2.50 Ang.  
RESPONSE: Due to the disorder of O8w and O9w, the occupancies of molecules are
set to be 0.5, and thus the short contact should be acceptable.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1401606'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C61 H84 N12 Ni2 O12, 18(H2 O)'
_chemical_formula_sum            'C61 H120 N12 Ni2 O30'
_chemical_formula_weight         1619.10

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   37.352(4)
_cell_length_b                   8.8340(10)
_cell_length_c                   29.562(3)
_cell_angle_alpha                90
_cell_angle_beta                 126.838(2)
_cell_angle_gamma                90
_cell_volume                     7806.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1432
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      20.97

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             3464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.570
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19283
_diffrn_reflns_av_unetI/netI     0.1419
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.721
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             7736
_reflns_number_gt                4183
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_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)+(0.0605P)²+0.8303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7736
_refine_ls_number_parameters     497
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1610
_refine_ls_wR_factor_gt          0.1278
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.978
_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
O4W O 0.17422(15) 0.8761(5) 0.73309(18) 0.0740(15) Uani 1 1 d . . . . .
H7W H 0.1654 0.8003 0.7419 0.111 Uiso 1 1 d R U . . .
H8W H 0.1989 0.8463 0.7402 0.111 Uiso 1 1 d R U . . .
O2W O 0.19594(14) 0.1305(5) 0.80495(18) 0.0653(13) Uani 1 1 d . . . . .
H4W H 0.1814 0.2137 0.7891 0.098 Uiso 1 1 d R U . . .
H3W H 0.1964 0.0576 0.7860 0.098 Uiso 1 1 d R U . . .
O6W O 0.1448(2) 0.0457(7) 0.6389(2) 0.142(3) Uani 1 1 d . . . . .
H11W H 0.1585 0.0629 0.6246 0.214 Uiso 1 1 d R U . . .
H12W H 0.1296 0.1245 0.6328 0.214 Uiso 1 1 d R U . . .
Ni1 Ni 0.0000 -0.5000 0.5000 0.0177(2) Uani 1 2 d S . P . .
Ni2 Ni 0.2500 1.2500 0.5000 0.0165(2) Uani 1 2 d S . P . .
O6 O 0.19847(9) 1.0807(3) 0.45298(12) 0.0219(8) Uani 1 1 d . . . . .
O5 O 0.16439(10) 1.0533(4) 0.49413(14) 0.0277(8) Uani 1 1 d . . . . .
O4 O -0.08587(10) -0.2791(4) 0.37838(13) 0.0243(8) Uani 1 1 d . . . . .
O3 O -0.01231(10) -0.3153(3) 0.44343(13) 0.0217(7) Uani 1 1 d . . . . .
O2 O 0.00165(9) 0.1768(4) 0.30251(13) 0.0227(7) Uani 1 1 d . . . . .
O1 O 0.05666(10) 0.5756(3) 0.29425(13) 0.0212(7) Uani 1 1 d . . . . .
N4 N 0.18898(12) 1.3747(4) 0.36722(16) 0.0251(10) Uani 1 1 d . . . . .
N5 N 0.20098(12) 1.4235(4) 0.45692(16) 0.0219(9) Uani 1 1 d . . . . .
N6 N 0.24033(11) 1.2623(4) 0.56070(15) 0.0192(9) Uani 1 1 d . . . . .
H6N H 0.2206 1.1784 0.5543 0.023 Uiso 1 1 calc R U . . .
N3 N -0.06177(12) -0.4069(5) 0.54267(16) 0.0242(9) Uani 1 1 d . . . . .
N1 N -0.06699(11) -0.5191(4) 0.46174(15) 0.0199(9) Uani 1 1 d . . . . .
H1 H -0.0815 -0.4303 0.4374 0.024 Uiso 1 1 calc R U . . .
N2 N 0.00939(12) -0.3436(4) 0.56065(15) 0.0200(9) Uani 1 1 d . . . . .
C1 C 0.0000 0.3830(7) 0.2500 0.0146(14) Uani 1 2 d S T P . .
C3 C -0.02875(13) 0.2815(5) 0.25900(18) 0.0179(11) Uani 1 1 d . . . . .
H3A H -0.0437 0.3416 0.2706 0.022 Uiso 1 1 calc R U . . .
H3B H -0.0512 0.2282 0.2244 0.022 Uiso 1 1 calc R U . . .
C2 C 0.02990(13) 0.4807(5) 0.30258(17) 0.0169(10) Uani 1 1 d . . . . .
H2A H 0.0117 0.5425 0.3087 0.020 Uiso 1 1 calc R U . . .
H2B H 0.0490 0.4169 0.3355 0.020 Uiso 1 1 calc R U . . .
C4 C -0.01417(15) 0.0673(5) 0.31916(19) 0.0199(11) Uani 1 1 d . . . . .
C9 C 0.01880(15) -0.0289(5) 0.3605(2) 0.0249(11) Uani 1 1 d . . . . .
H9 H 0.0479 -0.0219 0.3716 0.030 Uiso 1 1 calc R U . . .
C8 C 0.00837(15) -0.1345(5) 0.3850(2) 0.0246(11) Uani 1 1 d . . . . .
H8 H 0.0307 -0.1969 0.4135 0.029 Uiso 1 1 calc R U . . .
C7 C -0.03563(14) -0.1492(5) 0.36765(19) 0.0207(11) Uani 1 1 d . . . . .
C6 C -0.06808(15) -0.0576(5) 0.32378(19) 0.0211(11) Uani 1 1 d . . . . .
H6 H -0.0977 -0.0699 0.3103 0.025 Uiso 1 1 calc R U . . .
C5 C -0.05814(15) 0.0517(5) 0.29916(19) 0.0212(11) Uani 1 1 d . . . . .
H5 H -0.0805 0.1125 0.2700 0.025 Uiso 1 1 calc R U . . .
C11 C 0.08329(13) 0.6817(5) 0.33546(19) 0.0189(10) Uani 1 1 d . . . . .
C16 C 0.09035(13) 0.6878(5) 0.38684(18) 0.0184(10) Uani 1 1 d . . . . .
H16 H 0.0770 0.6174 0.3958 0.022 Uiso 1 1 calc R U . . .
C15 C 0.11771(13) 0.8003(5) 0.42498(19) 0.0201(11) Uani 1 1 d . . . . .
H15 H 0.1217 0.8065 0.4592 0.024 Uiso 1 1 calc R U . . .
C14 C 0.13913(14) 0.9033(5) 0.41365(19) 0.0189(10) Uani 1 1 d . . . . .
C17 C 0.16975(14) 1.0214(5) 0.45707(19) 0.0201(11) Uani 1 1 d . . . . .
C13 C 0.13231(15) 0.8919(5) 0.3621(2) 0.0246(11) Uani 1 1 d . . . . .
H13 H 0.1469 0.9590 0.3538 0.030 Uiso 1 1 calc R U . . .
C12 C 0.10457(15) 0.7839(5) 0.3231(2) 0.0242(11) Uani 1 1 d . . . . .
H12 H 0.1000 0.7791 0.2885 0.029 Uiso 1 1 calc R U . . .
C10 C -0.04512(15) -0.2552(5) 0.39880(19) 0.0218(11) Uani 1 1 d . . . . .
C24 C -0.08209(15) -0.6537(5) 0.4243(2) 0.0243(11) Uani 1 1 d . . . . .
H24A H -0.1143 -0.6500 0.3957 0.029 Uiso 1 1 calc R U . . .
H24B H -0.0748 -0.7454 0.4462 0.029 Uiso 1 1 calc R U . . .
C27 C 0.05877(14) -0.3455(5) 0.60394(19) 0.0235(11) Uani 1 1 d . . . . .
H27A H 0.0674 -0.4348 0.6275 0.028 Uiso 1 1 calc R U . . .
H27B H 0.0680 -0.2571 0.6280 0.028 Uiso 1 1 calc R U . . .
C28 C -0.00483(15) -0.1834(5) 0.5444(2) 0.0259(12) Uani 1 1 d . . . . .
H28A H 0.0083 -0.1427 0.5268 0.031 Uiso 1 1 calc R U . . .
H28B H 0.0063 -0.1244 0.5781 0.031 Uiso 1 1 calc R U . . .
C29 C -0.05571(15) -0.1680(6) 0.5034(2) 0.0291(12) Uani 1 1 d . . . . .
H29A H -0.0636 -0.0617 0.4991 0.035 Uiso 1 1 calc R U . . .
H29B H -0.0660 -0.2063 0.4666 0.035 Uiso 1 1 calc R U . . .
C26 C -0.01394(14) -0.4028(6) 0.58410(19) 0.0258(12) Uani 1 1 d . . . . .
H26A H -0.0032 -0.5042 0.5986 0.031 Uiso 1 1 calc R U . . .
H26B H -0.0065 -0.3393 0.6154 0.031 Uiso 1 1 calc R U . . .
C25 C -0.08024(15) -0.5245(5) 0.50048(19) 0.0243(11) Uani 1 1 d . . . . .
H25A H -0.1126 -0.5192 0.4778 0.029 Uiso 1 1 calc R U . . .
H25B H -0.0712 -0.6217 0.5196 0.029 Uiso 1 1 calc R U . . .
C30 C -0.07943(16) -0.2535(6) 0.5233(2) 0.0308(12) Uani 1 1 d . . . . .
H30A H -0.0760 -0.1978 0.5539 0.037 Uiso 1 1 calc R U . . .
H30B H -0.1111 -0.2594 0.4925 0.037 Uiso 1 1 calc R U . . .
C20 C 0.16849(15) 1.3783(5) 0.39604(19) 0.0247(11) Uani 1 1 d . . . . .
H20A H 0.1565 1.2789 0.3939 0.030 Uiso 1 1 calc R U . . .
H20B H 0.1438 1.4494 0.3770 0.030 Uiso 1 1 calc R U . . .
C21 C 0.20470(16) 1.5260(5) 0.3667(2) 0.0293(12) Uani 1 1 d . . . . .
H21A H 0.1790 1.5907 0.3421 0.035 Uiso 1 1 calc R U . . .
H21B H 0.2211 1.5192 0.3509 0.035 Uiso 1 1 calc R U . . .
C22 C 0.23447(16) 1.5986(5) 0.4247(2) 0.0266(12) Uani 1 1 d . . . . .
H22A H 0.2380 1.7053 0.4205 0.032 Uiso 1 1 calc R U . . .
H22B H 0.2638 1.5521 0.4459 0.032 Uiso 1 1 calc R U . . .
C23 C 0.21517(16) 1.5814(5) 0.4573(2) 0.0262(12) Uani 1 1 d . . . . .
H23A H 0.2375 1.6128 0.4961 0.031 Uiso 1 1 calc R U . . .
H23B H 0.1896 1.6481 0.4410 0.031 Uiso 1 1 calc R U . . .
C49 C 0.17995(15) 1.4195(6) 0.4863(2) 0.0260(12) Uani 1 1 d . . . . .
H49A H 0.1594 1.3346 0.4725 0.031 Uiso 1 1 calc R U . . .
H49B H 0.1630 1.5117 0.4782 0.031 Uiso 1 1 calc R U . . .
C19 C 0.21538(15) 1.4043(5) 0.54964(19) 0.0247(11) Uani 1 1 d . . . . .
H19A H 0.2356 1.4900 0.5639 0.030 Uiso 1 1 calc R U . . .
H19B H 0.2014 1.4022 0.5686 0.030 Uiso 1 1 calc R U . . .
C18 C 0.28146(15) 1.2507(6) 0.62038(19) 0.0258(11) Uani 1 1 d . . . . .
H18A H 0.2983 1.3439 0.6299 0.031 Uiso 1 1 calc R U . . .
H18B H 0.2723 1.2429 0.6449 0.031 Uiso 1 1 calc R U . . .
O1W O 0.15292(16) 0.8942(6) 0.5653(2) 0.0818(16) Uani 1 1 d . . . . .
H2W H 0.1515 0.9335 0.5377 0.123 Uiso 1 1 d R U . . .
H1W H 0.1675 0.8207 0.5882 0.123 Uiso 1 1 d R U . . .
O5W O 0.21225(16) 0.6765(6) 0.6380(2) 0.0991(19) Uani 1 1 d . . . . .
H10W H 0.2042 0.5989 0.6467 0.149 Uiso 1 1 d R U . . .
H9W H 0.2398 0.6712 0.6528 0.149 Uiso 1 1 d R U . . .
O8WA O 0.2118(3) 0.4853(15) 0.7107(6) 0.209(8) Uani 0.827(16) 1 d . . P . .
O8WB O 0.1835(12) 0.396(4) 0.645(2) 0.11(2) Uani 0.173(16) 1 d . . P . .
O9WB O 0.2469(8) 0.232(4) 0.7300(18) 0.168(13) Uani 0.43(4) 1 d . U P . .
O9WA O 0.2291(7) 0.173(2) 0.6858(13) 0.144(9) Uani 0.57(4) 1 d . U P . .
O3W O 0.15143(13) 0.3750(4) 0.72651(16) 0.0578(12) Uani 1 1 d . . . . .
H6W H 0.1321 0.3513 0.6927 0.087 Uiso 1 1 d R U . . .
H5W H 0.1740 0.4055 0.7301 0.087 Uiso 1 1 d R U . . .
O7W O 0.12932(12) 0.3474(5) 0.24829(16) 0.0617(13) Uani 1 1 d . . . . .
H14W H 0.1370 0.4188 0.2365 0.093 Uiso 1 1 d R U . . .
H13W H 0.1418 0.3666 0.2829 0.093 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4W H7W 0.8525 . ?
O4W H8W 0.8552 . ?
O2W H4W 0.8657 . ?
O2W H3W 0.8612 . ?
O6W H11W 0.8483 . ?
O6W H12W 0.8475 . ?
Ni1 N1 2.043(3) . ?
Ni1 N1 2.043(3) 5_546 ?
Ni1 N2 2.120(4) . ?
Ni1 N2 2.120(4) 5_546 ?
Ni1 O3 2.179(3) 5_546 ?
Ni1 O3 2.179(3) . ?
Ni2 N6 2.035(4) 7_576 ?
Ni2 N6 2.035(4) . ?
Ni2 N5 2.128(4) . ?
Ni2 N5 2.128(4) 7_576 ?
Ni2 O6 2.160(3) . ?
Ni2 O6 2.160(3) 7_576 ?
O6 C17 1.263(5) . ?
O5 C17 1.258(5) . ?
O4 C10 1.274(5) . ?
O3 C10 1.259(5) . ?
O2 C4 1.369(5) . ?
O2 C3 1.431(5) . ?
O1 C11 1.378(5) . ?
O1 C2 1.434(5) . ?
N4 C18 1.448(6) 7_576 ?
N4 C20 1.447(5) . ?
N4 C21 1.463(6) . ?
N5 C49 1.479(5) . ?
N5 C23 1.490(6) . ?
N5 C20 1.501(5) . ?
N6 C19 1.478(5) . ?
N6 C18 1.494(5) . ?
N6 H6N 0.9800 . ?
N3 C26 1.439(5) . ?
N3 C25 1.442(6) . ?
N3 C30 1.465(6) . ?
N1 C24 1.487(6) . ?
N1 C25 1.496(5) . ?
N1 H1 0.9800 . ?
N2 C28 1.486(5) . ?
N2 C27 1.486(5) . ?
N2 C26 1.496(5) . ?
C1 C2 1.525(5) 2 ?
C1 C2 1.525(5) . ?
C1 C3 1.539(5) . ?
C1 C3 1.540(5) 2 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C5 1.379(6) . ?
C4 C9 1.389(6) . ?
C9 C8 1.374(6) . ?
C9 H9 0.9300 . ?
C8 C7 1.403(6) . ?
C8 H8 0.9300 . ?
C7 C6 1.386(6) . ?
C7 C10 1.497(6) . ?
C6 C5 1.387(6) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C11 C16 1.378(6) . ?
C11 C12 1.389(6) . ?
C16 C15 1.386(6) . ?
C16 H16 0.9300 . ?
C15 C14 1.379(6) . ?
C15 H15 0.9300 . ?
C14 C13 1.391(6) . ?
C14 C17 1.511(6) . ?
C13 C12 1.371(6) . ?
C13 H13 0.9300 . ?
C12 H12 0.9300 . ?
C24 C27 1.525(6) 5_546 ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C27 C24 1.525(6) 5_546 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.529(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.526(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.517(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.518(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C49 C19 1.519(6) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C18 N4 1.448(6) 7_576 ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
O1W H2W 0.8586 . ?
O1W H1W 0.8578 . ?
O5W H10W 0.8487 . ?
O5W H9W 0.8430 . ?
O8WA O8WB 1.76(5) . ?
O9WB O9WA 1.18(3) . ?
O3W H6W 0.8368 . ?
O3W H5W 0.8294 . ?
O7W H14W 0.8486 . ?
O7W H13W 0.8484 . ?

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
H7W O4W H8W 103.8 . . ?
H4W O2W H3W 122.2 . . ?
H11W O6W H12W 106.0 . . ?
N1 Ni1 N1 180.0(2) . 5_546 ?
N1 Ni1 N2 92.79(14) . . ?
N1 Ni1 N2 87.21(14) 5_546 . ?
N1 Ni1 N2 87.21(14) . 5_546 ?
N1 Ni1 N2 92.78(14) 5_546 5_546 ?
N2 Ni1 N2 180.0 . 5_546 ?
N1 Ni1 O3 89.31(13) . 5_546 ?
N1 Ni1 O3 90.69(13) 5_546 5_546 ?
N2 Ni1 O3 89.25(13) . 5_546 ?
N2 Ni1 O3 90.75(13) 5_546 5_546 ?
N1 Ni1 O3 90.69(13) . . ?
N1 Ni1 O3 89.31(13) 5_546 . ?
N2 Ni1 O3 90.74(13) . . ?
N2 Ni1 O3 89.25(13) 5_546 . ?
O3 Ni1 O3 180.0 5_546 . ?
N6 Ni2 N6 180.0 7_576 . ?
N6 Ni2 N5 93.14(14) 7_576 . ?
N6 Ni2 N5 86.86(14) . . ?
N6 Ni2 N5 86.86(14) 7_576 7_576 ?
N6 Ni2 N5 93.14(14) . 7_576 ?
N5 Ni2 N5 180.0 . 7_576 ?
N6 Ni2 O6 87.50(13) 7_576 . ?
N6 Ni2 O6 92.50(13) . . ?
N5 Ni2 O6 89.92(13) . . ?
N5 Ni2 O6 90.08(13) 7_576 . ?
N6 Ni2 O6 92.50(13) 7_576 7_576 ?
N6 Ni2 O6 87.50(13) . 7_576 ?
N5 Ni2 O6 90.08(13) . 7_576 ?
N5 Ni2 O6 89.92(13) 7_576 7_576 ?
O6 Ni2 O6 180.00(11) . 7_576 ?
C17 O6 Ni2 134.9(3) . . ?
C10 O3 Ni1 138.2(3) . . ?
C4 O2 C3 119.9(3) . . ?
C11 O1 C2 117.0(3) . . ?
C18 N4 C20 117.4(4) 7_576 . ?
C18 N4 C21 116.8(4) 7_576 . ?
C20 N4 C21 110.1(4) . . ?
C49 N5 C23 109.2(4) . . ?
C49 N5 C20 111.4(3) . . ?
C23 N5 C20 106.6(4) . . ?
C49 N5 Ni2 101.6(3) . . ?
C23 N5 Ni2 119.7(3) . . ?
C20 N5 Ni2 108.3(3) . . ?
C19 N6 C18 112.7(4) . . ?
C19 N6 Ni2 105.8(3) . . ?
C18 N6 Ni2 115.9(3) . . ?
C19 N6 H6N 107.4 . . ?
C18 N6 H6N 107.4 . . ?
Ni2 N6 H6N 107.4 . . ?
C26 N3 C25 117.4(4) . . ?
C26 N3 C30 110.3(4) . . ?
C25 N3 C30 117.3(4) . . ?
C24 N1 C25 113.1(3) . . ?
C24 N1 Ni1 105.7(3) . . ?
C25 N1 Ni1 115.9(3) . . ?
C24 N1 H1 107.3 . . ?
C25 N1 H1 107.3 . . ?
Ni1 N1 H1 107.3 . . ?
C28 N2 C27 107.9(3) . . ?
C28 N2 C26 106.8(3) . . ?
C27 N2 C26 111.3(4) . . ?
C28 N2 Ni1 120.0(3) . . ?
C27 N2 Ni1 102.2(3) . . ?
C26 N2 Ni1 108.5(3) . . ?
C2 C1 C2 111.1(5) 2 . ?
C2 C1 C3 110.2(2) 2 . ?
C2 C1 C3 108.3(2) . . ?
C2 C1 C3 108.3(2) 2 2 ?
C2 C1 C3 110.2(2) . 2 ?
C3 C1 C3 108.8(5) . 2 ?
O2 C3 C1 105.8(3) . . ?
O2 C3 H3A 110.6 . . ?
C1 C3 H3A 110.6 . . ?
O2 C3 H3B 110.6 . . ?
C1 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
O1 C2 C1 108.4(3) . . ?
O1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O2 C4 C5 125.2(4) . . ?
O2 C4 C9 113.7(4) . . ?
C5 C4 C9 121.0(4) . . ?
C8 C9 C4 119.9(4) . . ?
C8 C9 H9 120.1 . . ?
C4 C9 H9 120.1 . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C6 C7 C8 117.6(4) . . ?
C6 C7 C10 122.9(4) . . ?
C8 C7 C10 119.3(4) . . ?
C7 C6 C5 122.6(4) . . ?
C7 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C4 C5 C6 118.0(4) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C16 C11 O1 124.1(4) . . ?
C16 C11 C12 120.2(4) . . ?
O1 C11 C12 115.6(4) . . ?
C11 C16 C15 119.0(4) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C14 C15 C16 121.8(4) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C15 C14 C13 117.9(4) . . ?
C15 C14 C17 120.2(4) . . ?
C13 C14 C17 121.9(4) . . ?
O5 C17 O6 125.3(4) . . ?
O5 C17 C14 117.4(4) . . ?
O6 C17 C14 117.3(4) . . ?
C12 C13 C14 121.4(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
O3 C10 O4 124.2(4) . . ?
O3 C10 C7 117.9(4) . . ?
O4 C10 C7 117.9(4) . . ?
N1 C24 C27 109.0(4) . 5_546 ?
N1 C24 H24A 109.9 . . ?
C27 C24 H24A 109.9 5_546 . ?
N1 C24 H24B 109.9 . . ?
C27 C24 H24B 109.9 5_546 . ?
H24A C24 H24B 108.3 . . ?
N2 C27 C24 110.5(4) . 5_546 ?
N2 C27 H27A 109.6 . . ?
C24 C27 H27A 109.6 5_546 . ?
N2 C27 H27B 109.6 . . ?
C24 C27 H27B 109.6 5_546 . ?
H27A C27 H27B 108.1 . . ?
N2 C28 C29 112.0(4) . . ?
N2 C28 H28A 109.2 . . ?
C29 C28 H28A 109.2 . . ?
N2 C28 H28B 109.2 . . ?
C29 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C28 112.5(4) . . ?
C30 C29 H29A 109.1 . . ?
C28 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
C28 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
N3 C26 N2 112.7(4) . . ?
N3 C26 H26A 109.1 . . ?
N2 C26 H26A 109.1 . . ?
N3 C26 H26B 109.1 . . ?
N2 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
N3 C25 N1 115.6(4) . . ?
N3 C25 H25A 108.4 . . ?
N1 C25 H25A 108.4 . . ?
N3 C25 H25B 108.4 . . ?
N1 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
N3 C30 C29 112.3(4) . . ?
N3 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
N3 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
N4 C20 N5 112.3(3) . . ?
N4 C20 H20A 109.1 . . ?
N5 C20 H20A 109.1 . . ?
N4 C20 H20B 109.1 . . ?
N5 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N4 C21 C22 113.7(4) . . ?
N4 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
N4 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 C23 111.7(4) . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
N5 C23 C22 113.0(4) . . ?
N5 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
N5 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
N5 C49 C19 110.4(4) . . ?
N5 C49 H49A 109.6 . . ?
C19 C49 H49A 109.6 . . ?
N5 C49 H49B 109.6 . . ?
C19 C49 H49B 109.6 . . ?
H49A C49 H49B 108.1 . . ?
N6 C19 C49 108.4(4) . . ?
N6 C19 H19A 110.0 . . ?
C49 C19 H19A 110.0 . . ?
N6 C19 H19B 110.0 . . ?
C49 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
N4 C18 N6 116.1(4) 7_576 . ?
N4 C18 H18A 108.3 7_576 . ?
N6 C18 H18A 108.3 . . ?
N4 C18 H18B 108.3 7_576 . ?
N6 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
H2W O1W H1W 134.8 . . ?
H10W O5W H9W 110.1 . . ?
H6W O3W H5W 108.3 . . ?
H14W O7W H13W 105.6 . . ?

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
C4 O2 C3 C1 -178.2(4) . . . . ?
C2 C1 C3 O2 170.0(3) 2 . . . ?
C2 C1 C3 O2 -68.4(4) . . . . ?
C3 C1 C3 O2 51.4(2) 2 . . . ?
C11 O1 C2 C1 174.7(3) . . . . ?
C2 C1 C2 O1 -58.8(3) 2 . . . ?
C3 C1 C2 O1 -179.9(3) . . . . ?
C3 C1 C2 O1 61.3(5) 2 . . . ?
C3 O2 C4 C5 -3.3(7) . . . . ?
C3 O2 C4 C9 178.3(4) . . . . ?
O2 C4 C9 C8 173.7(4) . . . . ?
C5 C4 C9 C8 -4.8(7) . . . . ?
C4 C9 C8 C7 1.8(7) . . . . ?
C9 C8 C7 C6 2.3(7) . . . . ?
C9 C8 C7 C10 -174.4(4) . . . . ?
C8 C7 C6 C5 -3.5(7) . . . . ?
C10 C7 C6 C5 173.0(4) . . . . ?
O2 C4 C5 C6 -174.7(4) . . . . ?
C9 C4 C5 C6 3.5(7) . . . . ?
C7 C6 C5 C4 0.7(7) . . . . ?
C2 O1 C11 C16 9.4(6) . . . . ?
C2 O1 C11 C12 -172.4(4) . . . . ?
O1 C11 C16 C15 -179.7(4) . . . . ?
C12 C11 C16 C15 2.2(6) . . . . ?
C11 C16 C15 C14 -2.1(6) . . . . ?
C16 C15 C14 C13 0.4(7) . . . . ?
C16 C15 C14 C17 -178.2(4) . . . . ?
Ni2 O6 C17 O5 0.4(7) . . . . ?
Ni2 O6 C17 C14 179.9(3) . . . . ?
C15 C14 C17 O5 -21.6(6) . . . . ?
C13 C14 C17 O5 159.9(4) . . . . ?
C15 C14 C17 O6 158.8(4) . . . . ?
C13 C14 C17 O6 -19.7(6) . . . . ?
C15 C14 C13 C12 1.2(7) . . . . ?
C17 C14 C13 C12 179.7(4) . . . . ?
C14 C13 C12 C11 -1.1(7) . . . . ?
C16 C11 C12 C13 -0.7(7) . . . . ?
O1 C11 C12 C13 -178.9(4) . . . . ?
Ni1 O3 C10 O4 13.4(8) . . . . ?
Ni1 O3 C10 C7 -166.4(3) . . . . ?
C6 C7 C10 O3 -169.0(4) . . . . ?
C8 C7 C10 O3 7.5(7) . . . . ?
C6 C7 C10 O4 11.2(7) . . . . ?
C8 C7 C10 O4 -172.3(4) . . . . ?
C25 N1 C24 C27 -167.9(4) . . . 5_546 ?
Ni1 N1 C24 C27 -40.1(4) . . . 5_546 ?
C28 N2 C27 C24 -85.5(4) . . . 5_546 ?
C26 N2 C27 C24 157.6(4) . . . 5_546 ?
Ni1 N2 C27 C24 42.0(4) . . . 5_546 ?
C27 N2 C28 C29 -175.4(4) . . . . ?
C26 N2 C28 C29 -55.6(5) . . . . ?
Ni1 N2 C28 C29 68.3(4) . . . . ?
N2 C28 C29 C30 48.9(6) . . . . ?
C25 N3 C26 N2 74.6(5) . . . . ?
C30 N3 C26 N2 -63.4(5) . . . . ?
C28 N2 C26 N3 64.3(5) . . . . ?
C27 N2 C26 N3 -178.1(4) . . . . ?
Ni1 N2 C26 N3 -66.4(4) . . . . ?
C26 N3 C25 N1 -63.2(5) . . . . ?
C30 N3 C25 N1 71.8(5) . . . . ?
C24 N1 C25 N3 172.5(4) . . . . ?
Ni1 N1 C25 N3 50.2(5) . . . . ?
C26 N3 C30 C29 52.5(5) . . . . ?
C25 N3 C30 C29 -85.6(5) . . . . ?
C28 C29 C30 N3 -46.1(6) . . . . ?
C18 N4 C20 N5 74.5(5) 7_576 . . . ?
C21 N4 C20 N5 -62.5(5) . . . . ?
C49 N5 C20 N4 -177.3(4) . . . . ?
C23 N5 C20 N4 63.5(5) . . . . ?
Ni2 N5 C20 N4 -66.4(4) . . . . ?
C18 N4 C21 C22 -84.8(5) 7_576 . . . ?
C20 N4 C21 C22 52.4(5) . . . . ?
N4 C21 C22 C23 -45.9(6) . . . . ?
C49 N5 C23 C22 -176.3(4) . . . . ?
C20 N5 C23 C22 -55.8(5) . . . . ?
Ni2 N5 C23 C22 67.4(5) . . . . ?
C21 C22 C23 N5 48.6(5) . . . . ?
C23 N5 C49 C19 -84.5(4) . . . . ?
C20 N5 C49 C19 157.9(4) . . . . ?
Ni2 N5 C49 C19 42.9(4) . . . . ?
C18 N6 C19 C49 169.0(4) . . . . ?
Ni2 N6 C19 C49 41.4(4) . . . . ?
N5 C49 C19 N6 -59.9(5) . . . . ?
C19 N6 C18 N4 -171.8(4) . . . 7_576 ?
Ni2 N6 C18 N4 -49.8(5) . . . 7_576 ?

_refine_diff_density_max         0.651
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.093
# start Validation Reply Form
_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact  O9WA   ..  O8WB    ..       2.40 Ang.  
RESPONSE: This alert comes from the disorder of O9w and O8w.
;
_vrf_PLAT420_3                   
;
PROBLEM: D-H Without Acceptor        O4W    -   H8W    ..     Please Check 
RESPONSE: The O4w-H8w bond points to the disordered O9w.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_sq
_database_code_depnum_ccdc_archive 'CCDC 1401607'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C57 H76 N12 Ni2 O12,4(C3 H7 N O),10(H2 O)'
_chemical_formula_sum            'C69 H124 N16 Ni2 O26'
_chemical_formula_weight         1711.25

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

_cell_length_a                   11.579(2)
_cell_length_b                   25.062(5)
_cell_length_c                   31.421(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9118(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    29127
_cell_measurement_theta_min      2.1075
_cell_measurement_theta_max      29.1270

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_F_000             3656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.155
_exptl_absorpt_coefficient_mu    0.490
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8851
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            60629
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.107
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8484
_reflns_number_gt                7736
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0770P)²+7.7189P] 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         8484
_refine_ls_number_parameters     375
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.1963
_refine_ls_wR_factor_gt          0.1926
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.002
_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
Ni1 Ni 1.12001(4) 0.77665(2) 0.88883(2) 0.05144(17) Uani 1 1 d . . . . .
O1 O 1.1468(3) 0.91111(11) 0.84932(9) 0.0792(9) Uani 1 1 d . . . . .
O2 O 1.0498(2) 0.83375(10) 0.84627(8) 0.0633(7) Uani 1 1 d . . . . .
O3 O 0.6439(3) 1.18691(12) 0.40782(8) 0.0720(8) Uani 1 1 d . . . . .
O4 O 0.8099(2) 1.22057(9) 0.43348(7) 0.0562(6) Uani 1 1 d . . . . .
O5 O 0.6791(2) 1.05824(9) 0.58052(7) 0.0492(6) Uani 1 1 d . . . . .
O6 O 0.8291(3) 0.94112(9) 0.68540(7) 0.0606(7) Uani 1 1 d . . . . .
N1 N 1.0837(4) 0.84475(16) 0.97526(11) 0.0868(12) Uani 1 1 d . U . . .
N2 N 0.9835(3) 0.78731(13) 0.93174(11) 0.0686(9) Uani 1 1 d . . . . .
N3 N 1.0155(4) 0.71931(12) 0.85941(12) 0.0744(10) Uani 1 1 d . . . . .
N4 N 1.2567(3) 0.76155(13) 0.84998(9) 0.0629(9) Uani 1 1 d . . . . .
H1N H 1.2976 0.7314 0.8629 0.076 Uiso 1 1 calc R U . . .
N5 N 1.1378(6) 0.70717(18) 0.80167(12) 0.1002(16) Uani 1 1 d . . . . .
N6 N 1.2188(3) 0.83631(12) 0.91428(9) 0.0614(8) Uani 1 1 d . . . . .
H2N H 1.1951 0.8692 0.8999 0.074 Uiso 1 1 calc R U . . .
C1 C 0.7500 1.0000 0.63442(12) 0.0374(9) Uani 1 2 d S T P . .
C2 C 0.8546(3) 0.98875(12) 0.66205(9) 0.0476(8) Uani 1 1 d . . . . .
H2A H 0.9227 0.9837 0.6445 0.057 Uiso 1 1 calc R U . . .
H2B H 0.8686 1.0182 0.6814 0.057 Uiso 1 1 calc R U . . .
C3 C 0.7789(3) 1.04764(12) 0.60650(9) 0.0411(7) Uani 1 1 d . . . . .
H3A H 0.7970 1.0785 0.6240 0.049 Uiso 1 1 calc R U . . .
H3B H 0.8453 1.0397 0.5887 0.049 Uiso 1 1 calc R U . . .
C4 C 0.8943(3) 0.92877(12) 0.72029(10) 0.0479(8) Uani 1 1 d . . . . .
C5 C 0.8540(3) 0.88566(14) 0.74381(11) 0.0551(9) Uani 1 1 d . . . . .
H5A H 0.7882 0.8673 0.7352 0.066 Uiso 1 1 calc R U . . .
C6 C 0.9121(3) 0.87036(14) 0.78001(12) 0.0583(9) Uani 1 1 d . . . . .
H6A H 0.8844 0.8419 0.7960 0.070 Uiso 1 1 calc R U . . .
C7 C 1.0125(3) 0.89697(13) 0.79313(10) 0.0506(8) Uani 1 1 d . . . . .
C8 C 1.0495(4) 0.93978(14) 0.76884(11) 0.0573(9) Uani 1 1 d . . . . .
H8A H 1.1149 0.9584 0.7774 0.069 Uiso 1 1 calc R U . . .
C9 C 0.9933(3) 0.95565(14) 0.73260(11) 0.0580(9) Uani 1 1 d . . . . .
H9A H 1.0212 0.9840 0.7165 0.070 Uiso 1 1 calc R U . . .
C10 C 0.6936(3) 1.09241(13) 0.54672(9) 0.0434(7) Uani 1 1 d . . . . .
C11 C 0.7900(3) 1.12427(13) 0.54137(10) 0.0459(7) Uani 1 1 d . . . . .
H11A H 0.8492 1.1242 0.5614 0.055 Uiso 1 1 calc R U . . .
C12 C 0.7965(3) 1.15624(12) 0.50562(10) 0.0470(8) Uani 1 1 d . . . . .
H12A H 0.8610 1.1778 0.5019 0.056 Uiso 1 1 calc R U . . .
C13 C 0.7102(3) 1.15714(13) 0.47529(9) 0.0439(7) Uani 1 1 d . . . . .
C14 C 0.6139(3) 1.12627(16) 0.48204(11) 0.0563(9) Uani 1 1 d . . . . .
H14A H 0.5537 1.1271 0.4625 0.068 Uiso 1 1 calc R U . . .
C15 C 0.6056(3) 1.09401(15) 0.51739(11) 0.0556(9) Uani 1 1 d . . . . .
H15A H 0.5400 1.0732 0.5215 0.067 Uiso 1 1 calc R U . . .
C16 C 0.7217(3) 1.19102(14) 0.43609(10) 0.0532(9) Uani 1 1 d . . . . .
C17 C 1.0741(4) 0.88001(15) 0.83260(12) 0.0623(10) Uani 1 1 d . . . . .
C18 C 0.9201(5) 0.83868(19) 0.92825(16) 0.0841(15) Uani 1 1 d . . . . .
H18A H 0.8463 0.8369 0.9427 0.101 Uiso 1 1 calc R U . . .
H18B H 0.9074 0.8483 0.8987 0.101 Uiso 1 1 calc R U . . .
C19 C 1.0008(5) 0.8783(2) 0.94999(15) 0.0911(16) Uani 1 1 d . . . . .
H19A H 1.0417 0.8996 0.9291 0.109 Uiso 1 1 calc R U . . .
H19B H 0.9577 0.9020 0.9685 0.109 Uiso 1 1 calc R U . . .
C20 C 1.0320(5) 0.79245(18) 0.97483(12) 0.0788(14) Uani 1 1 d . . . . .
H20A H 0.9718 0.7897 0.9962 0.095 Uiso 1 1 calc R U . . .
H20B H 1.0894 0.7651 0.9801 0.095 Uiso 1 1 calc R U . . .
C21 C 1.2055(5) 0.84647(19) 0.96024(13) 0.0842(14) Uani 1 1 d . U . . .
H21A H 1.2499 0.8201 0.9758 0.101 Uiso 1 1 calc R U . . .
H21B H 1.2376 0.8813 0.9667 0.101 Uiso 1 1 calc R U . . .
C22 C 1.3385(4) 0.82567(19) 0.90038(15) 0.0759(12) Uani 1 1 d . . . . .
H22A H 1.3723 0.7978 0.9178 0.091 Uiso 1 1 calc R U . . .
H22B H 1.3850 0.8576 0.9035 0.091 Uiso 1 1 calc R U . . .
C23 C 1.3360(4) 0.80840(18) 0.85408(14) 0.0756(13) Uani 1 1 d . . . . .
H23A H 1.3089 0.8375 0.8364 0.091 Uiso 1 1 calc R U . . .
H23B H 1.4131 0.7987 0.8448 0.091 Uiso 1 1 calc R U . . .
C24 C 1.2311(5) 0.7453(2) 0.80593(12) 0.0845(15) Uani 1 1 d . . . . .
H24A H 1.2118 0.7769 0.7896 0.101 Uiso 1 1 calc R U . . .
H24B H 1.3003 0.7300 0.7936 0.101 Uiso 1 1 calc R U . . .
C25 C 1.0242(6) 0.7267(2) 0.81222(15) 0.0941(18) Uani 1 1 d . . . . .
H25A H 0.9650 0.7064 0.7976 0.113 Uiso 1 1 calc R U . . .
H25B H 1.0165 0.7641 0.8046 0.113 Uiso 1 1 calc R U . . .
C26 C 1.0584(6) 0.66270(17) 0.86263(18) 0.0966(18) Uani 1 1 d . . . . .
H26A H 0.9964 0.6376 0.8573 0.116 Uiso 1 1 calc R U . . .
H26B H 1.0906 0.6558 0.8906 0.116 Uiso 1 1 calc R U . . .
C27 C 1.1503(6) 0.6586(2) 0.82879(17) 0.1037(19) Uani 1 1 d . . . . .
H27A H 1.2264 0.6574 0.8416 0.124 Uiso 1 1 calc R U . . .
H27B H 1.1393 0.6265 0.8119 0.124 Uiso 1 1 calc R U . . .
C28 C 0.8991(5) 0.7286(2) 0.8778(2) 0.0962(18) Uani 1 1 d . . . . .
H28A H 0.8509 0.6974 0.8733 0.115 Uiso 1 1 calc R U . . .
H28B H 0.8628 0.7587 0.8638 0.115 Uiso 1 1 calc R U . . .
C29 C 0.9100(4) 0.7395(2) 0.92458(18) 0.0906(16) Uani 1 1 d . . . . .
H29A H 0.8340 0.7454 0.9367 0.109 Uiso 1 1 calc R U . . .
H29B H 0.9441 0.7088 0.9386 0.109 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.034(3) . ?
Ni1 N6 2.046(3) . ?
Ni1 N3 2.094(4) . ?
Ni1 N2 2.095(4) . ?
Ni1 O2 2.120(2) . ?
Ni1 O4 2.145(2) 7_756 ?
O1 C17 1.262(5) . ?
O2 C17 1.268(4) . ?
O3 C16 1.269(4) . ?
O4 C16 1.265(4) . ?
O4 Ni1 2.145(2) 7_765 ?
O5 C10 1.374(3) . ?
O5 C3 1.439(4) . ?
O6 C4 1.367(4) . ?
O6 C2 1.432(4) . ?
N1 C20 1.441(6) . ?
N1 C21 1.488(7) . ?
N1 C19 1.504(6) . ?
N2 C20 1.471(5) . ?
N2 C18 1.486(5) . ?
N2 C29 1.488(6) . ?
N3 C28 1.485(7) . ?
N3 C25 1.498(6) . ?
N3 C26 1.507(5) . ?
N4 C23 1.497(6) . ?
N4 C24 1.473(5) . ?
N4 H1N 0.9800 . ?
N5 C25 1.442(8) . ?
N5 C24 1.448(7) . ?
N5 C27 1.494(6) . ?
N6 C22 1.477(6) . ?
N6 C21 1.475(5) . ?
N6 H2N 0.9800 . ?
C1 C3 1.519(3) 2_675 ?
C1 C3 1.519(3) . ?
C1 C2 1.517(4) . ?
C1 C2 1.517(4) 2_675 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C9 1.385(5) . ?
C4 C5 1.390(5) . ?
C5 C6 1.376(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.401(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.385(5) . ?
C7 C17 1.493(5) . ?
C8 C9 1.371(5) . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C10 C15 1.375(5) . ?
C10 C11 1.383(4) . ?
C11 C12 1.382(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.381(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.373(5) . ?
C13 C16 1.502(4) . ?
C14 C15 1.377(4) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C18 C19 1.525(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.518(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.507(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.499(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 N6 86.30(14) . . ?
N4 Ni1 N3 93.28(16) . . ?
N6 Ni1 N3 175.99(12) . . ?
N4 Ni1 N2 175.61(12) . . ?
N6 Ni1 N2 94.42(15) . . ?
N3 Ni1 N2 86.31(17) . . ?
N4 Ni1 O2 92.60(12) . . ?
N6 Ni1 O2 88.14(11) . . ?
N3 Ni1 O2 87.90(12) . . ?
N2 Ni1 O2 91.75(12) . . ?
N4 Ni1 O4 88.65(11) . 7_756 ?
N6 Ni1 O4 90.67(11) . 7_756 ?
N3 Ni1 O4 93.31(12) . 7_756 ?
N2 Ni1 O4 87.01(11) . 7_756 ?
O2 Ni1 O4 178.21(10) . 7_756 ?
C17 O2 Ni1 138.2(3) . . ?
C16 O4 Ni1 137.0(2) . 7_765 ?
C10 O5 C3 117.1(2) . . ?
C4 O6 C2 119.0(3) . . ?
C20 N1 C21 114.7(4) . . ?
C20 N1 C19 103.8(4) . . ?
C21 N1 C19 114.9(4) . . ?
C20 N2 C18 100.4(4) . . ?
C20 N2 C29 115.3(4) . . ?
C18 N2 C29 113.9(4) . . ?
C20 N2 Ni1 108.4(3) . . ?
C18 N2 Ni1 115.8(3) . . ?
C29 N2 Ni1 103.4(3) . . ?
C28 N3 C25 115.3(4) . . ?
C28 N3 C26 114.9(4) . . ?
C25 N3 C26 99.3(4) . . ?
C28 N3 Ni1 104.2(3) . . ?
C25 N3 Ni1 108.2(3) . . ?
C26 N3 Ni1 115.2(3) . . ?
C23 N4 C24 114.9(3) . . ?
C23 N4 Ni1 106.3(3) . . ?
C24 N4 Ni1 117.3(3) . . ?
C23 N4 H1N 105.8 . . ?
C24 N4 H1N 105.8 . . ?
Ni1 N4 H1N 105.8 . . ?
C25 N5 C24 115.7(4) . . ?
C25 N5 C27 103.6(5) . . ?
C24 N5 C27 114.4(5) . . ?
C22 N6 C21 114.7(4) . . ?
C22 N6 Ni1 106.1(3) . . ?
C21 N6 Ni1 116.8(3) . . ?
C22 N6 H2N 106.1 . . ?
C21 N6 H2N 106.1 . . ?
Ni1 N6 H2N 106.1 . . ?
C3 C1 C3 109.4(3) 2_675 . ?
C3 C1 C2 111.13(17) 2_675 . ?
C3 C1 C2 107.49(17) . . ?
C3 C1 C2 107.49(17) 2_675 2_675 ?
C3 C1 C2 111.14(17) . 2_675 ?
C2 C1 C2 110.2(3) . 2_675 ?
O6 C2 C1 106.5(3) . . ?
O6 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
O6 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
O5 C3 C1 107.2(2) . . ?
O5 C3 H3A 110.3 . . ?
C1 C3 H3A 110.3 . . ?
O5 C3 H3B 110.3 . . ?
C1 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
O6 C4 C9 124.9(3) . . ?
O6 C4 C5 114.6(3) . . ?
C9 C4 C5 120.5(3) . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C6 117.6(3) . . ?
C8 C7 C17 122.0(3) . . ?
C6 C7 C17 120.4(3) . . ?
C9 C8 C7 122.3(4) . . ?
C9 C8 H8A 118.8 . . ?
C7 C8 H8A 118.8 . . ?
C8 C9 C4 119.0(3) . . ?
C8 C9 H9A 120.5 . . ?
C4 C9 H9A 120.5 . . ?
O5 C10 C15 116.5(3) . . ?
O5 C10 C11 123.5(3) . . ?
C15 C10 C11 120.0(3) . . ?
C12 C11 C10 118.5(3) . . ?
C12 C11 H11A 120.8 . . ?
C10 C11 H11A 120.8 . . ?
C11 C12 C13 122.1(3) . . ?
C11 C12 H12A 118.9 . . ?
C13 C12 H12A 118.9 . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 C16 121.1(3) . . ?
C12 C13 C16 120.7(3) . . ?
C15 C14 C13 120.8(3) . . ?
C15 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C14 C15 C10 120.4(3) . . ?
C14 C15 H15A 119.8 . . ?
C10 C15 H15A 119.8 . . ?
O4 C16 O3 125.1(3) . . ?
O4 C16 C13 117.1(3) . . ?
O3 C16 C13 117.7(3) . . ?
O1 C17 O2 124.9(3) . . ?
O1 C17 C7 119.3(3) . . ?
O2 C17 C7 115.8(4) . . ?
N2 C18 C19 103.2(4) . . ?
N2 C18 H18A 111.1 . . ?
C19 C18 H18A 111.1 . . ?
N2 C18 H18B 111.1 . . ?
C19 C18 H18B 111.1 . . ?
H18A C18 H18B 109.1 . . ?
N1 C19 C18 105.2(4) . . ?
N1 C19 H19A 110.7 . . ?
C18 C19 H19A 110.7 . . ?
N1 C19 H19B 110.7 . . ?
C18 C19 H19B 110.7 . . ?
H19A C19 H19B 108.8 . . ?
N1 C20 N2 104.3(3) . . ?
N1 C20 H20A 110.9 . . ?
N2 C20 H20A 110.9 . . ?
N1 C20 H20B 110.9 . . ?
N2 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
N1 C21 N6 113.9(4) . . ?
N1 C21 H21A 108.8 . . ?
N6 C21 H21A 108.8 . . ?
N1 C21 H21B 108.8 . . ?
N6 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N6 C22 C23 108.5(3) . . ?
N6 C22 H22A 110.0 . . ?
C23 C22 H22A 110.0 . . ?
N6 C22 H22B 110.0 . . ?
C23 C22 H22B 110.0 . . ?
H22A C22 H22B 108.4 . . ?
N4 C23 C22 108.5(3) . . ?
N4 C23 H23A 110.0 . . ?
C22 C23 H23A 110.0 . . ?
N4 C23 H23B 110.0 . . ?
C22 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
N5 C24 N4 114.8(4) . . ?
N5 C24 H24A 108.6 . . ?
N4 C24 H24A 108.6 . . ?
N5 C24 H24B 108.6 . . ?
N4 C24 H24B 108.6 . . ?
H24A C24 H24B 107.5 . . ?
N5 C25 N3 104.3(4) . . ?
N5 C25 H25A 110.9 . . ?
N3 C25 H25A 110.9 . . ?
N5 C25 H25B 110.9 . . ?
N3 C25 H25B 110.9 . . ?
H25A C25 H25B 108.9 . . ?
N3 C26 C27 104.5(4) . . ?
N3 C26 H26A 110.9 . . ?
C27 C26 H26A 110.9 . . ?
N3 C26 H26B 110.9 . . ?
C27 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
N5 C27 C26 106.1(5) . . ?
N5 C27 H27A 110.5 . . ?
C26 C27 H27A 110.5 . . ?
N5 C27 H27B 110.5 . . ?
C26 C27 H27B 110.5 . . ?
H27A C27 H27B 108.7 . . ?
N3 C28 C29 109.5(4) . . ?
N3 C28 H28A 109.8 . . ?
C29 C28 H28A 109.8 . . ?
N3 C28 H28B 109.8 . . ?
C29 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
N2 C29 C28 110.1(4) . . ?
N2 C29 H29A 109.6 . . ?
C28 C29 H29A 109.6 . . ?
N2 C29 H29B 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.2 . . ?

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
C4 O6 C2 C1 -163.8(3) . . . . ?
C3 C1 C2 O6 -55.5(3) 2_675 . . . ?
C3 C1 C2 O6 -175.2(2) . . . . ?
C2 C1 C2 O6 63.6(2) 2_675 . . . ?
C10 O5 C3 C1 -166.8(2) . . . . ?
C3 C1 C3 O5 59.45(17) 2_675 . . . ?
C2 C1 C3 O5 -179.7(2) . . . . ?
C2 C1 C3 O5 -59.1(3) 2_675 . . . ?
C2 O6 C4 C9 -7.8(5) . . . . ?
C2 O6 C4 C5 172.3(3) . . . . ?
O6 C4 C5 C6 -178.9(3) . . . . ?
C9 C4 C5 C6 1.1(6) . . . . ?
C4 C5 C6 C7 -1.1(6) . . . . ?
C5 C6 C7 C8 1.2(6) . . . . ?
C5 C6 C7 C17 179.7(4) . . . . ?
C6 C7 C8 C9 -1.5(6) . . . . ?
C17 C7 C8 C9 -179.9(4) . . . . ?
C7 C8 C9 C4 1.5(6) . . . . ?
O6 C4 C9 C8 178.8(3) . . . . ?
C5 C4 C9 C8 -1.3(6) . . . . ?
C3 O5 C10 C15 167.4(3) . . . . ?
C3 O5 C10 C11 -12.8(4) . . . . ?
O5 C10 C11 C12 178.5(3) . . . . ?
C15 C10 C11 C12 -1.7(5) . . . . ?
C10 C11 C12 C13 -0.2(5) . . . . ?
C11 C12 C13 C14 2.0(5) . . . . ?
C11 C12 C13 C16 -178.0(3) . . . . ?
C12 C13 C14 C15 -2.1(6) . . . . ?
C16 C13 C14 C15 177.9(4) . . . . ?
C13 C14 C15 C10 0.3(6) . . . . ?
O5 C10 C15 C14 -178.6(3) . . . . ?
C11 C10 C15 C14 1.6(6) . . . . ?
Ni1 O4 C16 O3 1.5(6) 7_765 . . . ?
Ni1 O4 C16 C13 179.8(2) 7_765 . . . ?
C14 C13 C16 O4 176.1(3) . . . . ?
C12 C13 C16 O4 -3.9(5) . . . . ?
C14 C13 C16 O3 -5.5(5) . . . . ?
C12 C13 C16 O3 174.5(3) . . . . ?
Ni1 O2 C17 O1 -15.1(7) . . . . ?
Ni1 O2 C17 C7 163.3(3) . . . . ?
C8 C7 C17 O1 14.7(6) . . . . ?
C6 C7 C17 O1 -163.6(4) . . . . ?
C8 C7 C17 O2 -163.8(4) . . . . ?
C6 C7 C17 O2 17.8(6) . . . . ?
C20 N2 C18 C19 39.0(4) . . . . ?
C29 N2 C18 C19 162.9(4) . . . . ?
Ni1 N2 C18 C19 -77.4(4) . . . . ?
C20 N1 C19 C18 -12.7(5) . . . . ?
C21 N1 C19 C18 113.3(5) . . . . ?
N2 C18 C19 N1 -16.7(5) . . . . ?
C21 N1 C20 N2 -88.0(4) . . . . ?
C19 N1 C20 N2 38.2(4) . . . . ?
C18 N2 C20 N1 -48.9(4) . . . . ?
C29 N2 C20 N1 -171.7(4) . . . . ?
Ni1 N2 C20 N1 73.0(4) . . . . ?
C20 N1 C21 N6 69.4(5) . . . . ?
C19 N1 C21 N6 -50.8(5) . . . . ?
C22 N6 C21 N1 -166.7(4) . . . . ?
Ni1 N6 C21 N1 -41.7(4) . . . . ?
C21 N6 C22 C23 172.1(3) . . . . ?
Ni1 N6 C22 C23 41.6(4) . . . . ?
C24 N4 C23 C22 171.0(4) . . . . ?
Ni1 N4 C23 C22 39.5(4) . . . . ?
N6 C22 C23 N4 -55.5(4) . . . . ?
C25 N5 C24 N4 67.8(5) . . . . ?
C27 N5 C24 N4 -52.5(6) . . . . ?
C23 N4 C24 N5 -168.5(4) . . . . ?
Ni1 N4 C24 N5 -42.5(5) . . . . ?
C24 N5 C25 N3 -85.7(5) . . . . ?
C27 N5 C25 N3 40.4(5) . . . . ?
C28 N3 C25 N5 -170.8(4) . . . . ?
C26 N3 C25 N5 -47.5(5) . . . . ?
Ni1 N3 C25 N5 73.0(4) . . . . ?
C28 N3 C26 C27 159.1(4) . . . . ?
C25 N3 C26 C27 35.5(5) . . . . ?
Ni1 N3 C26 C27 -79.8(4) . . . . ?
C25 N5 C27 C26 -16.8(5) . . . . ?
C24 N5 C27 C26 110.1(5) . . . . ?
N3 C26 C27 N5 -12.5(5) . . . . ?
C25 N3 C28 C29 -159.6(4) . . . . ?
C26 N3 C28 C29 85.8(5) . . . . ?
Ni1 N3 C28 C29 -41.2(4) . . . . ?
C20 N2 C29 C28 -161.0(4) . . . . ?
C18 N2 C29 C28 83.7(5) . . . . ?
Ni1 N2 C29 C28 -42.9(4) . . . . ?
N3 C28 C29 N2 59.5(5) . . . . ?

_refine_diff_density_max         0.327
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.053
# start Validation Reply Form
_vrf_CHEMW03_4_sq                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The difference is due to the crystallization solvent
molecules that were removed by using SQUEEZE.
;
_vrf_PLAT051_4_sq                
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       6.28 %     
RESPONSE: The difference is due to the crystallization solvent
molecules that were removed by using SQUEEZE.
;
# end Validation Reply Form


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

data_5_sq
_database_code_depnum_ccdc_archive 'CCDC 1401608'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C59 H80 N12 Ni2 O12,4(C3 H7 N O),9(H2 O)'
_chemical_formula_sum            'C71 H126 N16 Ni2 O25'
_chemical_formula_weight         1721.29

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

_cell_length_a                   11.7659(7)
_cell_length_b                   25.7333(15)
_cell_length_c                   31.1417(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9428.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3240
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      19.10

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             3680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_exptl_absorpt_coefficient_mu    0.473
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38863
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.026
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8768
_reflns_number_gt                3788
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0813P)²+0.6727P] 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         8768
_refine_ls_number_parameters     385
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1970
_refine_ls_wR_factor_gt          0.1803
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.4683(3) 0.32145(12) 0.15392(10) 0.0772(10) Uani 1 1 d . . . . .
C1 C 0.4473(5) 0.3673(2) 0.16471(15) 0.0736(14) Uani 1 1 d . . . . .
O4 O 0.3790(4) 0.39752(13) 0.14597(12) 0.1148(16) Uani 1 1 d . . . . .
Ni1 Ni 0.60377(6) 0.76583(2) 0.61131(2) 0.0691(3) Uani 1 1 d . . . . .
O6 O 0.8120(2) 0.55756(9) 0.41593(8) 0.0490(7) Uani 1 1 d . . . . .
O5 O 0.6823(2) 0.44038(9) 0.31024(9) 0.0593(8) Uani 1 1 d . . . . .
O1 O 0.6729(3) 0.70965(12) 0.56689(9) 0.0674(9) Uani 1 1 d . . . . .
O2 O 0.8410(3) 0.68237(13) 0.59057(11) 0.0847(11) Uani 1 1 d . . . . .
C9 C 0.7500 0.5000 0.36195(15) 0.0347(13) Uani 1 2 d S T P . .
C11 C 0.7946(3) 0.58956(14) 0.45046(12) 0.0407(10) Uani 1 1 d . . . . .
C14 C 0.7744(4) 0.65186(14) 0.52330(12) 0.0484(11) Uani 1 1 d . . . . .
C10 C 0.7169(3) 0.54600(13) 0.38948(11) 0.0405(9) Uani 1 1 d . . . . .
H10A H 0.6981 0.5756 0.3716 0.049 Uiso 1 1 calc R U . . .
H10B H 0.6513 0.5375 0.4070 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6856(4) 0.64817(15) 0.49386(13) 0.0526(11) Uani 1 1 d . . . . .
H15 H 0.6192 0.6670 0.4986 0.063 Uiso 1 1 calc R U . . .
C5 C 0.6198(4) 0.42547(14) 0.27530(13) 0.0492(11) Uani 1 1 d . . . . .
C4 C 0.6606(4) 0.38178(15) 0.25402(14) 0.0594(12) Uani 1 1 d . . . . .
H4 H 0.7259 0.3652 0.2637 0.071 Uiso 1 1 calc R U . . .
C16 C 0.6942(3) 0.61666(14) 0.45736(12) 0.0485(11) Uani 1 1 d . . . . .
H16 H 0.6340 0.6139 0.4381 0.058 Uiso 1 1 calc R U . . .
C8 C 0.6500(3) 0.48567(13) 0.33374(11) 0.0445(11) Uani 1 1 d . . . . .
H8A H 0.5835 0.4786 0.3512 0.053 Uiso 1 1 calc R U . . .
H8B H 0.6323 0.5139 0.3142 0.053 Uiso 1 1 calc R U . . .
C12 C 0.8831(4) 0.59247(16) 0.47936(14) 0.0572(12) Uani 1 1 d . . . . .
H12 H 0.9498 0.5740 0.4744 0.069 Uiso 1 1 calc R U . . .
C13 C 0.8724(4) 0.62295(16) 0.51568(13) 0.0566(12) Uani 1 1 d . . . . .
H13 H 0.9318 0.6242 0.5354 0.068 Uiso 1 1 calc R U . . .
C28 C 0.7617(5) 0.68425(16) 0.56352(14) 0.0597(13) Uani 1 1 d . . . . .
C3 C 0.6040(4) 0.36319(17) 0.21857(14) 0.0619(13) Uani 1 1 d . . . . .
H3 H 0.6306 0.3336 0.2046 0.074 Uiso 1 1 calc R U . . .
C7 C 0.4690(4) 0.43147(15) 0.22443(14) 0.0660(13) Uani 1 1 d . . . . .
H7 H 0.4055 0.4489 0.2141 0.079 Uiso 1 1 calc R U . . .
C6 C 0.5241(4) 0.44928(15) 0.26089(13) 0.0596(13) Uani 1 1 d . . . . .
H6 H 0.4952 0.4778 0.2756 0.072 Uiso 1 1 calc R U . . .
C2 C 0.5084(4) 0.38794(16) 0.20355(13) 0.0605(13) Uani 1 1 d . . . . .
N3 N 0.7437(4) 0.75689(15) 0.64717(11) 0.0760(12) Uani 1 1 d . . . . .
H3A H 0.7844 0.7276 0.6343 0.091 Uiso 1 1 calc R U . . .
N2 N 0.6904(6) 0.82260(16) 0.58190(14) 0.0983(16) Uani 1 1 d . . . . .
H2 H 0.6653 0.8544 0.5964 0.118 Uiso 1 1 calc R U . . .
N4 N 0.5172(5) 0.70949(17) 0.6466(2) 0.1102(19) Uani 1 1 d . . . . .
N5 N 0.4649(5) 0.7703(3) 0.57141(19) 0.139(3) Uani 1 1 d . . . . .
C21 C 0.5306(7) 0.7181(2) 0.6935(2) 0.121(3) Uani 1 1 d . . . . .
H21A H 0.5163 0.7541 0.7009 0.145 Uiso 1 1 calc R U . . .
H21B H 0.4793 0.6961 0.7097 0.145 Uiso 1 1 calc R U . . .
C20 C 0.7309(6) 0.7430(3) 0.69331(17) 0.113(2) Uani 1 1 d . . . . .
H20A H 0.8035 0.7307 0.7040 0.136 Uiso 1 1 calc R U . . .
H20B H 0.7114 0.7742 0.7093 0.136 Uiso 1 1 calc R U . . .
C19 C 0.8176(5) 0.8038(2) 0.6386(2) 0.105(2) Uani 1 1 d . . . . .
H19A H 0.7929 0.8326 0.6563 0.127 Uiso 1 1 calc R U . . .
H19B H 0.8959 0.7959 0.6458 0.127 Uiso 1 1 calc R U . . .
C23 C 0.5698(7) 0.6555(2) 0.6442(3) 0.131(3) Uani 1 1 d . . . . .
H23A H 0.5144 0.6291 0.6515 0.158 Uiso 1 1 calc R U . . .
H23B H 0.5988 0.6486 0.6156 0.158 Uiso 1 1 calc R U . . .
C27 C 0.6684(8) 0.8330(3) 0.5347(2) 0.149(3) Uani 1 1 d . U . . .
H27A H 0.6899 0.8686 0.5282 0.179 Uiso 1 1 calc R U . . .
H27B H 0.7160 0.8102 0.5176 0.179 Uiso 1 1 calc R U . . .
C22 C 0.6635(8) 0.6566(2) 0.6759(3) 0.153(3) Uani 1 1 d . . . . .
H22A H 0.7366 0.6573 0.6615 0.183 Uiso 1 1 calc R U . . .
H22B H 0.6604 0.6261 0.6943 0.183 Uiso 1 1 calc R U . . .
C25 C 0.4007(7) 0.7230(4) 0.5810(4) 0.195(6) Uani 1 1 d . . . . .
H25A H 0.4328 0.6939 0.5654 0.234 Uiso 1 1 calc R U . . .
H25B H 0.3223 0.7272 0.5721 0.234 Uiso 1 1 calc R U . . .
C26 C 0.4995(8) 0.7746(3) 0.5268(2) 0.162(3) Uani 1 1 d . U . . .
H26A H 0.4341 0.7721 0.5080 0.195 Uiso 1 1 calc R U . . .
H26B H 0.5527 0.7473 0.5195 0.195 Uiso 1 1 calc R U . . .
C24 C 0.4066(8) 0.7117(3) 0.6337(3) 0.170(4) Uani 1 1 d . . . . .
H24A H 0.3675 0.7392 0.6490 0.204 Uiso 1 1 calc R U . . .
H24B H 0.3690 0.6791 0.6402 0.204 Uiso 1 1 calc R U . . .
C18 C 0.8095(8) 0.8178(2) 0.5935(3) 0.115(3) Uani 1 1 d . . . . .
H18 H 0.8398 0.7884 0.5771 0.138 Uiso 1 1 calc R U . . .
C17 C 0.8752(8) 0.8650(3) 0.5797(3) 0.204(4) Uani 1 1 d . U . . .
H17A H 0.8399 0.8801 0.5549 0.306 Uiso 1 1 calc R U . . .
H17B H 0.9518 0.8552 0.5729 0.306 Uiso 1 1 calc R U . . .
H17C H 0.8760 0.8900 0.6026 0.306 Uiso 1 1 calc R U . . .
N6 N 0.6469(7) 0.7044(2) 0.70149(17) 0.119(2) Uani 1 1 d . U . . .
N1 N 0.5530(8) 0.8254(3) 0.5229(2) 0.157(3) Uani 1 1 d . U . . .
C29 C 0.3932(7) 0.8190(3) 0.5736(3) 0.158(3) Uani 1 1 d . U . . .
H29A H 0.3210 0.8144 0.5590 0.190 Uiso 1 1 calc R U . . .
H29B H 0.3796 0.8296 0.6030 0.190 Uiso 1 1 calc R U . . .
C30 C 0.4662(7) 0.8562(3) 0.5509(2) 0.157(3) Uani 1 1 d . U . . .
H30A H 0.5064 0.8777 0.5715 0.189 Uiso 1 1 calc R U . . .
H30B H 0.4204 0.8786 0.5328 0.189 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C1 1.252(5) . ?
O3 Ni1 2.128(3) 8_655 ?
C1 O4 1.261(5) . ?
C1 C2 1.503(6) . ?
Ni1 N3 2.003(4) . ?
Ni1 N2 2.003(5) . ?
Ni1 N5 2.056(5) . ?
Ni1 N4 2.085(5) . ?
Ni1 O3 2.128(3) 8_666 ?
Ni1 O1 2.160(3) . ?
O6 C11 1.370(4) . ?
O6 C10 1.421(4) . ?
O5 C5 1.368(4) . ?
O5 C8 1.427(4) . ?
O1 C28 1.237(5) . ?
O2 C28 1.259(5) . ?
C9 C10 1.513(4) . ?
C9 C10 1.513(4) 2_665 ?
C9 C8 1.513(4) 2_665 ?
C9 C8 1.514(4) . ?
C11 C12 1.378(5) . ?
C11 C16 1.389(5) . ?
C14 C15 1.393(5) . ?
C14 C13 1.393(5) . ?
C14 C28 1.512(5) . ?
C15 C16 1.400(5) . ?
C5 C6 1.358(5) . ?
C5 C4 1.391(5) . ?
C4 C3 1.375(5) . ?
C12 C13 1.382(5) . ?
C3 C2 1.375(6) . ?
C7 C2 1.376(5) . ?
C7 C6 1.385(5) . ?
N3 C20 1.488(6) . ?
N3 C19 1.510(6) . ?
N2 C18 1.452(8) . ?
N2 C27 1.516(8) . ?
N4 C24 1.363(9) . ?
N4 C21 1.484(7) . ?
N4 C23 1.522(7) . ?
N5 C26 1.451(9) . ?
N5 C25 1.463(11) . ?
N5 C29 1.511(8) . ?
C21 N6 1.435(8) . ?
C20 N6 1.425(7) . ?
C19 C18 1.452(8) . ?
C23 C22 1.482(10) . ?
C27 N1 1.421(9) . ?
C22 N6 1.479(8) . ?
C25 C24 1.668(13) . ?
C26 N1 1.457(10) . ?
C18 C17 1.503(8) . ?
N1 C30 1.559(9) . ?
C29 C30 1.467(10) . ?

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
C1 O3 Ni1 136.3(3) . 8_655 ?
O3 C1 O4 125.7(4) . . ?
O3 C1 C2 117.0(5) . . ?
O4 C1 C2 117.3(4) . . ?
N3 Ni1 N2 85.4(2) . . ?
N3 Ni1 N5 175.41(17) . . ?
N2 Ni1 N5 95.0(3) . . ?
N3 Ni1 N4 91.6(2) . . ?
N2 Ni1 N4 175.4(2) . . ?
N5 Ni1 N4 88.2(3) . . ?
N3 Ni1 O3 93.28(14) . 8_666 ?
N2 Ni1 O3 89.86(15) . 8_666 ?
N5 Ni1 O3 91.29(16) . 8_666 ?
N4 Ni1 O3 86.80(15) . 8_666 ?
N3 Ni1 O1 88.32(13) . . ?
N2 Ni1 O1 90.22(15) . . ?
N5 Ni1 O1 87.11(15) . . ?
N4 Ni1 O1 93.21(15) . . ?
O3 Ni1 O1 178.40(13) 8_666 . ?
C11 O6 C10 117.6(3) . . ?
C5 O5 C8 119.6(3) . . ?
C28 O1 Ni1 136.6(3) . . ?
C10 C9 C10 111.0(4) . 2_665 ?
C10 C9 C8 109.78(19) . 2_665 ?
C10 C9 C8 108.62(19) 2_665 2_665 ?
C10 C9 C8 108.62(19) . . ?
C10 C9 C8 109.78(19) 2_665 . ?
C8 C9 C8 109.1(4) 2_665 . ?
C12 C11 O6 115.6(3) . . ?
C12 C11 C16 120.9(3) . . ?
O6 C11 C16 123.4(4) . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 C28 120.6(4) . . ?
C13 C14 C28 121.2(4) . . ?
O6 C10 C9 106.8(3) . . ?
C14 C15 C16 121.3(4) . . ?
C6 C5 O5 125.6(3) . . ?
C6 C5 C4 119.6(4) . . ?
O5 C5 C4 114.8(4) . . ?
C3 C4 C5 119.8(4) . . ?
C11 C16 C15 118.6(4) . . ?
O5 C8 C9 106.9(3) . . ?
C11 C12 C13 119.8(4) . . ?
C12 C13 C14 121.2(4) . . ?
O1 C28 O2 126.2(4) . . ?
O1 C28 C14 116.4(4) . . ?
O2 C28 C14 117.4(4) . . ?
C2 C3 C4 120.5(4) . . ?
C2 C7 C6 120.0(4) . . ?
C5 C6 C7 120.6(4) . . ?
C3 C2 C7 119.5(4) . . ?
C3 C2 C1 120.1(4) . . ?
C7 C2 C1 120.5(5) . . ?
C20 N3 C19 114.9(4) . . ?
C20 N3 Ni1 118.8(4) . . ?
C19 N3 Ni1 106.4(3) . . ?
C18 N2 C27 114.9(6) . . ?
C18 N2 Ni1 108.4(4) . . ?
C27 N2 Ni1 119.1(5) . . ?
C24 N4 C21 112.6(7) . . ?
C24 N4 C23 114.3(5) . . ?
C21 N4 C23 98.2(6) . . ?
C24 N4 Ni1 106.4(6) . . ?
C21 N4 Ni1 111.3(4) . . ?
C23 N4 Ni1 114.2(4) . . ?
C26 N5 C25 113.8(7) . . ?
C26 N5 C29 97.8(6) . . ?
C25 N5 C29 113.1(7) . . ?
C26 N5 Ni1 111.1(5) . . ?
C25 N5 Ni1 103.9(5) . . ?
C29 N5 Ni1 117.6(4) . . ?
N6 C21 N4 103.6(5) . . ?
N6 C20 N3 114.2(5) . . ?
C18 C19 N3 109.4(5) . . ?
C22 C23 N4 104.6(5) . . ?
N1 C27 N2 113.0(7) . . ?
C23 C22 N6 106.0(7) . . ?
N5 C25 C24 109.0(6) . . ?
N5 C26 N1 105.7(6) . . ?
N4 C24 C25 109.7(8) . . ?
N2 C18 C19 109.0(6) . . ?
N2 C18 C17 110.9(7) . . ?
C19 C18 C17 116.4(7) . . ?
C21 N6 C20 117.3(6) . . ?
C21 N6 C22 103.7(7) . . ?
C20 N6 C22 113.1(6) . . ?
C27 N1 C26 121.0(7) . . ?
C27 N1 C30 114.2(7) . . ?
C26 N1 C30 97.2(8) . . ?
C30 C29 N5 101.1(7) . . ?
C29 C30 N1 108.8(7) . . ?

_refine_diff_density_max         0.444
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.052
# start Validation Reply Form
_vrf_CHEMW03_5_sq                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE:The difference is due to the crystallization solvent
molecules that were removed by using SQUEEZE.
;
# end Validation Reply Form


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

data_6
_database_code_depnum_ccdc_archive 'CCDC 1401609'
_audit_update_record             
;
2015-10-14 deposited with the CCDC.
2015-11-13 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         'C61 H84 N12 Ni2 O12,20(H2 O)'
_chemical_formula_sum            'C61 H124 N12 Ni2 O32'
_chemical_formula_weight         1655.13

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

_cell_length_a                   11.817(2)
_cell_length_b                   24.760(5)
_cell_length_c                   32.256(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9438(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    27733
_cell_measurement_theta_min      2.0738
_cell_measurement_theta_max      29.1226

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             3544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.48
_exptl_absorpt_coefficient_mu    0.474
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7782
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            50366
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.011
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8290
_reflns_number_gt                5343
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1919P)²+20.5474P] 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         8290
_refine_ls_number_parameters     369
_refine_ls_number_restraints     386
_refine_ls_R_factor_all          0.1482
_refine_ls_R_factor_gt           0.1202
_refine_ls_wR_factor_ref         0.3528
_refine_ls_wR_factor_gt          0.3256
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.976
_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
O1 O -0.0040(5) 1.16958(17) 0.15347(14) 0.0783(11) Uani 1 1 d . . . . .
C1 C -0.0239(7) 1.1227(3) 0.1658(2) 0.0783(11) Uani 1 1 d . U . . .
O2 O -0.0921(8) 1.0891(2) 0.1478(2) 0.136(3) Uani 1 1 d . . . . .
Ni1 Ni 0.08192(9) 0.72399(3) 0.61150(2) 0.0712(4) Uani 1 1 d . . . . .
C9 C 0.2500 1.0000 0.3674(2) 0.0432(14) Uani 1 2 d S TU P . .
C11 C 0.2846(5) 0.90505(19) 0.45496(15) 0.0490(7) Uani 1 1 d . U . . .
C5 C 0.1332(6) 1.0721(2) 0.27953(16) 0.0575(13) Uani 1 1 d . U . . .
C10 C 0.2160(4) 0.95228(19) 0.39629(14) 0.0439(11) Uani 1 1 d . U . . .
H10A H 0.1508 0.9623 0.4129 0.053 Uiso 1 1 calc R U . . .
H10B H 0.1959 0.9210 0.3797 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2683(5) 0.8373(2) 0.52415(16) 0.0551(12) Uani 1 1 d . U . . .
C3 C 0.1241(6) 1.1337(2) 0.22234(17) 0.0639(14) Uani 1 1 d . U . . .
H3 H 0.1493 1.1650 0.2093 0.077 Uiso 1 1 calc R U . . .
C15 C 0.1769(5) 0.8429(2) 0.49539(15) 0.0500(11) Uani 1 1 d . U . . .
H15 H 0.1093 0.8246 0.5000 0.060 Uiso 1 1 calc R U . . .
C12 C 0.3773(5) 0.89824(19) 0.48311(14) 0.0490(7) Uani 1 1 d . U . . .
H12 H 0.4448 0.9167 0.4787 0.059 Uiso 1 1 calc R U . . .
C4 C 0.1757(5) 1.1169(2) 0.25835(16) 0.0582(13) Uani 1 1 d . U . . .
H4 H 0.2386 1.1352 0.2685 0.070 Uiso 1 1 calc R U . . .
C13 C 0.3665(6) 0.8645(2) 0.51641(16) 0.0590(13) Uani 1 1 d . U . . .
H13 H 0.4276 0.8600 0.5343 0.071 Uiso 1 1 calc R U . . .
C8 C 0.1524(5) 1.0153(2) 0.34013(15) 0.0519(12) Uani 1 1 d . U . . .
H8A H 0.1334 0.9856 0.3218 0.062 Uiso 1 1 calc R U . . .
H8B H 0.0865 1.0237 0.3569 0.062 Uiso 1 1 calc R U . . .
C2 C 0.0330(7) 1.1042(2) 0.20493(19) 0.0707(15) Uani 1 1 d . U . . .
C6 C 0.0422(7) 1.0437(3) 0.26365(19) 0.0728(16) Uani 1 1 d . U . . .
H6 H 0.0159 1.0134 0.2776 0.087 Uiso 1 1 calc R U . . .
C17 C 0.2561(6) 0.8010(2) 0.56086(18) 0.0669(9) Uani 1 1 d . U . . .
C16 C 0.1882(5) 0.87520(19) 0.46086(15) 0.0490(7) Uani 1 1 d . U . . .
H16 H 0.1301 0.8768 0.4414 0.059 Uiso 1 1 calc R U . . .
C7 C -0.0097(7) 1.0594(3) 0.2278(2) 0.0751(16) Uani 1 1 d . U . . .
H7 H -0.0730 1.0409 0.2183 0.090 Uiso 1 1 calc R U . . .
O4 O 0.1852(4) 1.06113(14) 0.31673(11) 0.0611(10) Uani 1 1 d . . . . .
O3 O 0.3085(4) 0.93962(14) 0.42247(11) 0.0558(9) Uani 1 1 d . . . . .
N2 N 0.2240(6) 0.7286(2) 0.64667(15) 0.0788(16) Uani 1 1 d . . . . .
H2 H 0.2689 0.7589 0.6361 0.095 Uiso 1 1 calc R U . . .
N6 N -0.0010(6) 0.7884(2) 0.6441(2) 0.0860(18) Uani 1 1 d . . . . .
N3 N 0.1647(8) 0.6603(3) 0.5794(2) 0.114(2) Uani 1 1 d D U . . .
H3A H 0.1351 0.6271 0.5919 0.137 Uiso 1 1 calc R U . . .
N5 N -0.0694(8) 0.7191(3) 0.5748(2) 0.111(3) Uani 1 1 d D . . . .
N1 N 0.1295(8) 0.7840(3) 0.7006(2) 0.101(2) Uani 1 1 d . . . . .
N4 N 0.0203(11) 0.6756(5) 0.5201(3) 0.162(4) Uani 1 1 d D U . . .
C21 C 0.0150(8) 0.7781(3) 0.6884(3) 0.092(2) Uani 1 1 d . U . . .
H21A H -0.0314 0.8031 0.7042 0.110 Uiso 1 1 calc R U . . .
H21B H -0.0101 0.7418 0.6948 0.110 Uiso 1 1 calc R U . . .
C25 C 0.1286(12) 0.6578(6) 0.5339(3) 0.155(4) Uani 1 1 d D U . . .
H25A H 0.1843 0.6781 0.5182 0.186 Uiso 1 1 calc R U . . .
H25B H 0.1360 0.6204 0.5253 0.186 Uiso 1 1 calc R U . . .
C31 C -0.1216(9) 0.7812(4) 0.6306(3) 0.112(3) Uani 1 1 d . U . . .
H31A H -0.1645 0.8137 0.6364 0.134 Uiso 1 1 calc R U . . .
H31B H -0.1559 0.7515 0.6456 0.134 Uiso 1 1 calc R U . . .
C18 C 0.0360(9) 0.8459(3) 0.6335(3) 0.102(2) Uani 1 1 d . U . . .
H18A H -0.0170 0.8716 0.6452 0.123 Uiso 1 1 calc R U . . .
H18B H 0.0367 0.8506 0.6036 0.123 Uiso 1 1 calc R U . . .
C22 C 0.2015(8) 0.7397(4) 0.6933(2) 0.097(2) Uani 1 1 d . U . . .
H22A H 0.1682 0.7077 0.7056 0.116 Uiso 1 1 calc R U . . .
H22B H 0.2733 0.7463 0.7070 0.116 Uiso 1 1 calc R U . . .
C19 C 0.1554(9) 0.8562(4) 0.6511(3) 0.110(2) Uani 1 1 d . U . . .
H19A H 0.2095 0.8377 0.6335 0.132 Uiso 1 1 calc R U . . .
H19B H 0.1709 0.8946 0.6490 0.132 Uiso 1 1 calc R U . . .
C30 C -0.1230(11) 0.7693(4) 0.5833(4) 0.123(3) Uani 1 1 d . U . . .
H30A H -0.2005 0.7682 0.5735 0.148 Uiso 1 1 calc R U . . .
H30B H -0.0839 0.7980 0.5686 0.148 Uiso 1 1 calc R U . . .
C29 C -0.0448(12) 0.7215(5) 0.5310(3) 0.150(5) Uani 1 1 d D U . . .
H29A H -0.1147 0.7219 0.5152 0.180 Uiso 1 1 calc R U . . .
H29B H -0.0030 0.7542 0.5246 0.180 Uiso 1 1 calc R U . . .
C20 C 0.1774(11) 0.8390(4) 0.6956(3) 0.124(3) Uani 1 1 d . U . . .
H20A H 0.2581 0.8387 0.7012 0.149 Uiso 1 1 calc R U . . .
H20B H 0.1414 0.8639 0.7147 0.149 Uiso 1 1 calc R U . . .
C24 C 0.2857(10) 0.6635(4) 0.5936(3) 0.119(3) Uani 1 1 d . U . . .
H24A H 0.3257 0.6903 0.5773 0.142 Uiso 1 1 calc R U . . .
H24B H 0.3222 0.6289 0.5893 0.142 Uiso 1 1 calc R U . . .
C23 C 0.2914(9) 0.6789(4) 0.6403(3) 0.108(3) Uani 1 1 d . U . . .
H23A H 0.2611 0.6497 0.6571 0.129 Uiso 1 1 calc R U . . .
H23B H 0.3693 0.6850 0.6484 0.129 Uiso 1 1 calc R U . . .
O6 O 0.1565(4) 0.78072(16) 0.56751(12) 0.0669(9) Uani 1 1 d . U . . .
O5 O 0.3406(5) 0.7936(2) 0.58307(15) 0.0879(15) Uani 1 1 d . . . . .
C27 C -0.1164(11) 0.6229(5) 0.5669(3) 0.141(3) Uani 1 1 d D U . . .
H27A H -0.1757 0.5959 0.5684 0.170 Uiso 1 1 calc R U . . .
H27B H -0.0556 0.6118 0.5852 0.170 Uiso 1 1 calc R U . . .
C28 C -0.1597(10) 0.6739(4) 0.5801(3) 0.127(3) Uani 1 1 d D U . . .
H28A H -0.1821 0.6716 0.6090 0.153 Uiso 1 1 calc R U . . .
H28B H -0.2263 0.6828 0.5639 0.153 Uiso 1 1 calc R U . . .
C26 C -0.0736(12) 0.6263(5) 0.5241(3) 0.151(4) Uani 1 1 d D U . . .
H26A H -0.1361 0.6331 0.5053 0.181 Uiso 1 1 calc R U . . .
H26B H -0.0389 0.5923 0.5163 0.181 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.248(8) . ?
O1 Ni1 2.120(4) 8_565 ?
C1 O2 1.296(9) . ?
C1 C2 1.502(9) . ?
Ni1 N2 2.030(6) . ?
Ni1 O1 2.120(4) 8_556 ?
Ni1 N3 2.124(7) . ?
Ni1 N6 2.147(6) . ?
Ni1 N5 2.147(9) . ?
Ni1 O6 2.183(4) . ?
C9 C8 1.500(7) 2_575 ?
C9 C8 1.501(7) . ?
C9 C10 1.557(6) 2_575 ?
C9 C10 1.557(6) . ?
C11 C16 1.372(8) . ?
C11 O3 1.382(6) . ?
C11 C12 1.433(7) . ?
C5 O4 1.376(6) . ?
C5 C6 1.382(9) . ?
C5 C4 1.397(8) . ?
C10 O3 1.416(6) . ?
C14 C13 1.365(9) . ?
C14 C15 1.431(8) . ?
C14 C17 1.495(8) . ?
C3 C4 1.377(8) . ?
C3 C2 1.416(9) . ?
C15 C16 1.378(7) . ?
C12 C13 1.366(7) . ?
C8 O4 1.417(6) . ?
C2 C7 1.425(9) . ?
C6 C7 1.366(9) . ?
C17 O5 1.243(8) . ?
C17 O6 1.297(8) . ?
N2 C23 1.481(10) . ?
N2 C22 1.552(9) . ?
N6 C21 1.464(10) . ?
N6 C31 1.500(13) . ?
N6 C18 1.528(10) . ?
N3 C24 1.502(14) . ?
N3 C25 1.532(8) . ?
N5 C30 1.420(12) . ?
N5 C29 1.446(8) . ?
N5 C28 1.557(13) . ?
N1 C22 1.409(11) . ?
N1 C21 1.417(12) . ?
N1 C20 1.484(12) . ?
N4 C29 1.417(9) . ?
N4 C25 1.424(9) . ?
N4 C26 1.654(16) . ?
C31 C30 1.555(15) . ?
C18 C19 1.543(14) . ?
C19 C20 1.519(13) . ?
C24 C23 1.555(13) . ?
C27 C28 1.428(8) . ?
C27 C26 1.473(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 Ni1 135.4(5) . 8_565 ?
O1 C1 O2 124.9(6) . . ?
O1 C1 C2 117.8(6) . . ?
O2 C1 C2 117.3(6) . . ?
N2 Ni1 O1 92.2(2) . 8_556 ?
N2 Ni1 N3 86.1(3) . . ?
O1 Ni1 N3 92.3(2) 8_556 . ?
N2 Ni1 N6 93.6(3) . . ?
O1 Ni1 N6 87.8(2) 8_556 . ?
N3 Ni1 N6 179.7(4) . . ?
N2 Ni1 N5 179.4(3) . . ?
O1 Ni1 N5 87.4(2) 8_556 . ?
N3 Ni1 N5 94.2(4) . . ?
N6 Ni1 N5 86.1(3) . . ?
N2 Ni1 O6 89.6(2) . . ?
O1 Ni1 O6 178.1(2) 8_556 . ?
N3 Ni1 O6 88.6(2) . . ?
N6 Ni1 O6 91.4(2) . . ?
N5 Ni1 O6 90.8(2) . . ?
C8 C9 C8 108.1(6) 2_575 . ?
C8 C9 C10 110.1(3) 2_575 2_575 ?
C8 C9 C10 111.0(3) . 2_575 ?
C8 C9 C10 110.9(3) 2_575 . ?
C8 C9 C10 110.1(3) . . ?
C10 C9 C10 106.6(5) 2_575 . ?
C16 C11 O3 127.4(5) . . ?
C16 C11 C12 119.0(4) . . ?
O3 C11 C12 113.4(5) . . ?
O4 C5 C6 124.8(5) . . ?
O4 C5 C4 115.0(5) . . ?
C6 C5 C4 120.1(5) . . ?
O3 C10 C9 109.0(4) . . ?
C13 C14 C15 118.4(5) . . ?
C13 C14 C17 121.6(5) . . ?
C15 C14 C17 119.9(5) . . ?
C4 C3 C2 121.0(6) . . ?
C16 C15 C14 120.4(5) . . ?
C13 C12 C11 119.9(5) . . ?
C3 C4 C5 119.6(6) . . ?
C14 C13 C12 121.6(6) . . ?
O4 C8 C9 107.7(4) . . ?
C3 C2 C7 117.8(6) . . ?
C3 C2 C1 121.1(6) . . ?
C7 C2 C1 120.9(6) . . ?
C7 C6 C5 121.3(6) . . ?
O5 C17 O6 125.3(6) . . ?
O5 C17 C14 117.8(6) . . ?
O6 C17 C14 116.8(6) . . ?
C11 C16 C15 120.4(5) . . ?
C6 C7 C2 120.0(7) . . ?
C5 O4 C8 120.0(4) . . ?
C11 O3 C10 115.6(4) . . ?
C23 N2 C22 112.0(6) . . ?
C23 N2 Ni1 108.7(5) . . ?
C22 N2 Ni1 114.2(5) . . ?
C21 N6 C31 112.7(7) . . ?
C21 N6 C18 110.1(7) . . ?
C31 N6 C18 108.5(7) . . ?
C21 N6 Ni1 106.9(5) . . ?
C31 N6 Ni1 101.7(5) . . ?
C18 N6 Ni1 116.8(5) . . ?
C24 N3 C25 124.0(8) . . ?
C24 N3 Ni1 104.6(6) . . ?
C25 N3 Ni1 111.7(7) . . ?
C30 N5 C29 104.0(8) . . ?
C30 N5 C28 107.6(9) . . ?
C29 N5 C28 105.8(9) . . ?
C30 N5 Ni1 102.5(7) . . ?
C29 N5 Ni1 111.7(8) . . ?
C28 N5 Ni1 123.5(6) . . ?
C22 N1 C21 116.8(7) . . ?
C22 N1 C20 117.7(9) . . ?
C21 N1 C20 115.4(8) . . ?
C29 N4 C25 131.2(12) . . ?
C29 N4 C26 102.0(11) . . ?
C25 N4 C26 110.6(11) . . ?
N1 C21 N6 112.1(7) . . ?
N4 C25 N3 122.5(10) . . ?
N6 C31 C30 108.5(8) . . ?
N6 C18 C19 109.5(7) . . ?
N1 C22 N2 113.8(7) . . ?
C20 C19 C18 117.3(9) . . ?
N5 C30 C31 110.4(8) . . ?
N4 C29 N5 108.6(9) . . ?
N1 C20 C19 107.1(9) . . ?
N3 C24 C23 110.4(8) . . ?
N2 C23 C24 108.4(7) . . ?
C17 O6 Ni1 136.3(4) . . ?
C28 C27 C26 110.5(11) . . ?
C27 C28 N5 111.0(10) . . ?
C27 C26 N4 110.3(10) . . ?

_refine_diff_density_max         1.074
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.099
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.032 -0.008 -0.001 4751 1470 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_6                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The difference is due to the crystallization solvent
molecules that were removed by using SQUEEZE.
;
_vrf_RFACR01_6                   
;
PROBLEM: The value of the weighted R factor is > 0.35
RESPONSE: Due to the low resolution and extensive disorder of
macrocyclic ligand.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1401610'
_audit_update_record             
;
2015-10-14 deposited with the CCDC.
2015-11-13 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         'C63 H88 N12 Ni2 O12,18(H2 O)'
_chemical_formula_sum            'C63 H124 N12 Ni2 O30'
_chemical_formula_weight         1647.15

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

_cell_length_a                   12.0122(8)
_cell_length_b                   25.0230(18)
_cell_length_c                   31.873(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9580.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3424
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      19.82

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_F_000             3528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.48
_exptl_absorpt_coefficient_mu    0.466
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35003
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.035
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8506
_reflns_number_gt                4225
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1448P)²+0.2500P] 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         8506
_refine_ls_number_parameters     397
_refine_ls_number_restraints     397
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0794
_refine_ls_wR_factor_ref         0.2592
_refine_ls_wR_factor_gt          0.2384
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.0113(3) 0.32337(15) 0.15556(11) 0.0664(12) Uani 1 1 d . . . . .
C1 C -0.0304(5) 0.3712(2) 0.16714(16) 0.0556(14) Uani 1 1 d . U . . .
O1 O -0.0956(4) 0.40161(16) 0.14884(12) 0.0761(13) Uani 1 1 d . . . . .
Ni1 Ni 0.08646(6) 0.76829(3) 0.61275(2) 0.0550(3) Uani 1 1 d . U . . .
C11 C 0.2838(4) 0.59328(17) 0.45286(12) 0.0329(10) Uani 1 1 d . U . . .
C9 C 0.2500 0.5000 0.36531(16) 0.0279(13) Uani 1 2 d S TU P . .
C14 C 0.2621(4) 0.65827(19) 0.52323(13) 0.0376(10) Uani 1 1 d . U . . .
C16 C 0.3725(4) 0.59881(19) 0.48023(13) 0.0399(11) Uani 1 1 d . U . . .
H16 H 0.4388 0.5806 0.4753 0.048 Uiso 1 1 calc R U . . .
C10 C 0.2126(4) 0.54607(18) 0.39343(12) 0.0335(10) Uani 1 1 d . U . . .
H10A H 0.1903 0.5764 0.3765 0.040 Uiso 1 1 calc R U . . .
H10B H 0.1497 0.5352 0.4105 0.040 Uiso 1 1 calc R U . . .
C12 C 0.1857(4) 0.61900(19) 0.45975(14) 0.0420(11) Uani 1 1 d . U . . .
H12 H 0.1266 0.6146 0.4412 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1552(4) 0.48417(18) 0.33801(13) 0.0384(11) Uani 1 1 d . U . . .
H8A H 0.0913 0.4747 0.3551 0.046 Uiso 1 1 calc R U . . .
H8B H 0.1345 0.5136 0.3199 0.046 Uiso 1 1 calc R U . . .
C13 C 0.1745(4) 0.6521(2) 0.49491(14) 0.0417(11) Uani 1 1 d . U . . .
H13 H 0.1080 0.6702 0.4994 0.050 Uiso 1 1 calc R U . . .
C5 C 0.1349(4) 0.42628(19) 0.27784(14) 0.0397(11) Uani 1 1 d . U . . .
C15 C 0.3619(4) 0.63168(19) 0.51497(14) 0.0414(11) Uani 1 1 d . U . . .
H15 H 0.4220 0.6361 0.5330 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1722(4) 0.38168(19) 0.25689(14) 0.0463(12) Uani 1 1 d . U . . .
H4 H 0.2344 0.3636 0.2669 0.056 Uiso 1 1 calc R U . . .
C2 C 0.0287(4) 0.3893(2) 0.20478(14) 0.0449(11) Uani 1 1 d . U . . .
C7 C -0.0062(4) 0.4361(2) 0.22512(15) 0.0550(13) Uani 1 1 d . U . . .
H7 H -0.0644 0.4559 0.2137 0.066 Uiso 1 1 calc R U . . .
C3 C 0.1199(4) 0.3635(2) 0.22169(16) 0.0493(12) Uani 1 1 d . U . . .
H3 H 0.1463 0.3327 0.2087 0.059 Uiso 1 1 calc R U . . .
C17 C 0.2506(5) 0.6929(2) 0.56066(14) 0.0452(12) Uani 1 1 d . U . . .
C6 C 0.0440(5) 0.4539(2) 0.26202(16) 0.0538(13) Uani 1 1 d . U . . .
H6 H 0.0168 0.4839 0.2759 0.065 Uiso 1 1 calc R U . . .
O4 O 0.3039(3) 0.56008(13) 0.41942(9) 0.0424(8) Uani 1 1 d . . . . .
O5 O 0.1567(3) 0.71192(16) 0.56844(11) 0.0601(11) Uani 1 1 d . . . . .
O3 O 0.1898(3) 0.43864(12) 0.31303(9) 0.0467(9) Uani 1 1 d . . . . .
N1 N 0.1616(4) 0.82864(18) 0.58110(13) 0.0614(13) Uani 1 1 d . . . . .
H1 H 0.1291 0.8621 0.5915 0.074 Uiso 1 1 calc R U . . .
N2 N 0.2273(4) 0.76416(19) 0.64721(13) 0.0611(13) Uani 1 1 d . . . . .
H2 H 0.2721 0.7347 0.6360 0.073 Uiso 1 1 calc R U . . .
N4 N 0.0096(6) 0.7054(2) 0.6458(2) 0.099(2) Uani 1 1 d . U . . .
N5 N -0.0598(5) 0.7741(3) 0.5760(2) 0.1044(15) Uani 1 1 d D U . . .
N6 N 0.0285(7) 0.8217(4) 0.52052(18) 0.125(3) Uani 1 1 d D . . . .
C20 C 0.2890(5) 0.8148(3) 0.63854(19) 0.0658(16) Uani 1 1 d . U . . .
H20A H 0.2576 0.8436 0.6551 0.079 Uiso 1 1 calc R U . . .
H20B H 0.3665 0.8107 0.6465 0.079 Uiso 1 1 calc R U . . .
C19 C 0.2818(5) 0.8278(3) 0.5952(2) 0.0698(17) Uani 1 1 d . U . . .
H19 H 0.3216 0.8005 0.5791 0.084 Uiso 1 1 calc R U . . .
C30 C -0.0272(9) 0.7758(5) 0.5315(3) 0.140(4) Uani 1 1 d D U . . .
H30A H 0.0200 0.7453 0.5255 0.168 Uiso 1 1 calc R U . . .
H30B H -0.0935 0.7727 0.5143 0.168 Uiso 1 1 calc R U . . .
C32 C -0.1165(6) 0.7211(3) 0.5900(3) 0.1044(15) Uani 1 1 d . U . . .
H32A H -0.1953 0.7228 0.5835 0.125 Uiso 1 1 calc R U . . .
H32B H -0.0849 0.6916 0.5742 0.125 Uiso 1 1 calc R U . . .
C29 C -0.0409(9) 0.8692(5) 0.5270(3) 0.161(3) Uani 1 1 d . U . . .
H29A H -0.0980 0.8704 0.5055 0.193 Uiso 1 1 calc R U . . .
H29B H 0.0049 0.9009 0.5240 0.193 Uiso 1 1 calc R U . . .
C31 C 0.1407(7) 0.8268(3) 0.5350(2) 0.097(2) Uani 1 1 d . U . . .
H31A H 0.1713 0.8592 0.5229 0.117 Uiso 1 1 calc R U . . .
H31B H 0.1829 0.7971 0.5237 0.117 Uiso 1 1 calc R U . . .
C27 C -0.1368(7) 0.8182(4) 0.5824(3) 0.117(3) Uani 1 1 d . U . . .
H27A H -0.2044 0.8109 0.5668 0.140 Uiso 1 1 calc R U . . .
H27B H -0.1566 0.8194 0.6119 0.140 Uiso 1 1 calc R U . . .
C26 C -0.1023(7) 0.7105(3) 0.6354(3) 0.112(2) Uani 1 1 d . U . . .
H26A H -0.1348 0.7395 0.6514 0.135 Uiso 1 1 calc R U . . .
H26B H -0.1412 0.6778 0.6428 0.135 Uiso 1 1 calc R U . . .
C28 C -0.0965(8) 0.8698(5) 0.5703(3) 0.137(3) Uani 1 1 d . U . . .
H28A H -0.0433 0.8822 0.5910 0.165 Uiso 1 1 calc R U . . .
H28B H -0.1582 0.8949 0.5699 0.165 Uiso 1 1 calc R U . . .
C24 C 0.0462(9) 0.6493(3) 0.6369(3) 0.121(3) Uani 1 1 d . U . . .
H24A H -0.0048 0.6246 0.6505 0.145 Uiso 1 1 calc R U . . .
H24B H 0.0425 0.6429 0.6069 0.145 Uiso 1 1 calc R U . . .
C22 C 0.1812(9) 0.6565(4) 0.6970(3) 0.139(3) Uani 1 1 d . U . . .
H22A H 0.1440 0.6326 0.7164 0.167 Uiso 1 1 calc R U . . .
H22B H 0.2607 0.6542 0.7022 0.167 Uiso 1 1 calc R U . . .
C25 C 0.0330(9) 0.7142(3) 0.6930(3) 0.117(3) Uani 1 1 d . U . . .
H25A H 0.0050 0.7491 0.7009 0.140 Uiso 1 1 calc R U . . .
H25B H -0.0084 0.6878 0.7089 0.140 Uiso 1 1 calc R U . . .
N3 N 0.1438(9) 0.7110(3) 0.7045(2) 0.120(3) Uani 1 1 d . U . . .
C21 C 0.2094(7) 0.7534(3) 0.69428(19) 0.093(2) Uani 1 1 d . U . . .
H21A H 0.2817 0.7481 0.7072 0.112 Uiso 1 1 calc R U . . .
H21B H 0.1771 0.7852 0.7067 0.112 Uiso 1 1 calc R U . . .
C18 C 0.3260(9) 0.8849(4) 0.5814(3) 0.156(4) Uani 1 1 d . U . . .
H18A H 0.2990 0.9115 0.6006 0.235 Uiso 1 1 calc R U . . .
H18B H 0.2998 0.8929 0.5536 0.235 Uiso 1 1 calc R U . . .
H18C H 0.4059 0.8850 0.5816 0.235 Uiso 1 1 calc R U . . .
C23 C 0.1563(9) 0.6387(4) 0.6512(3) 0.130(3) Uani 1 1 d . U . . .
H23A H 0.2082 0.6566 0.6326 0.156 Uiso 1 1 calc R U . . .
H23B H 0.1699 0.6006 0.6490 0.156 Uiso 1 1 calc R U . . .
O6 O 0.3369(3) 0.70072(16) 0.58279(12) 0.0702(12) 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
O2 C1 1.273(6) . ?
O2 Ni1 2.139(3) 8 ?
C1 O1 1.238(6) . ?
C1 C2 1.466(7) . ?
Ni1 N2 2.020(5) . ?
Ni1 N1 2.028(5) . ?
Ni1 N4 2.106(6) . ?
Ni1 N5 2.117(6) . ?
Ni1 O2 2.139(3) 8_566 ?
Ni1 O5 2.167(3) . ?
C11 C12 1.360(6) . ?
C11 O4 1.373(5) . ?
C11 C16 1.384(6) . ?
C9 C8 1.487(5) 2_565 ?
C9 C8 1.487(5) . ?
C9 C10 1.528(5) . ?
C9 C10 1.528(5) 2_565 ?
C14 C13 1.394(6) . ?
C14 C15 1.397(6) . ?
C14 C17 1.481(6) . ?
C16 C15 1.385(6) . ?
C10 O4 1.419(5) . ?
C12 C13 1.400(6) . ?
C8 O3 1.451(5) . ?
C5 O3 1.337(5) . ?
C5 C4 1.376(6) . ?
C5 C6 1.387(7) . ?
C4 C3 1.365(6) . ?
C2 C3 1.381(7) . ?
C2 C7 1.403(7) . ?
C7 C6 1.394(6) . ?
C17 O5 1.250(6) . ?
C17 O6 1.269(6) . ?
N1 C31 1.491(8) . ?
N1 C19 1.512(8) . ?
N2 C20 1.495(8) . ?
N2 C21 1.540(8) . ?
N4 C26 1.389(10) . ?
N4 C24 1.500(10) . ?
N4 C25 1.547(10) . ?
N5 C27 1.455(9) . ?
N5 C30 1.472(8) . ?
N5 C32 1.557(11) . ?
N6 C30 1.375(8) . ?
N6 C31 1.430(10) . ?
N6 C29 1.467(11) . ?
C20 C19 1.422(8) . ?
C19 C18 1.586(11) . ?
C32 C26 1.482(12) . ?
C29 C28 1.532(12) . ?
C27 C28 1.432(13) . ?
C24 C23 1.423(12) . ?
C22 N3 1.455(11) . ?
C22 C23 1.558(12) . ?
C25 N3 1.382(12) . ?
N3 C21 1.360(10) . ?

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
C1 O2 Ni1 135.6(4) . 8 ?
O1 C1 O2 123.7(5) . . ?
O1 C1 C2 120.1(5) . . ?
O2 C1 C2 116.1(5) . . ?
N2 Ni1 N1 86.3(2) . . ?
N2 Ni1 N4 93.3(3) . . ?
N1 Ni1 N4 179.6(3) . . ?
N2 Ni1 N5 178.8(3) . . ?
N1 Ni1 N5 92.5(3) . . ?
N4 Ni1 N5 87.9(3) . . ?
N2 Ni1 O2 92.27(17) . 8_566 ?
N1 Ni1 O2 91.45(16) . 8_566 ?
N4 Ni1 O2 88.69(17) . 8_566 ?
N5 Ni1 O2 87.62(19) . 8_566 ?
N2 Ni1 O5 89.71(16) . . ?
N1 Ni1 O5 89.27(16) . . ?
N4 Ni1 O5 90.59(18) . . ?
N5 Ni1 O5 90.41(17) . . ?
O2 Ni1 O5 177.93(15) 8_566 . ?
C12 C11 O4 124.3(4) . . ?
C12 C11 C16 121.2(4) . . ?
O4 C11 C16 114.5(4) . . ?
C8 C9 C8 108.4(5) 2_565 . ?
C8 C9 C10 111.5(2) 2_565 . ?
C8 C9 C10 108.6(2) . . ?
C8 C9 C10 108.6(2) 2_565 2_565 ?
C8 C9 C10 111.6(2) . 2_565 ?
C10 C9 C10 108.1(5) . 2_565 ?
C13 C14 C15 118.2(4) . . ?
C13 C14 C17 121.1(4) . . ?
C15 C14 C17 120.7(4) . . ?
C11 C16 C15 119.5(4) . . ?
O4 C10 C9 107.6(3) . . ?
C11 C12 C13 119.5(4) . . ?
O3 C8 C9 108.1(3) . . ?
C14 C13 C12 120.8(4) . . ?
O3 C5 C4 115.7(4) . . ?
O3 C5 C6 125.3(4) . . ?
C4 C5 C6 118.9(4) . . ?
C16 C15 C14 120.8(4) . . ?
C3 C4 C5 121.3(5) . . ?
C3 C2 C7 116.6(4) . . ?
C3 C2 C1 123.9(5) . . ?
C7 C2 C1 119.4(5) . . ?
C6 C7 C2 121.7(5) . . ?
C4 C3 C2 122.0(5) . . ?
O5 C17 O6 124.6(4) . . ?
O5 C17 C14 117.8(4) . . ?
O6 C17 C14 117.5(5) . . ?
C5 C6 C7 119.3(5) . . ?
C11 O4 C10 117.8(3) . . ?
C17 O5 Ni1 136.8(3) . . ?
C5 O3 C8 120.0(3) . . ?
C31 N1 C19 116.9(5) . . ?
C31 N1 Ni1 113.1(5) . . ?
C19 N1 Ni1 105.5(3) . . ?
C20 N2 C21 113.5(5) . . ?
C20 N2 Ni1 105.8(4) . . ?
C21 N2 Ni1 114.9(4) . . ?
C26 N4 C24 108.9(7) . . ?
C26 N4 C25 113.2(6) . . ?
C24 N4 C25 105.2(7) . . ?
C26 N4 Ni1 103.8(6) . . ?
C24 N4 Ni1 118.5(4) . . ?
C25 N4 Ni1 107.5(4) . . ?
C27 N5 C30 106.4(8) . . ?
C27 N5 C32 109.2(6) . . ?
C30 N5 C32 114.6(6) . . ?
C27 N5 Ni1 120.2(5) . . ?
C30 N5 Ni1 108.3(5) . . ?
C32 N5 Ni1 98.4(5) . . ?
C30 N6 C31 116.8(8) . . ?
C30 N6 C29 111.4(9) . . ?
C31 N6 C29 114.7(9) . . ?
C19 C20 N2 110.1(5) . . ?
C20 C19 N1 110.5(5) . . ?
C20 C19 C18 117.0(6) . . ?
N1 C19 C18 103.0(6) . . ?
N6 C30 N5 113.5(8) . . ?
C26 C32 N5 112.5(6) . . ?
N6 C29 C28 112.6(8) . . ?
N6 C31 N1 118.7(6) . . ?
C28 C27 N5 115.6(8) . . ?
N4 C26 C32 111.1(7) . . ?
C27 C28 C29 112.4(9) . . ?
C23 C24 N4 112.7(7) . . ?
N3 C22 C23 111.2(8) . . ?
N3 C25 N4 115.1(7) . . ?
C21 N3 C25 116.7(8) . . ?
C21 N3 C22 120.8(9) . . ?
C25 N3 C22 108.0(9) . . ?
N3 C21 N2 116.8(6) . . ?
C24 C23 C22 115.2(9) . . ?

_refine_diff_density_max         0.699
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.077
# 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 -0.010 0.008 0.001 4762 1216 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_7                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The difference is due to the crystallization solvent
molecules that were removed by using SQUEEZE.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1401611'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2015-11-13 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         'C65 H100 N12 Ni2 O12, 4(H2 O)'
_chemical_formula_sum            'C65 H108 N12 Ni2 O16'
_chemical_formula_weight         1431.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   18.7966(7)
_cell_length_b                   18.7966(7)
_cell_length_c                   21.2715(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7515.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1767
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      20.00

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             3064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_absorpt_coefficient_mu    0.570
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16659
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.446
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3789
_reflns_number_gt                2424
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'Diamond 3.2'
_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)+(0.0666P)²+2.2023P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3789
_refine_ls_number_parameters     257
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1192
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Ni1 Ni 0.0000 0.5000 1.0000 0.03192(19) Uani 1 2 d S . P . .
O4 O 0.10111(11) 0.45341(12) 0.97720(10) 0.0420(6) Uani 1 1 d . . . . .
O3 O 0.38727(10) 0.31081(11) 0.88230(9) 0.0312(5) Uani 1 1 d . . . . .
O2 O 0.15928(13) 0.44317(15) 1.06800(11) 0.0616(8) Uani 1 1 d . . . . .
O1 O 0.20093(16) 0.59470(18) 0.94764(13) 0.0732(9) Uani 1 1 d G . . . .
H1A H 0.2305 0.5671 0.9676 0.110 Uiso 1 1 d G U . . .
H1B H 0.2028 0.5855 0.9076 0.110 Uiso 1 1 d G U . . .
C1 C 0.5000 0.2500 0.8750 0.0192(11) Uani 1 4 d S T P . .
C2 C 0.44412(13) 0.28236(14) 0.91859(13) 0.0239(6) Uani 1 1 d . . . . .
H2A H 0.4257 0.2454 0.9475 0.029 Uiso 1 1 calc R U . . .
H2B H 0.4660 0.3205 0.9442 0.029 Uiso 1 1 calc R U . . .
C6 C 0.21665(15) 0.40449(16) 0.97555(14) 0.0328(7) Uani 1 1 d . . . . .
C3 C 0.33297(15) 0.34134(16) 0.91553(13) 0.0305(7) Uani 1 1 d . . . . .
C7 C 0.27613(15) 0.38408(17) 1.00873(14) 0.0341(7) Uani 1 1 d . . . . .
H7 H 0.2778 0.3922 1.0528 0.041 Uiso 1 1 calc R U . . .
C8 C 0.33347(15) 0.35212(17) 0.97955(14) 0.0340(7) Uani 1 1 d . . . . .
H8 H 0.3734 0.3375 1.0037 0.041 Uiso 1 1 calc R U . . .
C5 C 0.21670(17) 0.3932(2) 0.91130(16) 0.0543(11) Uani 1 1 d . . . . .
H5 H 0.1763 0.4067 0.8873 0.065 Uiso 1 1 calc R U . . .
C4 C 0.27439(18) 0.3627(2) 0.88127(16) 0.0538(11) Uani 1 1 d . . . . .
H4 H 0.2737 0.3564 0.8370 0.065 Uiso 1 1 calc R U . . .
C9 C 0.15483(17) 0.43638(17) 1.00964(15) 0.0370(8) Uani 1 1 d . . . . .
C13 C -0.01044(18) 0.43138(19) 0.87410(16) 0.0484(9) Uani 1 1 d . . . . .
H13A H -0.0239 0.4364 0.8293 0.058 Uiso 1 1 calc R U . . .
H13B H 0.0408 0.4191 0.8756 0.058 Uiso 1 1 calc R U . . .
C11 C 0.0164(2) 0.62229(19) 0.92447(16) 0.0519(10) Uani 1 1 d . . . . .
H11A H 0.0456 0.6622 0.9085 0.062 Uiso 1 1 calc R U . . .
H11B H -0.0334 0.6389 0.9285 0.062 Uiso 1 1 calc R U . . .
C10 C 0.0278(2) 0.65037(19) 1.03808(18) 0.0524(10) Uani 1 1 d . . . . .
H10A H 0.0518 0.6960 1.0288 0.063 Uiso 1 1 calc R U . . .
H10B H -0.0241 0.6596 1.0392 0.063 Uiso 1 1 calc R U . . .
C12 C 0.02006(18) 0.56044(19) 0.87930(16) 0.0485(9) Uani 1 1 d . . . . .
H12A H 0.0000 0.5744 0.8381 0.058 Uiso 1 1 calc R U . . .
H12B H 0.0702 0.5460 0.8730 0.058 Uiso 1 1 calc R U . . .
N3 N 0.04316(15) 0.59924(16) 0.98609(13) 0.0431(7) Uani 1 1 d . . . . .
H3 H 0.0863(18) 0.5948(19) 0.9810(16) 0.052 Uiso 1 1 d . U . . .
N2 N -0.02092(14) 0.50088(15) 0.90574(13) 0.0374(7) Uani 1 1 d . . . . .
H2 H -0.0676(18) 0.5083(17) 0.9036(14) 0.045 Uiso 1 1 d . U . . .
N1 N -0.05013(15) 0.37392(16) 0.90076(14) 0.0504(8) Uani 1 1 d . U . . .
C14 C -0.12763(19) 0.3773(2) 0.8913(2) 0.0616(11) Uani 1 1 d . U . . .
H14A H -0.1516 0.3522 0.9263 0.074 Uiso 0.438(12) 1 calc R U P A 1
H14B H -0.1430 0.4276 0.8923 0.074 Uiso 0.438(12) 1 calc R U P A 1
H14C H -0.1489 0.3964 0.9304 0.074 Uiso 0.562(12) 1 calc R U P A 2
H14D H -0.1368 0.4126 0.8577 0.074 Uiso 0.562(12) 1 calc R U P A 2
C15B C -0.1501(5) 0.3454(8) 0.8315(6) 0.072(4) Uani 0.438(12) 1 d . U P A 1
H15B H -0.1326 0.3799 0.7992 0.087 Uiso 0.438(12) 1 calc R U P A 1
C16B C -0.2313(7) 0.3501(9) 0.8258(9) 0.095(5) Uani 0.438(12) 1 d . U P A 1
H16A H -0.2534 0.3187 0.8570 0.143 Uiso 0.438(12) 1 calc R U P A 1
H16B H -0.2459 0.3354 0.7835 0.143 Uiso 0.438(12) 1 calc R U P A 1
H16C H -0.2466 0.3992 0.8333 0.143 Uiso 0.438(12) 1 calc R U P A 1
C17B C -0.1226(9) 0.2648(9) 0.8288(8) 0.106(6) Uani 0.562(12) 1 d . U P A 2
H17A H -0.1197 0.2879 0.7876 0.160 Uiso 0.562(12) 1 calc R U P A 2
H17B H -0.1464 0.2187 0.8245 0.160 Uiso 0.562(12) 1 calc R U P A 2
H17C H -0.0746 0.2577 0.8455 0.160 Uiso 0.562(12) 1 calc R U P A 2
C15A C -0.1662(4) 0.3133(5) 0.8751(6) 0.069(3) Uani 0.562(12) 1 d . U P A 2
H15A H -0.1657 0.2855 0.9152 0.083 Uiso 0.562(12) 1 calc R U P A 2
C17A C -0.1352(12) 0.2834(13) 0.8071(9) 0.090(5) Uani 0.438(12) 1 d . U P A 1
H17D H -0.0853 0.2716 0.8156 0.134 Uiso 0.438(12) 1 calc R U P A 1
H17E H -0.1430 0.2850 0.7616 0.134 Uiso 0.438(12) 1 calc R U P A 1
H17F H -0.1660 0.2470 0.8258 0.134 Uiso 0.438(12) 1 calc R U P A 1
C16A C -0.2451(5) 0.3276(7) 0.8647(8) 0.106(5) Uani 0.562(12) 1 d . U P A 2
H16D H -0.2676 0.3396 0.9049 0.159 Uiso 0.562(12) 1 calc R U P A 2
H16E H -0.2676 0.2850 0.8471 0.159 Uiso 0.562(12) 1 calc R U P A 2
H16F H -0.2507 0.3674 0.8353 0.159 Uiso 0.562(12) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.043(3) 9_567 ?
Ni1 N2 2.043(3) . ?
Ni1 N3 2.056(3) 9_567 ?
Ni1 N3 2.056(3) . ?
Ni1 O4 2.148(2) 9_567 ?
Ni1 O4 2.148(2) . ?
O4 C9 1.264(4) . ?
O3 C3 1.368(3) . ?
O3 C2 1.423(3) . ?
O2 C9 1.251(4) . ?
O1 H1A 0.8705 . ?
O1 H1B 0.8699 . ?
C1 C2 1.527(3) . ?
C1 C2 1.527(3) 16_657 ?
C1 C2 1.527(3) 6_554 ?
C1 C2 1.527(3) 11_667 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C6 C7 1.377(4) . ?
C6 C5 1.383(4) . ?
C6 C9 1.495(4) . ?
C3 C8 1.377(4) . ?
C3 C4 1.380(4) . ?
C7 C8 1.381(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C5 C4 1.383(4) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C13 N1 1.430(4) . ?
C13 N2 1.483(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C11 N3 1.469(4) . ?
C11 C12 1.510(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C10 N1 1.441(4) 9_567 ?
C10 N3 1.494(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 N2 1.471(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N3 H3 0.82(3) . ?
N2 H2 0.89(3) . ?
N1 C10 1.442(4) 9_567 ?
N1 C14 1.472(4) . ?
C14 C15A 1.446(8) . ?
C14 C15B 1.468(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
C15B C17A 1.31(2) . ?
C15B C16B 1.535(15) . ?
C15B H15B 1.0000 . ?
C16B H16A 0.9800 . ?
C16B H16B 0.9800 . ?
C16B H16C 0.9800 . ?
C17B C15A 1.572(16) . ?
C17B H17A 0.9800 . ?
C17B H17B 0.9800 . ?
C17B H17C 0.9800 . ?
C15A C16A 1.522(12) . ?
C15A H15A 1.0000 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?

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
N2 Ni1 N2 180.0 9_567 . ?
N2 Ni1 N3 85.83(11) 9_567 9_567 ?
N2 Ni1 N3 94.17(11) . 9_567 ?
N2 Ni1 N3 94.17(11) 9_567 . ?
N2 Ni1 N3 85.83(11) . . ?
N3 Ni1 N3 180.0 9_567 . ?
N2 Ni1 O4 87.25(9) 9_567 9_567 ?
N2 Ni1 O4 92.75(9) . 9_567 ?
N3 Ni1 O4 89.32(10) 9_567 9_567 ?
N3 Ni1 O4 90.68(10) . 9_567 ?
N2 Ni1 O4 92.75(9) 9_567 . ?
N2 Ni1 O4 87.25(9) . . ?
N3 Ni1 O4 90.68(10) 9_567 . ?
N3 Ni1 O4 89.33(10) . . ?
O4 Ni1 O4 180.00(11) 9_567 . ?
C9 O4 Ni1 133.4(2) . . ?
C3 O3 C2 116.0(2) . . ?
H1A O1 H1B 109.4 . . ?
C2 C1 C2 111.63(10) . 16_657 ?
C2 C1 C2 105.2(2) . 6_554 ?
C2 C1 C2 111.63(10) 16_657 6_554 ?
C2 C1 C2 111.63(10) . 11_667 ?
C2 C1 C2 105.2(2) 16_657 11_667 ?
C2 C1 C2 111.63(10) 6_554 11_667 ?
O3 C2 C1 109.68(19) . . ?
O3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C7 C6 C5 117.6(3) . . ?
C7 C6 C9 119.6(3) . . ?
C5 C6 C9 122.8(3) . . ?
O3 C3 C8 124.6(2) . . ?
O3 C3 C4 116.4(3) . . ?
C8 C3 C4 119.0(3) . . ?
C6 C7 C8 121.6(3) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C3 C8 C7 120.2(3) . . ?
C3 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
O2 C9 O4 124.7(3) . . ?
O2 C9 C6 118.1(3) . . ?
O4 C9 C6 117.2(3) . . ?
N1 C13 N2 114.6(3) . . ?
N1 C13 H13A 108.6 . . ?
N2 C13 H13A 108.6 . . ?
N1 C13 H13B 108.6 . . ?
N2 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
N3 C11 C12 109.0(3) . . ?
N3 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N1 C10 N3 114.1(3) 9_567 . ?
N1 C10 H10A 108.7 9_567 . ?
N3 C10 H10A 108.7 . . ?
N1 C10 H10B 108.7 9_567 . ?
N3 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
N2 C12 C11 108.6(3) . . ?
N2 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
N2 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C11 N3 C10 113.9(3) . . ?
C11 N3 Ni1 105.1(2) . . ?
C10 N3 Ni1 113.6(2) . . ?
C11 N3 H3 105(2) . . ?
C10 N3 H3 111(3) . . ?
Ni1 N3 H3 108(3) . . ?
C12 N2 C13 115.3(3) . . ?
C12 N2 Ni1 106.3(2) . . ?
C13 N2 Ni1 114.4(2) . . ?
C12 N2 H2 112(2) . . ?
C13 N2 H2 104(2) . . ?
Ni1 N2 H2 104(2) . . ?
C13 N1 C10 116.4(3) . 9_567 ?
C13 N1 C14 115.4(3) . . ?
C10 N1 C14 115.2(3) 9_567 . ?
C15A C14 N1 119.6(4) . . ?
C15B C14 N1 112.7(5) . . ?
C15B C14 H14A 109.1 . . ?
N1 C14 H14A 109.1 . . ?
C15B C14 H14B 109.1 . . ?
N1 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C15A C14 H14C 107.4 . . ?
N1 C14 H14C 107.4 . . ?
C15A C14 H14D 107.4 . . ?
N1 C14 H14D 107.4 . . ?
H14C C14 H14D 107.0 . . ?
C17A C15B C14 130.4(13) . . ?
C17A C15B C16B 103.5(14) . . ?
C14 C15B C16B 109.3(9) . . ?
C17A C15B H15B 103.6 . . ?
C14 C15B H15B 103.6 . . ?
C16B C15B H15B 103.6 . . ?
C15B C16B H16A 109.5 . . ?
C15B C16B H16B 109.5 . . ?
H16A C16B H16B 109.5 . . ?
C15B C16B H16C 109.5 . . ?
H16A C16B H16C 109.5 . . ?
H16B C16B H16C 109.5 . . ?
C15A C17B H17A 109.5 . . ?
C15A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C15A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C14 C15A C16A 112.1(7) . . ?
C14 C15A C17B 111.6(9) . . ?
C16A C15A C17B 121.2(10) . . ?
C14 C15A H15A 103.1 . . ?
C16A C15A H15A 103.1 . . ?
C17B C15A H15A 103.1 . . ?
C15B C17A H17D 109.5 . . ?
C15B C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C15B C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C15A C16A H16D 109.5 . . ?
C15A C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
C15A C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 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
C3 O3 C2 C1 179.7(2) . . . . ?
C2 C1 C2 O3 -55.6(3) 16_657 . . . ?
C2 C1 C2 O3 -176.9(3) 6_554 . . . ?
C2 C1 C2 O3 61.8(3) 11_667 . . . ?
C2 O3 C3 C8 6.6(4) . . . . ?
C2 O3 C3 C4 -173.8(3) . . . . ?
C5 C6 C7 C8 -1.3(5) . . . . ?
C9 C6 C7 C8 177.7(3) . . . . ?
O3 C3 C8 C7 179.4(3) . . . . ?
C4 C3 C8 C7 -0.2(5) . . . . ?
C6 C7 C8 C3 1.5(5) . . . . ?
C7 C6 C5 C4 -0.2(6) . . . . ?
C9 C6 C5 C4 -179.1(4) . . . . ?
O3 C3 C4 C5 179.1(3) . . . . ?
C8 C3 C4 C5 -1.2(6) . . . . ?
C6 C5 C4 C3 1.4(6) . . . . ?
Ni1 O4 C9 O2 1.4(6) . . . . ?
Ni1 O4 C9 C6 -179.9(2) . . . . ?
C7 C6 C9 O2 -0.3(5) . . . . ?
C5 C6 C9 O2 178.6(4) . . . . ?
C7 C6 C9 O4 -179.1(3) . . . . ?
C5 C6 C9 O4 -0.2(5) . . . . ?
N3 C11 C12 N2 56.9(4) . . . . ?
C12 C11 N3 C10 -167.4(3) . . . . ?
C12 C11 N3 Ni1 -42.4(3) . . . . ?
N1 C10 N3 C11 176.5(3) 9_567 . . . ?
N1 C10 N3 Ni1 56.2(4) 9_567 . . . ?
C11 C12 N2 C13 -167.7(3) . . . . ?
C11 C12 N2 Ni1 -39.8(3) . . . . ?
N1 C13 N2 C12 179.4(3) . . . . ?
N1 C13 N2 Ni1 55.7(3) . . . . ?
N2 C13 N1 C10 -70.1(4) . . . 9_567 ?
N2 C13 N1 C14 69.6(4) . . . . ?
C13 N1 C14 C15A 138.0(7) . . . . ?
C10 N1 C14 C15A -81.7(7) 9_567 . . . ?
C13 N1 C14 C15B 86.5(8) . . . . ?
C10 N1 C14 C15B -133.2(8) 9_567 . . . ?
N1 C14 C15B C17A 51(2) . . . . ?
N1 C14 C15B C16B 179.2(8) . . . . ?
N1 C14 C15A C16A -177.7(7) . . . . ?
N1 C14 C15A C17B -38.0(11) . . . . ?

_refine_diff_density_max         0.337
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.059
# start Validation Reply Form
_vrf_PLAT420_8                   
;
PROBLEM: D-H Without Acceptor        O1     -   H1A    ..     Please Check 
RESPONSE: The O1-H1A point to the benzene ring to from weak O-H pai interaction.
;
# end Validation Reply Form
