# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_cp_CN_sq
_database_code_depnum_ccdc_archive 'CCDC 1898504'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        cp-flexMOF(CN)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H124 N32 Ni4 O16'
_chemical_formula_sum            'C88 H124 N32 Ni4 O16'
_chemical_formula_weight         2121.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.063(2)
_cell_length_b                   15.927(3)
_cell_length_c                   16.581(3)
_cell_angle_alpha                86.837(8)
_cell_angle_beta                 74.753(5)
_cell_angle_gamma                78.205(9)
_cell_volume                     2509.8(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    44291
_cell_measurement_theta_min      1.795
_cell_measurement_theta_max      32.853

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             1116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.782
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16553
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.795
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measured_fraction_theta_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.932
_reflns_number_total             8602
_reflns_number_gt                4676
_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       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2015b)'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  CIFTAB
_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)+(0.1179P)²] 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         8602
_refine_ls_number_parameters     637
_refine_ls_number_restraints     599
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0723
_refine_ls_wR_factor_ref         0.2083
_refine_ls_wR_factor_gt          0.1769
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.960
_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 0.000000 0.500000 0.000000 0.0456(3) Uani 1 2 d S U P . .
Ni2 Ni 0.000000 0.000000 0.500000 0.0542(3) Uani 1 2 d S U P . .
Ni3 Ni 0.500000 0.000000 0.000000 0.0526(3) Uani 1 2 d S U P . .
Ni4 Ni 0.000000 0.500000 0.500000 0.0563(3) Uani 1 2 d S U P . .
O1 O -0.2736(5) 0.4369(3) 0.1566(3) 0.0709(13) Uani 1 1 d . U . . .
O2 O -0.0425(4) 0.4032(3) 0.0964(2) 0.0538(11) Uani 1 1 d . U . . .
O3 O -0.1393(5) 0.2268(3) 0.5212(2) 0.0722(14) Uani 1 1 d . U . . .
O4 O -0.0176(5) 0.1187(3) 0.4343(2) 0.0616(12) Uani 1 1 d . U . . .
O5 O 0.5766(5) 0.0143(3) 0.1927(3) 0.0835(15) Uani 1 1 d . U . . .
O6 O 0.4111(4) 0.0554(3) 0.1226(3) 0.0615(11) Uani 1 1 d . U . . .
O7 O 0.1876(5) 0.2937(3) 0.5150(3) 0.0770(14) Uani 1 1 d . U . . .
O8 O 0.0948(5) 0.3821(3) 0.4261(2) 0.0596(11) Uani 1 1 d . U . . .
N1 N 0.1988(5) 0.4295(3) -0.0411(3) 0.0476(12) Uani 1 1 d . U . . .
H1 H 0.252109 0.464773 -0.084741 0.057 Uiso 1 1 calc R U . . .
N2 N 0.0609(5) 0.5679(3) 0.0802(3) 0.0486(12) Uani 1 1 d . U . . .
H2 H 0.106749 0.613778 0.047760 0.058 Uiso 1 1 calc R U . . .
N3 N 0.2903(5) 0.4776(3) 0.0631(3) 0.0489(12) Uani 1 1 d . U . . .
N4 N 0.5093(6) 0.2460(4) 0.1016(4) 0.0711(16) Uani 1 1 d . U . . .
N5 N 0.2084(7) 0.0068(4) 0.4858(4) 0.0765(16) Uani 1 1 d . U . . .
H5 H 0.218986 0.066609 0.468102 0.092 Uiso 1 1 calc R U . . .
N6 N -0.0676(7) 0.0601(4) 0.6143(3) 0.0758(16) Uani 1 1 d . U . . .
H6 H -0.075282 0.123298 0.604832 0.091 Uiso 1 1 calc R U . . .
N7 N 0.1676(11) 0.0415(5) 0.6309(6) 0.111(2) Uani 1 1 d . U . . .
N8 N 0.3336(12) 0.2832(7) 0.7003(6) 0.150(4) Uani 1 1 d . U . . .
N9 N 0.5640(5) 0.1131(3) -0.0402(3) 0.0572(13) Uani 1 1 d . U . . .
H9 H 0.553413 0.148777 0.009708 0.069 Uiso 1 1 calc R U . . .
N10 N 0.6827(5) -0.0547(3) 0.0305(3) 0.0563(13) Uani 1 1 d . U . . .
H10 H 0.677502 -0.031626 0.086397 0.068 Uiso 1 1 calc R U . . .
N11 N 0.8083(6) 0.0535(4) -0.0411(4) 0.0724(16) Uani 1 1 d . U . . .
N12 N 1.0346(8) 0.1874(5) -0.1356(5) 0.104(2) Uani 1 1 d . U . . .
N13 N -0.0789(6) 0.5462(3) 0.4027(3) 0.0607(14) Uani 1 1 d . U . . .
H13 H -0.121513 0.608255 0.413630 0.073 Uiso 1 1 calc R U . . .
N14 N 0.1790(6) 0.5509(4) 0.4602(3) 0.0657(14) Uani 1 1 d . U . . .
H14 H 0.153851 0.613221 0.475060 0.079 Uiso 1 1 calc R U . . .
N15 N 0.1444(6) 0.5817(4) 0.3200(3) 0.0665(15) Uani 1 1 d . U . . .
N16 N 0.3289(8) 0.6796(4) 0.1261(4) 0.098(2) Uani 1 1 d . U . . .
C1 C -0.1521(7) 0.3980(4) 0.1539(4) 0.0575(16) Uani 1 1 d . U . . .
C2 C -0.1321(6) 0.3443(4) 0.2297(3) 0.0494(14) Uani 1 1 d . U . . .
C3 C -0.2482(6) 0.3317(4) 0.2936(4) 0.0548(16) Uani 1 1 d . U . . .
H3 H -0.340680 0.355119 0.289162 0.066 Uiso 1 1 calc R U . . .
C4 C -0.2271(7) 0.2844(4) 0.3643(4) 0.0574(16) Uani 1 1 d . U . . .
H4 H -0.306620 0.275497 0.407132 0.069 Uiso 1 1 calc R U . . .
C5 C -0.0934(6) 0.2500(4) 0.3740(3) 0.0516(15) Uani 1 1 d . U . . .
C6 C 0.0228(6) 0.2650(4) 0.3109(3) 0.0525(15) Uani 1 1 d . U . . .
C7 C 0.0017(6) 0.3115(4) 0.2400(3) 0.0468(14) Uani 1 1 d . U . . .
H7 H 0.081162 0.321158 0.197469 0.056 Uiso 1 1 calc R U . . .
C8 C -0.0824(7) 0.1969(4) 0.4508(4) 0.0563(16) Uani 1 1 d . U . . .
C9 C 0.4629(7) 0.0584(4) 0.1833(4) 0.0648(17) Uani 1 1 d . U . . .
C10 C 0.3829(7) 0.1227(4) 0.2518(4) 0.0560(15) Uani 1 1 d . U . . .
C11 C 0.2477(6) 0.1666(4) 0.2525(4) 0.0508(14) Uani 1 1 d . U . . .
H11 H 0.207016 0.155774 0.209533 0.061 Uiso 1 1 calc R U . . .
C12 C 0.1702(6) 0.2262(4) 0.3150(3) 0.0501(14) Uani 1 1 d . U . . .
C13 C 0.2326(7) 0.2446(4) 0.3773(4) 0.0563(15) Uani 1 1 d . U . . .
C14 C 0.3659(7) 0.1996(4) 0.3749(4) 0.0605(16) Uani 1 1 d . U . . .
H14A H 0.408128 0.209674 0.417448 0.073 Uiso 1 1 calc R U . . .
C15 C 0.4414(7) 0.1399(4) 0.3131(4) 0.0614(16) Uani 1 1 d . U . . .
H15 H 0.533755 0.111084 0.313433 0.074 Uiso 1 1 calc R U . . .
C16 C 0.1650(7) 0.3111(4) 0.4456(4) 0.0621(17) Uani 1 1 d . U . . .
C17 C 0.1612(6) 0.5148(4) 0.1234(3) 0.0505(14) Uani 1 1 d . U . . .
H17A H 0.182381 0.550759 0.163347 0.061 Uiso 1 1 calc R U . . .
H17B H 0.117991 0.468425 0.155288 0.061 Uiso 1 1 calc R U . . .
C18 C 0.2821(6) 0.4033(4) 0.0182(3) 0.0524(15) Uani 1 1 d . U . . .
H18A H 0.377928 0.374327 -0.011707 0.063 Uiso 1 1 calc R U . . .
H18B H 0.239356 0.362025 0.058453 0.063 Uiso 1 1 calc R U . . .
C19 C 0.1781(7) 0.3561(4) -0.0853(4) 0.0550(16) Uani 1 1 d . U . . .
H19A H 0.141361 0.313454 -0.044271 0.066 Uiso 1 1 calc R U . . .
H19B H 0.268628 0.327616 -0.122310 0.066 Uiso 1 1 calc R U . . .
C20 C -0.0737(6) 0.6091(4) 0.1367(3) 0.0525(15) Uani 1 1 d . U . . .
H20A H -0.059036 0.656446 0.167584 0.063 Uiso 1 1 calc R U . . .
H20B H -0.110992 0.566743 0.177933 0.063 Uiso 1 1 calc R U . . .
C21 C 0.4134(7) 0.4664(4) 0.0977(4) 0.0567(15) Uani 1 1 d . U . . .
H21A H 0.415595 0.522232 0.120324 0.068 Uiso 1 1 calc R U . . .
H21B H 0.499197 0.451015 0.051423 0.068 Uiso 1 1 calc R U . . .
C22 C 0.4196(7) 0.3973(4) 0.1681(4) 0.0566(16) Uani 1 1 d . U . . .
H22A H 0.484827 0.408152 0.200016 0.068 Uiso 1 1 calc R U . . .
H22B H 0.325191 0.402210 0.207210 0.068 Uiso 1 1 calc R U . . .
C23 C 0.4664(7) 0.3105(5) 0.1339(4) 0.0590(17) Uani 1 1 d . U . . .
C24 C -0.2080(9) 0.0432(5) 0.6514(5) 0.086(2) Uani 1 1 d . U . . .
H24A H -0.258202 0.084649 0.697041 0.103 Uiso 1 1 calc R U . . .
H24B H -0.200975 -0.015298 0.675524 0.103 Uiso 1 1 calc R U . . .
C25 C 0.2874(9) -0.0512(5) 0.4135(6) 0.093(3) Uani 1 1 d . U . . .
H25A H 0.380441 -0.036100 0.388989 0.112 Uiso 1 1 calc R U . . .
H25B H 0.302856 -0.111356 0.433247 0.112 Uiso 1 1 calc R U . . .
C26 C 0.0296(12) 0.0316(7) 0.6680(6) 0.105(3) Uani 1 1 d . U . . .
H26A H -0.005985 0.064684 0.720744 0.126 Uiso 1 1 calc R U . . .
H26B H 0.030141 -0.029647 0.682308 0.126 Uiso 1 1 calc R U . . .
C27 C 0.2544(10) -0.0112(6) 0.5646(7) 0.103(2) Uani 1 1 d . U . . .
H27A H 0.253980 -0.071957 0.580501 0.123 Uiso 1 1 calc R U . . .
H27B H 0.351926 -0.002232 0.554655 0.123 Uiso 1 1 calc R U . . .
C28 C 0.1966(14) 0.1241(8) 0.6316(8) 0.140(3) Uani 1 1 d . U . . .
H28A H 0.106861 0.165055 0.652430 0.168 Uiso 1 1 calc R U . . .
H28B H 0.238402 0.140649 0.573448 0.168 Uiso 1 1 calc R U . . .
C29 C 0.2901(11) 0.1320(7) 0.6820(8) 0.124(3) Uani 1 1 d . U . . .
H29A H 0.380875 0.093102 0.658436 0.149 Uiso 1 1 calc R U . . .
H29B H 0.250894 0.110439 0.738662 0.149 Uiso 1 1 calc R U . . .
C30 C 0.3193(12) 0.2153(8) 0.6915(7) 0.125(4) Uani 1 1 d . U . . .
C31 C 0.6802(7) -0.1475(4) 0.0415(4) 0.0638(18) Uani 1 1 d . U . . .
H31A H 0.748779 -0.175028 0.072979 0.077 Uiso 1 1 calc R U . . .
H31B H 0.706353 -0.175699 -0.013751 0.077 Uiso 1 1 calc R U . . .
C32 C 0.4651(7) 0.1575(4) -0.0885(5) 0.0670(18) Uani 1 1 d . U . . .
H32A H 0.489798 0.131791 -0.144865 0.080 Uiso 1 1 calc R U . . .
H32B H 0.470129 0.218991 -0.094977 0.080 Uiso 1 1 calc R U . . .
C33 C 0.8088(7) -0.0356(4) -0.0271(5) 0.071(2) Uani 1 1 d . U . . .
H33A H 0.890552 -0.061466 -0.005239 0.085 Uiso 1 1 calc R U . . .
H33B H 0.821482 -0.063230 -0.081397 0.085 Uiso 1 1 calc R U . . .
C34 C 0.7125(7) 0.0982(4) -0.0890(5) 0.0675(18) Uani 1 1 d . U . . .
H34A H 0.723230 0.063954 -0.139161 0.081 Uiso 1 1 calc R U . . .
H34B H 0.738371 0.154053 -0.108107 0.081 Uiso 1 1 calc R U . . .
C35 C 0.8096(8) 0.0999(5) 0.0310(5) 0.0773(19) Uani 1 1 d . U . . .
H35A H 0.879368 0.065899 0.058456 0.093 Uiso 1 1 calc R U . . .
H35B H 0.716116 0.106385 0.071340 0.093 Uiso 1 1 calc R U . . .
C36 C 0.8454(8) 0.1896(5) 0.0092(5) 0.086(2) Uani 1 1 d . U . . .
H36A H 0.759145 0.230907 0.005456 0.103 Uiso 1 1 calc R U . . .
H36B H 0.879330 0.208809 0.054583 0.103 Uiso 1 1 calc R U . . .
C37 C 0.9541(9) 0.1897(5) -0.0709(6) 0.086(2) Uani 1 1 d . U . . .
C38 C 0.2768(8) 0.5075(5) 0.5082(4) 0.0707(19) Uani 1 1 d . U . . .
H38A H 0.350155 0.541194 0.505924 0.085 Uiso 1 1 calc R U . . .
H38B H 0.323197 0.450038 0.484340 0.085 Uiso 1 1 calc R U . . .
C39 C -0.1937(7) 0.5010(5) 0.4017(4) 0.0657(18) Uani 1 1 d . U . . .
H39A H -0.154079 0.443581 0.376175 0.079 Uiso 1 1 calc R U . . .
H39B H -0.255529 0.534085 0.368629 0.079 Uiso 1 1 calc R U . . .
C40 C 0.2419(8) 0.5430(5) 0.3675(4) 0.0673(18) Uani 1 1 d . U . . .
H40A H 0.324795 0.570655 0.352136 0.081 Uiso 1 1 calc R U . . .
H40B H 0.274505 0.481558 0.352676 0.081 Uiso 1 1 calc R U . . .
C41 C 0.0270(7) 0.5399(4) 0.3226(4) 0.0628(17) Uani 1 1 d . U . . .
H41A H 0.064654 0.478517 0.308790 0.075 Uiso 1 1 calc R U . . .
H41B H -0.019250 0.565589 0.278726 0.075 Uiso 1 1 calc R U . . .
C42 C 0.1047(8) 0.6757(4) 0.3225(4) 0.072(2) Uani 1 1 d . U . . .
H42A H 0.064732 0.694670 0.381327 0.087 Uiso 1 1 calc R U . . .
H42B H 0.031146 0.694646 0.292148 0.087 Uiso 1 1 calc R U . . .
C43 C 0.2300(10) 0.7177(5) 0.2834(5) 0.087(2) Uani 1 1 d . U . . .
H43A H 0.200042 0.780815 0.288863 0.104 Uiso 1 1 calc R U . . .
H43B H 0.303480 0.699007 0.313812 0.104 Uiso 1 1 calc R U . . .
C44 C 0.2880(9) 0.6956(5) 0.1960(5) 0.086(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.043(4) . ?
Ni1 N1 2.043(4) 2_565 ?
Ni1 N2 2.043(5) . ?
Ni1 N2 2.043(5) 2_565 ?
Ni1 O2 2.180(4) 2_565 ?
Ni1 O2 2.180(4) . ?
Ni2 N6 2.055(5) 2_556 ?
Ni2 N6 2.055(5) . ?
Ni2 N5 2.072(6) . ?
Ni2 N5 2.072(6) 2_556 ?
Ni2 O4 2.129(4) . ?
Ni2 O4 2.129(4) 2_556 ?
Ni3 N10 2.045(5) . ?
Ni3 N10 2.045(5) 2_655 ?
Ni3 N9 2.055(5) . ?
Ni3 N9 2.055(5) 2_655 ?
Ni3 O6 2.152(4) 2_655 ?
Ni3 O6 2.152(4) . ?
Ni4 N13 2.019(5) . ?
Ni4 N13 2.019(5) 2_566 ?
Ni4 N14 2.062(6) . ?
Ni4 N14 2.062(6) 2_566 ?
Ni4 O8 2.201(4) . ?
Ni4 O8 2.201(4) 2_566 ?
O1 C1 1.244(7) . ?
O2 C1 1.268(7) . ?
O3 C8 1.231(7) . ?
O4 C8 1.288(7) . ?
O5 C9 1.257(8) . ?
O6 C9 1.257(8) . ?
O7 C16 1.237(7) . ?
O8 C16 1.278(7) . ?
N1 C18 1.446(7) . ?
N1 C19 1.491(8) . ?
N1 H1 1.0000 . ?
N2 C20 1.477(7) . ?
N2 C17 1.486(7) . ?
N2 H2 1.0000 . ?
N3 C17 1.451(7) . ?
N3 C18 1.459(8) . ?
N3 C21 1.473(8) . ?
N4 C23 1.134(8) . ?
N5 C27 1.492(11) . ?
N5 C25 1.499(10) . ?
N5 H5 1.0000 . ?
N6 C24 1.459(10) . ?
N6 C26 1.480(11) . ?
N6 H6 1.0000 . ?
N7 C26 1.400(12) . ?
N7 C27 1.403(12) . ?
N7 C28 1.406(13) . ?
N8 C30 1.141(12) . ?
N9 C34 1.478(7) . ?
N9 C32 1.483(9) . ?
N9 H9 1.0000 . ?
N10 C33 1.450(8) . ?
N10 C31 1.484(8) . ?
N10 H10 1.0000 . ?
N11 C33 1.425(9) . ?
N11 C35 1.443(10) . ?
N11 C34 1.458(9) . ?
N12 C37 1.159(10) . ?
N13 C41 1.462(7) . ?
N13 C39 1.484(9) . ?
N13 H13 1.0000 . ?
N14 C38 1.467(9) . ?
N14 C40 1.502(7) . ?
N14 H14 1.0000 . ?
N15 C40 1.438(9) . ?
N15 C41 1.461(9) . ?
N15 C42 1.468(9) . ?
N16 C44 1.148(9) . ?
C1 C2 1.515(8) . ?
C2 C7 1.392(8) . ?
C2 C3 1.396(8) . ?
C3 C4 1.397(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(8) . ?
C5 C8 1.506(8) . ?
C6 C7 1.395(8) . ?
C6 C12 1.504(9) . ?
C7 H7 0.9500 . ?
C9 C10 1.515(9) . ?
C10 C15 1.366(9) . ?
C10 C11 1.393(9) . ?
C11 C12 1.401(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.414(9) . ?
C13 C14 1.377(9) . ?
C13 C16 1.516(9) . ?
C14 C15 1.391(9) . ?
C14 H14A 0.9500 . ?
C15 H15 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.522(8) 2_565 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.564(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.461(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 C25 1.486(12) 2_556 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.441(15) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.442(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C31 C32 1.501(9) 2_655 ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.545(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.482(11) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C38 C39 1.521(8) 2_566 ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.525(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.446(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 . 2_565 ?
N1 Ni1 N2 91.74(19) . . ?
N1 Ni1 N2 88.26(19) 2_565 . ?
N1 Ni1 N2 88.26(19) . 2_565 ?
N1 Ni1 N2 91.74(19) 2_565 2_565 ?
N2 Ni1 N2 180.0 . 2_565 ?
N1 Ni1 O2 91.65(16) . 2_565 ?
N1 Ni1 O2 88.35(16) 2_565 2_565 ?
N2 Ni1 O2 89.99(17) . 2_565 ?
N2 Ni1 O2 90.01(17) 2_565 2_565 ?
N1 Ni1 O2 88.35(16) . . ?
N1 Ni1 O2 91.65(16) 2_565 . ?
N2 Ni1 O2 90.01(17) . . ?
N2 Ni1 O2 89.99(17) 2_565 . ?
O2 Ni1 O2 180.0 2_565 . ?
N6 Ni2 N6 180.0 2_556 . ?
N6 Ni2 N5 86.1(3) 2_556 . ?
N6 Ni2 N5 93.9(3) . . ?
N6 Ni2 N5 93.9(3) 2_556 2_556 ?
N6 Ni2 N5 86.1(3) . 2_556 ?
N5 Ni2 N5 180.0(3) . 2_556 ?
N6 Ni2 O4 87.61(19) 2_556 . ?
N6 Ni2 O4 92.39(19) . . ?
N5 Ni2 O4 86.4(2) . . ?
N5 Ni2 O4 93.6(2) 2_556 . ?
N6 Ni2 O4 92.39(19) 2_556 2_556 ?
N6 Ni2 O4 87.61(19) . 2_556 ?
N5 Ni2 O4 93.6(2) . 2_556 ?
N5 Ni2 O4 86.4(2) 2_556 2_556 ?
O4 Ni2 O4 180.0 . 2_556 ?
N10 Ni3 N10 180.0 . 2_655 ?
N10 Ni3 N9 94.3(2) . . ?
N10 Ni3 N9 85.7(2) 2_655 . ?
N10 Ni3 N9 85.7(2) . 2_655 ?
N10 Ni3 N9 94.3(2) 2_655 2_655 ?
N9 Ni3 N9 180.0 . 2_655 ?
N10 Ni3 O6 88.66(19) . 2_655 ?
N10 Ni3 O6 91.34(19) 2_655 2_655 ?
N9 Ni3 O6 91.49(19) . 2_655 ?
N9 Ni3 O6 88.51(19) 2_655 2_655 ?
N10 Ni3 O6 91.34(19) . . ?
N10 Ni3 O6 88.66(19) 2_655 . ?
N9 Ni3 O6 88.51(19) . . ?
N9 Ni3 O6 91.49(19) 2_655 . ?
O6 Ni3 O6 180.0 2_655 . ?
N13 Ni4 N13 180.0 . 2_566 ?
N13 Ni4 N14 94.9(2) . . ?
N13 Ni4 N14 85.1(2) 2_566 . ?
N13 Ni4 N14 85.1(2) . 2_566 ?
N13 Ni4 N14 94.9(2) 2_566 2_566 ?
N14 Ni4 N14 180.00(16) . 2_566 ?
N13 Ni4 O8 86.72(18) . . ?
N13 Ni4 O8 93.28(18) 2_566 . ?
N14 Ni4 O8 93.32(19) . . ?
N14 Ni4 O8 86.68(19) 2_566 . ?
N13 Ni4 O8 93.28(18) . 2_566 ?
N13 Ni4 O8 86.72(18) 2_566 2_566 ?
N14 Ni4 O8 86.68(19) . 2_566 ?
N14 Ni4 O8 93.32(19) 2_566 2_566 ?
O8 Ni4 O8 180.0 . 2_566 ?
C1 O2 Ni1 131.2(4) . . ?
C8 O4 Ni2 136.9(4) . . ?
C9 O6 Ni3 131.9(4) . . ?
C16 O8 Ni4 129.9(4) . . ?
C18 N1 C19 113.3(4) . . ?
C18 N1 Ni1 119.0(3) . . ?
C19 N1 Ni1 103.4(4) . . ?
C18 N1 H1 106.8 . . ?
C19 N1 H1 106.8 . . ?
Ni1 N1 H1 106.8 . . ?
C20 N2 C17 114.4(4) . . ?
C20 N2 Ni1 103.2(4) . . ?
C17 N2 Ni1 113.7(4) . . ?
C20 N2 H2 108.4 . . ?
C17 N2 H2 108.4 . . ?
Ni1 N2 H2 108.4 . . ?
C17 N3 C18 114.9(5) . . ?
C17 N3 C21 112.1(5) . . ?
C18 N3 C21 114.8(5) . . ?
C27 N5 C25 116.3(7) . . ?
C27 N5 Ni2 113.3(5) . . ?
C25 N5 Ni2 104.3(5) . . ?
C27 N5 H5 107.5 . . ?
C25 N5 H5 107.5 . . ?
Ni2 N5 H5 107.5 . . ?
C24 N6 C26 112.7(6) . . ?
C24 N6 Ni2 105.9(5) . . ?
C26 N6 Ni2 112.6(5) . . ?
C24 N6 H6 108.5 . . ?
C26 N6 H6 108.5 . . ?
Ni2 N6 H6 108.5 . . ?
C26 N7 C27 121.4(8) . . ?
C26 N7 C28 117.2(10) . . ?
C27 N7 C28 115.1(10) . . ?
C34 N9 C32 113.3(5) . . ?
C34 N9 Ni3 111.7(4) . . ?
C32 N9 Ni3 105.7(4) . . ?
C34 N9 H9 108.7 . . ?
C32 N9 H9 108.7 . . ?
Ni3 N9 H9 108.7 . . ?
C33 N10 C31 114.5(5) . . ?
C33 N10 Ni3 114.6(4) . . ?
C31 N10 Ni3 105.6(4) . . ?
C33 N10 H10 107.2 . . ?
C31 N10 H10 107.2 . . ?
Ni3 N10 H10 107.2 . . ?
C33 N11 C35 114.6(6) . . ?
C33 N11 C34 115.9(6) . . ?
C35 N11 C34 114.4(6) . . ?
C41 N13 C39 112.2(5) . . ?
C41 N13 Ni4 113.6(4) . . ?
C39 N13 Ni4 107.8(4) . . ?
C41 N13 H13 107.7 . . ?
C39 N13 H13 107.7 . . ?
Ni4 N13 H13 107.7 . . ?
C38 N14 C40 112.4(5) . . ?
C38 N14 Ni4 106.5(4) . . ?
C40 N14 Ni4 113.0(4) . . ?
C38 N14 H14 108.3 . . ?
C40 N14 H14 108.3 . . ?
Ni4 N14 H14 108.3 . . ?
C40 N15 C41 117.3(6) . . ?
C40 N15 C42 116.5(6) . . ?
C41 N15 C42 113.2(6) . . ?
O1 C1 O2 126.3(6) . . ?
O1 C1 C2 116.5(5) . . ?
O2 C1 C2 117.0(6) . . ?
C7 C2 C3 118.5(5) . . ?
C7 C2 C1 121.0(5) . . ?
C3 C2 C1 120.4(6) . . ?
C2 C3 C4 119.4(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 122.2(5) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 C8 117.9(5) . . ?
C6 C5 C8 123.9(6) . . ?
C7 C6 C5 119.6(6) . . ?
C7 C6 C12 119.1(5) . . ?
C5 C6 C12 121.2(5) . . ?
C2 C7 C6 122.1(5) . . ?
C2 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
O3 C8 O4 125.5(6) . . ?
O3 C8 C5 120.8(6) . . ?
O4 C8 C5 113.5(5) . . ?
O5 C9 O6 126.5(6) . . ?
O5 C9 C10 116.1(7) . . ?
O6 C9 C10 117.4(6) . . ?
C15 C10 C11 118.6(6) . . ?
C15 C10 C9 121.2(6) . . ?
C11 C10 C9 120.2(6) . . ?
C10 C11 C12 121.9(6) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C13 119.1(6) . . ?
C11 C12 C6 116.2(6) . . ?
C13 C12 C6 124.7(5) . . ?
C14 C13 C12 117.3(6) . . ?
C14 C13 C16 117.6(6) . . ?
C12 C13 C16 125.0(6) . . ?
C13 C14 C15 123.0(7) . . ?
C13 C14 H14A 118.5 . . ?
C15 C14 H14A 118.5 . . ?
C10 C15 C14 120.0(6) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
O7 C16 O8 125.2(6) . . ?
O7 C16 C13 117.0(6) . . ?
O8 C16 C13 117.7(5) . . ?
N3 C17 N2 110.4(4) . . ?
N3 C17 H17A 109.6 . . ?
N2 C17 H17A 109.6 . . ?
N3 C17 H17B 109.6 . . ?
N2 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
N1 C18 N3 110.4(4) . . ?
N1 C18 H18A 109.6 . . ?
N3 C18 H18A 109.6 . . ?
N1 C18 H18B 109.6 . . ?
N3 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N1 C19 C20 108.1(5) . 2_565 ?
N1 C19 H19A 110.1 . . ?
C20 C19 H19A 110.1 2_565 . ?
N1 C19 H19B 110.1 . . ?
C20 C19 H19B 110.1 2_565 . ?
H19A C19 H19B 108.4 . . ?
N2 C20 C19 109.1(4) . 2_565 ?
N2 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 2_565 . ?
N2 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 2_565 . ?
H20A C20 H20B 108.3 . . ?
N3 C21 C22 115.8(5) . . ?
N3 C21 H21A 108.3 . . ?
C22 C21 H21A 108.3 . . ?
N3 C21 H21B 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C23 C22 C21 111.8(5) . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
N4 C23 C22 174.2(7) . . ?
N6 C24 C25 109.7(6) . 2_556 ?
N6 C24 H24A 109.7 . . ?
C25 C24 H24A 109.7 2_556 . ?
N6 C24 H24B 109.7 . . ?
C25 C24 H24B 109.7 2_556 . ?
H24A C24 H24B 108.2 . . ?
C24 C25 N5 110.6(6) 2_556 . ?
C24 C25 H25A 109.5 2_556 . ?
N5 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 2_556 . ?
N5 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
N7 C26 N6 113.6(8) . . ?
N7 C26 H26A 108.8 . . ?
N6 C26 H26A 108.8 . . ?
N7 C26 H26B 108.8 . . ?
N6 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
N7 C27 N5 112.4(7) . . ?
N7 C27 H27A 109.1 . . ?
N5 C27 H27A 109.1 . . ?
N7 C27 H27B 109.1 . . ?
N5 C27 H27B 109.1 . . ?
H27A C27 H27B 107.9 . . ?
N7 C28 C29 114.5(10) . . ?
N7 C28 H28A 108.6 . . ?
C29 C28 H28A 108.6 . . ?
N7 C28 H28B 108.6 . . ?
C29 C28 H28B 108.6 . . ?
H28A C28 H28B 107.6 . . ?
C28 C29 C30 118.9(11) . . ?
C28 C29 H29A 107.6 . . ?
C30 C29 H29A 107.6 . . ?
C28 C29 H29B 107.6 . . ?
C30 C29 H29B 107.6 . . ?
H29A C29 H29B 107.0 . . ?
N8 C30 C29 175.7(13) . . ?
N10 C31 C32 108.7(5) . 2_655 ?
N10 C31 H31A 109.9 . . ?
C32 C31 H31A 109.9 2_655 . ?
N10 C31 H31B 109.9 . . ?
C32 C31 H31B 109.9 2_655 . ?
H31A C31 H31B 108.3 . . ?
N9 C32 C31 107.8(5) . 2_655 ?
N9 C32 H32A 110.1 . . ?
C31 C32 H32A 110.1 2_655 . ?
N9 C32 H32B 110.1 . . ?
C31 C32 H32B 110.1 2_655 . ?
H32A C32 H32B 108.5 . . ?
N11 C33 N10 114.6(5) . . ?
N11 C33 H33A 108.6 . . ?
N10 C33 H33A 108.6 . . ?
N11 C33 H33B 108.6 . . ?
N10 C33 H33B 108.6 . . ?
H33A C33 H33B 107.6 . . ?
N11 C34 N9 112.7(5) . . ?
N11 C34 H34A 109.0 . . ?
N9 C34 H34A 109.0 . . ?
N11 C34 H34B 109.0 . . ?
N9 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
N11 C35 C36 113.2(7) . . ?
N11 C35 H35A 108.9 . . ?
C36 C35 H35A 108.9 . . ?
N11 C35 H35B 108.9 . . ?
C36 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C37 C36 C35 112.1(7) . . ?
C37 C36 H36A 109.2 . . ?
C35 C36 H36A 109.2 . . ?
C37 C36 H36B 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
N12 C37 C36 176.2(10) . . ?
N14 C38 C39 108.2(6) . 2_566 ?
N14 C38 H38A 110.1 . . ?
C39 C38 H38A 110.1 2_566 . ?
N14 C38 H38B 110.1 . . ?
C39 C38 H38B 110.1 2_566 . ?
H38A C38 H38B 108.4 . . ?
N13 C39 C38 107.7(6) . 2_566 ?
N13 C39 H39A 110.2 . . ?
C38 C39 H39A 110.2 2_566 . ?
N13 C39 H39B 110.2 . . ?
C38 C39 H39B 110.2 2_566 . ?
H39A C39 H39B 108.5 . . ?
N15 C40 N14 112.8(5) . . ?
N15 C40 H40A 109.0 . . ?
N14 C40 H40A 109.0 . . ?
N15 C40 H40B 109.0 . . ?
N14 C40 H40B 109.0 . . ?
H40A C40 H40B 107.8 . . ?
N15 C41 N13 114.8(5) . . ?
N15 C41 H41A 108.6 . . ?
N13 C41 H41A 108.6 . . ?
N15 C41 H41B 108.6 . . ?
N13 C41 H41B 108.6 . . ?
H41A C41 H41B 107.5 . . ?
N15 C42 C43 111.8(6) . . ?
N15 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
N15 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 111.5(7) . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
C42 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
N16 C44 C43 177.2(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 O1 19.1(11) . . . . ?
Ni1 O2 C1 C2 -156.1(4) . . . . ?
O1 C1 C2 C7 -167.7(6) . . . . ?
O2 C1 C2 C7 7.9(9) . . . . ?
O1 C1 C2 C3 7.7(10) . . . . ?
O2 C1 C2 C3 -176.6(6) . . . . ?
C7 C2 C3 C4 -2.2(9) . . . . ?
C1 C2 C3 C4 -177.8(6) . . . . ?
C2 C3 C4 C5 0.9(10) . . . . ?
C3 C4 C5 C6 1.1(10) . . . . ?
C3 C4 C5 C8 -177.4(6) . . . . ?
C4 C5 C6 C7 -1.7(9) . . . . ?
C8 C5 C6 C7 176.8(6) . . . . ?
C4 C5 C6 C12 -176.9(6) . . . . ?
C8 C5 C6 C12 1.5(10) . . . . ?
C3 C2 C7 C6 1.7(9) . . . . ?
C1 C2 C7 C6 177.2(6) . . . . ?
C5 C6 C7 C2 0.3(10) . . . . ?
C12 C6 C7 C2 175.7(6) . . . . ?
Ni2 O4 C8 O3 13.7(12) . . . . ?
Ni2 O4 C8 C5 -161.8(4) . . . . ?
C4 C5 C8 O3 -57.2(10) . . . . ?
C6 C5 C8 O3 124.3(7) . . . . ?
C4 C5 C8 O4 118.5(7) . . . . ?
C6 C5 C8 O4 -59.9(9) . . . . ?
Ni3 O6 C9 O5 -14.8(11) . . . . ?
Ni3 O6 C9 C10 163.8(4) . . . . ?
O5 C9 C10 C15 9.2(10) . . . . ?
O6 C9 C10 C15 -169.6(6) . . . . ?
O5 C9 C10 C11 -171.8(6) . . . . ?
O6 C9 C10 C11 9.5(9) . . . . ?
C15 C10 C11 C12 -1.2(9) . . . . ?
C9 C10 C11 C12 179.7(5) . . . . ?
C10 C11 C12 C13 2.2(9) . . . . ?
C10 C11 C12 C6 -176.6(5) . . . . ?
C7 C6 C12 C11 -60.2(8) . . . . ?
C5 C6 C12 C11 115.1(6) . . . . ?
C7 C6 C12 C13 121.1(7) . . . . ?
C5 C6 C12 C13 -63.7(9) . . . . ?
C11 C12 C13 C14 -2.6(8) . . . . ?
C6 C12 C13 C14 176.1(6) . . . . ?
C11 C12 C13 C16 176.3(6) . . . . ?
C6 C12 C13 C16 -5.0(9) . . . . ?
C12 C13 C14 C15 2.1(10) . . . . ?
C16 C13 C14 C15 -176.9(6) . . . . ?
C11 C10 C15 C14 0.6(9) . . . . ?
C9 C10 C15 C14 179.7(6) . . . . ?
C13 C14 C15 C10 -1.1(10) . . . . ?
Ni4 O8 C16 O7 4.0(11) . . . . ?
Ni4 O8 C16 C13 -172.7(4) . . . . ?
C14 C13 C16 O7 -37.5(9) . . . . ?
C12 C13 C16 O7 143.6(7) . . . . ?
C14 C13 C16 O8 139.4(7) . . . . ?
C12 C13 C16 O8 -39.5(9) . . . . ?
C18 N3 C17 N2 -77.9(6) . . . . ?
C21 N3 C17 N2 148.7(5) . . . . ?
C20 N2 C17 N3 -179.6(5) . . . . ?
Ni1 N2 C17 N3 62.2(6) . . . . ?
C19 N1 C18 N3 -176.2(4) . . . . ?
Ni1 N1 C18 N3 -54.3(6) . . . . ?
C17 N3 C18 N1 71.8(6) . . . . ?
C21 N3 C18 N1 -156.0(5) . . . . ?
C18 N1 C19 C20 172.6(5) . . . 2_565 ?
Ni1 N1 C19 C20 42.4(5) . . . 2_565 ?
C17 N2 C20 C19 -167.1(5) . . . 2_565 ?
Ni1 N2 C20 C19 -43.1(5) . . . 2_565 ?
C17 N3 C21 C22 68.2(7) . . . . ?
C18 N3 C21 C22 -65.3(6) . . . . ?
N3 C21 C22 C23 78.3(7) . . . . ?
C26 N6 C24 C25 -164.9(7) . . . 2_556 ?
Ni2 N6 C24 C25 -41.3(6) . . . 2_556 ?
C27 N5 C25 C24 163.9(7) . . . 2_556 ?
Ni2 N5 C25 C24 38.3(7) . . . 2_556 ?
C27 N7 C26 N6 -71.4(11) . . . . ?
C28 N7 C26 N6 79.4(11) . . . . ?
C24 N6 C26 N7 175.6(7) . . . . ?
Ni2 N6 C26 N7 55.8(9) . . . . ?
C26 N7 C27 N5 70.0(11) . . . . ?
C28 N7 C27 N5 -81.5(11) . . . . ?
C25 N5 C27 N7 -175.1(7) . . . . ?
Ni2 N5 C27 N7 -54.2(9) . . . . ?
C26 N7 C28 C29 113.5(12) . . . . ?
C27 N7 C28 C29 -93.8(12) . . . . ?
N7 C28 C29 C30 -176.0(10) . . . . ?
C33 N10 C31 C32 -169.0(6) . . . 2_655 ?
Ni3 N10 C31 C32 -42.0(6) . . . 2_655 ?
C34 N9 C32 C31 164.9(5) . . . 2_655 ?
Ni3 N9 C32 C31 42.3(6) . . . 2_655 ?
C35 N11 C33 N10 66.3(8) . . . . ?
C34 N11 C33 N10 -70.4(8) . . . . ?
C31 N10 C33 N11 176.9(6) . . . . ?
Ni3 N10 C33 N11 54.6(8) . . . . ?
C33 N11 C34 N9 74.0(8) . . . . ?
C35 N11 C34 N9 -62.8(8) . . . . ?
C32 N9 C34 N11 -179.2(6) . . . . ?
Ni3 N9 C34 N11 -59.9(7) . . . . ?
C33 N11 C35 C36 165.9(6) . . . . ?
C34 N11 C35 C36 -56.8(8) . . . . ?
N11 C35 C36 C37 -37.9(9) . . . . ?
C40 N14 C38 C39 -165.6(6) . . . 2_566 ?
Ni4 N14 C38 C39 -41.3(7) . . . 2_566 ?
C41 N13 C39 C38 166.3(5) . . . 2_566 ?
Ni4 N13 C39 C38 40.6(6) . . . 2_566 ?
C41 N15 C40 N14 -69.4(8) . . . . ?
C42 N15 C40 N14 69.4(7) . . . . ?
C38 N14 C40 N15 177.1(6) . . . . ?
Ni4 N14 C40 N15 56.4(7) . . . . ?
C40 N15 C41 N13 70.0(7) . . . . ?
C42 N15 C41 N13 -70.1(7) . . . . ?
C39 N13 C41 N15 -178.8(6) . . . . ?
Ni4 N13 C41 N15 -56.3(7) . . . . ?
C40 N15 C42 C43 64.1(7) . . . . ?
C41 N15 C42 C43 -155.4(6) . . . . ?
N15 C42 C43 C44 61.9(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 1.00 1.93 2.864(6) 154.8 2_565 yes
N6 H6 O3 1.00 2.20 3.050(7) 141.8 . yes
N9 H9 N4 1.00 2.13 3.115(9) 167.7 . yes
N10 H10 O5 1.00 1.89 2.813(7) 152.2 . yes
N13 H13 O7 1.00 1.91 2.833(7) 152.1 2_566 yes
N14 H14 O3 1.00 2.53 3.502(7) 165.3 2_566 yes

_refine_diff_density_max         0.631
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.091



# start Validation Reply Form
_vrf_PLAT029_cp_CN_sq            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.932 Why?
RESPONSE: Since the Pohang Accelerator Laboratory 2D-SMC beamline
goniostat has only one omega-axis, diffrn_measured_fraction_theta_full value is not
fully covered as 0.932, especially for the low symmetry such as the monoclinic and
triclinic system. As this is an inherent problem, other shelx OMIT command were not
helpful to improve the completeness.
;
# 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_cp_OH_sq
_database_code_depnum_ccdc_archive 'CCDC 1898505'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        cp-flexMOF(OH)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H132 N24 Ni4 O24'
_chemical_formula_sum            'C80 H132 N24 Ni4 O24'
_chemical_formula_weight         2048.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.819(3)
_cell_length_b                   15.316(3)
_cell_length_c                   16.301(3)
_cell_angle_alpha                90.994(10)
_cell_angle_beta                 103.450(7)
_cell_angle_gamma                90.421(10)
_cell_volume                     2383.7(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    39647
_cell_measurement_theta_min      1.803
_cell_measurement_theta_max      32.838

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             1084
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.824
_shelx_estimated_absorpt_T_min   0.960
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15154
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.803
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.920
_reflns_number_total             8088
_reflns_number_gt                4866
_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       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  CIFTAB
_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)+(0.1810P)²] 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         8088
_refine_ls_number_parameters     605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2616
_refine_ls_wR_factor_gt          0.2282
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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 0.500000 1.000000 0.000000 0.0654(3) Uani 1 2 d S . P . .
Ni2 Ni 1.000000 1.000000 0.500000 0.0669(3) Uani 1 2 d S . P . .
Ni3 Ni 0.500000 0.500000 0.000000 0.0682(4) Uani 1 2 d S . P . .
Ni4 Ni 0.500000 0.500000 0.500000 0.0711(4) Uani 1 2 d S . P . .
O1 O 0.3484(5) 0.7842(3) -0.0114(3) 0.0823(13) Uani 1 1 d . . . . .
O2 O 0.4663(5) 0.8903(3) 0.0712(2) 0.0704(11) Uani 1 1 d . . . . .
O3 O 1.0251(5) 0.9776(3) 0.2893(2) 0.0767(12) Uani 1 1 d . . . . .
O4 O 0.8975(5) 0.9375(3) 0.3812(2) 0.0754(12) Uani 1 1 d . . . . .
O5 O 0.6724(6) 0.6937(3) -0.0159(3) 0.0903(15) Uani 1 1 d . . . . .
O6 O 0.5824(5) 0.6158(3) 0.0731(2) 0.0714(11) Uani 1 1 d . . . . .
O7 O 0.2359(5) 0.6254(3) 0.3749(3) 0.0809(12) Uani 1 1 d . . . . .
O8 O 0.4598(5) 0.5860(3) 0.3949(3) 0.0761(12) Uani 1 1 d . . . . .
O9 O 0.8566(7) 0.7308(4) -0.1022(4) 0.1095(17) Uani 1 1 d . . . . .
H9 H 0.798046 0.734821 -0.072115 0.164 Uiso 1 1 calc R U . . .
O10 O 1.3090(7) 0.9983(5) 0.3105(4) 0.124(2) Uani 1 1 d . . . . .
H10A H 1.223695 0.991334 0.309469 0.186 Uiso 1 1 calc R U . . .
O11 O 0.1989(6) 0.7505(4) -0.1764(3) 0.0923(14) Uani 1 1 d . . . . .
H11 H 0.243595 0.760798 -0.126615 0.138 Uiso 1 1 calc R U . . .
O12 O 0.2472(6) 0.3532(5) 0.2498(3) 0.118(2) Uani 1 1 d . . . . .
H12 H 0.227086 0.341054 0.197868 0.177 Uiso 1 1 calc R U . . .
N1 N 0.7074(6) 0.9686(3) 0.0324(3) 0.0695(13) Uani 1 1 d . . . . .
H1 H 0.714257 0.908283 0.055425 0.083 Uiso 1 1 calc R U . . .
N2 N 0.4657(6) 0.9278(4) -0.1097(3) 0.0708(13) Uani 1 1 d . . . . .
H2 H 0.454142 0.865193 -0.095989 0.085 Uiso 1 1 calc R U . . .
N3 N 0.7114(6) 0.9050(4) -0.1027(3) 0.0816(16) Uani 1 1 d . . . . .
N4 N 1.1079(6) 0.8870(4) 0.5292(3) 0.0778(15) Uani 1 1 d . . . . .
H4 H 1.092288 0.850462 0.476337 0.093 Uiso 1 1 calc R U . . .
N5 N 1.1472(6) 1.0556(4) 0.4485(3) 0.0746(14) Uani 1 1 d . . . . .
H5 H 1.131741 1.031521 0.389564 0.090 Uiso 1 1 calc R U . . .
N6 N 1.3240(6) 0.9460(5) 0.5002(3) 0.0850(16) Uani 1 1 d . . . . .
N7 N 0.5928(6) 0.5288(4) -0.0966(3) 0.0723(14) Uani 1 1 d . . . . .
H7 H 0.630257 0.589886 -0.086577 0.087 Uiso 1 1 calc R U . . .
N8 N 0.3208(6) 0.5676(4) -0.0492(3) 0.0761(14) Uani 1 1 d . . . . .
H8 H 0.340132 0.631077 -0.035608 0.091 Uiso 1 1 calc R U . . .
N9 N 0.3766(6) 0.5815(4) -0.1891(3) 0.0761(14) Uani 1 1 d . . . . .
N10 N 0.4625(6) 0.3985(4) 0.4159(3) 0.0782(15) Uani 1 1 d . . . . .
H10 H 0.421910 0.423226 0.359125 0.094 Uiso 1 1 calc R U . . .
N11 N 0.2956(6) 0.5056(4) 0.5114(3) 0.0787(15) Uani 1 1 d . . . . .
H11A H 0.242145 0.538144 0.461736 0.094 Uiso 1 1 calc R U . . .
N12 N 0.2268(6) 0.3672(4) 0.4372(3) 0.0795(15) Uani 1 1 d . . . . .
C1 C 0.4044(7) 0.8181(4) 0.0578(4) 0.0675(15) Uani 1 1 d . . . . .
C2 C 0.3949(6) 0.7680(4) 0.1373(3) 0.0618(14) Uani 1 1 d . . . . .
C3 C 0.2635(7) 0.7488(4) 0.1505(4) 0.0690(16) Uani 1 1 d . . . . .
H3 H 0.182081 0.765441 0.110037 0.083 Uiso 1 1 calc R U . . .
C4 C 0.2502(7) 0.7059(4) 0.2218(3) 0.0682(16) Uani 1 1 d . . . . .
H4A H 0.159603 0.695266 0.231158 0.082 Uiso 1 1 calc R U . . .
C5 C 0.3671(7) 0.6781(4) 0.2800(3) 0.0677(16) Uani 1 1 d . . . . .
C6 C 0.4979(7) 0.6971(4) 0.2675(3) 0.0673(15) Uani 1 1 d . . . . .
H6 H 0.578322 0.678433 0.307686 0.081 Uiso 1 1 calc R U . . .
C7 C 0.5158(6) 0.7432(4) 0.1971(3) 0.0625(14) Uani 1 1 d . . . . .
C8 C 0.3501(8) 0.6257(4) 0.3561(4) 0.0713(17) Uani 1 1 d . . . . .
C9 C 0.9344(7) 0.9299(4) 0.3120(4) 0.0715(16) Uani 1 1 d . . . . .
C10 C 0.8630(7) 0.8598(4) 0.2498(4) 0.0675(15) Uani 1 1 d . . . . .
C11 C 0.7332(6) 0.8266(4) 0.2527(3) 0.0634(14) Uani 1 1 d . . . . .
H11B H 0.692883 0.844045 0.297895 0.076 Uiso 1 1 calc R U . . .
C12 C 0.6596(7) 0.7685(4) 0.1914(3) 0.0645(15) Uani 1 1 d . . . . .
C13 C 0.7189(7) 0.7416(4) 0.1261(4) 0.0646(15) Uani 1 1 d . . . . .
C14 C 0.8548(7) 0.7737(4) 0.1263(4) 0.0695(16) Uani 1 1 d . . . . .
H14 H 0.898837 0.753392 0.083607 0.083 Uiso 1 1 calc R U . . .
C15 C 0.9245(7) 0.8323(4) 0.1847(3) 0.0672(15) Uani 1 1 d . . . . .
H15 H 1.013759 0.854222 0.181497 0.081 Uiso 1 1 calc R U . . .
C16 C 0.6519(7) 0.6798(4) 0.0559(4) 0.0730(17) Uani 1 1 d . . . . .
C17 C 0.3295(7) 0.9587(5) -0.1602(4) 0.0737(17) Uani 1 1 d . . . . .
H17A H 0.290572 0.915798 -0.205882 0.088 Uiso 1 1 calc R U . . .
H17B H 0.342951 1.015108 -0.186237 0.088 Uiso 1 1 calc R U . . .
C18 C 0.7705(7) 1.0301(4) 0.1031(4) 0.0734(17) Uani 1 1 d . . . . .
H18A H 0.789360 1.087308 0.080354 0.088 Uiso 1 1 calc R U . . .
H18B H 0.860484 1.006775 0.135433 0.088 Uiso 1 1 calc R U . . .
C19 C 0.5797(7) 0.9337(5) -0.1551(4) 0.0784(18) Uani 1 1 d . . . . .
H19A H 0.555375 0.897054 -0.207189 0.094 Uiso 1 1 calc R U . . .
H19B H 0.589792 0.994910 -0.171687 0.094 Uiso 1 1 calc R U . . .
C20 C 0.7785(8) 0.9691(5) -0.0370(4) 0.0804(18) Uani 1 1 d . . . . .
H20A H 0.878359 0.954309 -0.015642 0.096 Uiso 1 1 calc R U . . .
H20B H 0.773959 1.028102 -0.061214 0.096 Uiso 1 1 calc R U . . .
C21 C 0.8133(9) 0.8785(6) -0.1521(5) 0.095(2) Uani 1 1 d . . . . .
H21A H 0.864290 0.931042 -0.164041 0.114 Uiso 1 1 calc R U . . .
H21B H 0.761854 0.852898 -0.206856 0.114 Uiso 1 1 calc R U . . .
C22 C 0.9167(9) 0.8140(6) -0.1083(5) 0.102(2) Uani 1 1 d . . . . .
H22A H 0.991901 0.807747 -0.139139 0.122 Uiso 1 1 calc R U . . .
H22B H 0.959922 0.836588 -0.050792 0.122 Uiso 1 1 calc R U . . .
C23 C 1.0409(9) 0.8411(5) 0.5881(4) 0.090(2) Uani 1 1 d . . . . .
H23A H 1.073495 0.866398 0.645721 0.108 Uiso 1 1 calc R U . . .
H23B H 1.065616 0.778495 0.589573 0.108 Uiso 1 1 calc R U . . .
C24 C 1.1144(8) 1.1491(5) 0.4414(4) 0.087(2) Uani 1 1 d . . . . .
H24A H 1.161986 1.176230 0.400761 0.105 Uiso 1 1 calc R U . . .
H24B H 1.147899 1.178930 0.496912 0.105 Uiso 1 1 calc R U . . .
C25 C 1.2936(7) 1.0358(6) 0.4910(4) 0.086(2) Uani 1 1 d . . . . .
H25A H 1.356421 1.062179 0.458497 0.103 Uiso 1 1 calc R U . . .
H25B H 1.315058 1.064147 0.547628 0.103 Uiso 1 1 calc R U . . .
C26 C 1.2620(8) 0.9010(5) 0.5595(4) 0.0849(19) Uani 1 1 d . . . . .
H26A H 1.280617 0.935108 0.613193 0.102 Uiso 1 1 calc R U . . .
H26B H 1.307433 0.843598 0.571248 0.102 Uiso 1 1 calc R U . . .
C27 C 1.3226(10) 0.8924(7) 0.4217(5) 0.113(3) Uani 1 1 d . . . . .
H27A H 1.367228 0.835874 0.439423 0.135 Uiso 1 1 calc R U . . .
H27B H 1.223605 0.879624 0.393544 0.135 Uiso 1 1 calc R U . . .
C28 C 1.3900(11) 0.9286(8) 0.3595(6) 0.127(3) Uani 1 1 d . . . . .
H28A H 1.404480 0.881248 0.320446 0.153 Uiso 1 1 calc R U . . .
H28B H 1.483259 0.952175 0.388581 0.153 Uiso 1 1 calc R U . . .
C29 C 0.7109(8) 0.4721(5) -0.0897(4) 0.0820(19) Uani 1 1 d . . . . .
H29A H 0.777616 0.496911 -0.120424 0.098 Uiso 1 1 calc R U . . .
H29B H 0.679187 0.414111 -0.115060 0.098 Uiso 1 1 calc R U . . .
C30 C 0.2173(8) 0.5374(5) -0.0031(4) 0.086(2) Uani 1 1 d . . . . .
H30A H 0.176644 0.480509 -0.026947 0.103 Uiso 1 1 calc R U . . .
H30B H 0.140411 0.579993 -0.008991 0.103 Uiso 1 1 calc R U . . .
C31 C 0.4934(8) 0.5259(5) -0.1814(4) 0.081(2) Uani 1 1 d . . . . .
H31A H 0.545272 0.542040 -0.224349 0.097 Uiso 1 1 calc R U . . .
H31B H 0.458906 0.465104 -0.194059 0.097 Uiso 1 1 calc R U . . .
C32 C 0.2729(8) 0.5568(5) -0.1438(4) 0.0823(19) Uani 1 1 d . . . . .
H32A H 0.245936 0.494887 -0.157596 0.099 Uiso 1 1 calc R U . . .
H32B H 0.188360 0.592448 -0.163655 0.099 Uiso 1 1 calc R U . . .
C33 C 0.4120(9) 0.6744(5) -0.1861(4) 0.0842(19) Uani 1 1 d . . . . .
H33A H 0.490406 0.683021 -0.214028 0.101 Uiso 1 1 calc R U . . .
H33B H 0.445040 0.693450 -0.126386 0.101 Uiso 1 1 calc R U . . .
C34 C 0.2936(9) 0.7310(5) -0.2272(4) 0.087(2) Uani 1 1 d . . . . .
H34A H 0.332415 0.786367 -0.243042 0.105 Uiso 1 1 calc R U . . .
H34B H 0.241589 0.701458 -0.279850 0.105 Uiso 1 1 calc R U . . .
C35 C 0.5988(8) 0.3644(5) 0.4139(4) 0.086(2) Uani 1 1 d . . . . .
H35A H 0.591155 0.326766 0.362999 0.103 Uiso 1 1 calc R U . . .
H35B H 0.633834 0.328483 0.464140 0.103 Uiso 1 1 calc R U . . .
C36 C 0.3006(8) 0.5620(5) 0.5873(4) 0.085(2) Uani 1 1 d . . . . .
H36A H 0.332011 0.527774 0.639115 0.102 Uiso 1 1 calc R U . . .
H36B H 0.206360 0.585064 0.586355 0.102 Uiso 1 1 calc R U . . .
C37 C 0.3595(8) 0.3315(5) 0.4326(4) 0.087(2) Uani 1 1 d . . . . .
H37A H 0.344221 0.286250 0.387200 0.105 Uiso 1 1 calc R U . . .
H37B H 0.400756 0.302725 0.486455 0.105 Uiso 1 1 calc R U . . .
C38 C 0.2256(8) 0.4204(5) 0.5101(4) 0.0820(19) Uani 1 1 d . . . . .
H38A H 0.271731 0.388376 0.561072 0.098 Uiso 1 1 calc R U . . .
H38B H 0.127116 0.430072 0.512826 0.098 Uiso 1 1 calc R U . . .
C39 C 0.1376(9) 0.4021(7) 0.3577(5) 0.113(3) Uani 1 1 d . . . . .
H39A H 0.042800 0.412056 0.366982 0.135 Uiso 1 1 calc R U . . .
H39B H 0.176457 0.459725 0.347626 0.135 Uiso 1 1 calc R U . . .
C40 C 0.1232(10) 0.3489(7) 0.2814(5) 0.122(3) Uani 1 1 d . . . . .
H40A H 0.104280 0.287481 0.293685 0.146 Uiso 1 1 calc R U . . .
H40B H 0.042549 0.369470 0.237875 0.146 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 N1 2.045(5) . ?
Ni1 N1 2.045(5) 2_675 ?
Ni1 N2 2.045(5) . ?
Ni1 N2 2.045(5) 2_675 ?
Ni1 O2 2.126(4) 2_675 ?
Ni1 O2 2.126(4) . ?
Ni2 N5 2.023(5) 2_776 ?
Ni2 N5 2.023(5) . ?
Ni2 N4 2.041(6) . ?
Ni2 N4 2.041(6) 2_776 ?
Ni2 O4 2.167(4) . ?
Ni2 O4 2.167(4) 2_776 ?
Ni3 N7 2.047(5) . ?
Ni3 N7 2.047(5) 2_665 ?
Ni3 N8 2.053(6) 2_665 ?
Ni3 N8 2.053(6) . ?
Ni3 O6 2.162(4) 2_665 ?
Ni3 O6 2.162(4) . ?
Ni4 N10 2.028(6) 2_666 ?
Ni4 N10 2.028(6) . ?
Ni4 N11 2.061(6) . ?
Ni4 N11 2.061(6) 2_666 ?
Ni4 O8 2.143(4) . ?
Ni4 O8 2.143(4) 2_666 ?
O1 C1 1.237(7) . ?
O2 C1 1.249(7) . ?
O3 C9 1.272(8) . ?
O4 C9 1.265(7) . ?
O5 C16 1.256(7) . ?
O6 C16 1.262(7) . ?
O7 C8 1.229(8) . ?
O8 C8 1.280(8) . ?
O9 C22 1.414(10) . ?
O9 H9 0.8400 . ?
O10 C28 1.469(11) . ?
O10 H10A 0.8400 . ?
O11 C34 1.413(8) . ?
O11 H11 0.8400 . ?
O12 C40 1.430(10) . ?
O12 H12 0.8400 . ?
N1 C20 1.460(8) . ?
N1 C18 1.490(8) . ?
N1 H1 1.0000 . ?
N2 C19 1.482(8) . ?
N2 C17 1.483(8) . ?
N2 H2 1.0000 . ?
N3 C19 1.450(9) . ?
N3 C20 1.473(9) . ?
N3 C21 1.478(9) . ?
N4 C23 1.470(8) . ?
N4 C26 1.491(9) . ?
N4 H4 1.0000 . ?
N5 C24 1.471(9) . ?
N5 C25 1.479(9) . ?
N5 H5 1.0000 . ?
N6 C25 1.413(10) . ?
N6 C26 1.439(9) . ?
N6 C27 1.506(10) . ?
N7 C29 1.438(9) . ?
N7 C31 1.494(8) . ?
N7 H7 1.0000 . ?
N8 C30 1.474(9) . ?
N8 C32 1.509(8) . ?
N8 H8 1.0000 . ?
N9 C31 1.418(9) . ?
N9 C32 1.442(8) . ?
N9 C33 1.460(9) . ?
N10 C35 1.448(9) . ?
N10 C37 1.508(9) . ?
N10 H10 1.0000 . ?
N11 C38 1.467(9) . ?
N11 C36 1.487(8) . ?
N11 H11A 1.0000 . ?
N12 C38 1.432(9) . ?
N12 C37 1.434(10) . ?
N12 C39 1.494(10) . ?
C1 C2 1.538(8) . ?
C2 C3 1.387(8) . ?
C2 C7 1.409(8) . ?
C3 C4 1.378(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.377(9) . ?
C5 C8 1.528(8) . ?
C6 C7 1.403(8) . ?
C6 H6 0.9500 . ?
C7 C12 1.485(8) . ?
C9 C10 1.516(8) . ?
C10 C11 1.379(8) . ?
C10 C15 1.397(8) . ?
C11 C12 1.392(8) . ?
C11 H11B 0.9500 . ?
C12 C13 1.385(8) . ?
C13 C14 1.418(9) . ?
C13 C16 1.497(8) . ?
C14 C15 1.355(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.512(9) 2_675 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.490(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.498(11) 2_776 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.449(12) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.523(9) 2_665 ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.491(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.496(10) 2_666 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.453(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 . 2_675 ?
N1 Ni1 N2 92.7(2) . . ?
N1 Ni1 N2 87.3(2) 2_675 . ?
N1 Ni1 N2 87.3(2) . 2_675 ?
N1 Ni1 N2 92.7(2) 2_675 2_675 ?
N2 Ni1 N2 180.0(3) . 2_675 ?
N1 Ni1 O2 93.78(19) . 2_675 ?
N1 Ni1 O2 86.22(19) 2_675 2_675 ?
N2 Ni1 O2 87.49(18) . 2_675 ?
N2 Ni1 O2 92.51(18) 2_675 2_675 ?
N1 Ni1 O2 86.22(19) . . ?
N1 Ni1 O2 93.78(19) 2_675 . ?
N2 Ni1 O2 92.51(18) . . ?
N2 Ni1 O2 87.49(18) 2_675 . ?
O2 Ni1 O2 180.0 2_675 . ?
N5 Ni2 N5 180.0 2_776 . ?
N5 Ni2 N4 85.6(2) 2_776 . ?
N5 Ni2 N4 94.4(2) . . ?
N5 Ni2 N4 94.4(2) 2_776 2_776 ?
N5 Ni2 N4 85.6(2) . 2_776 ?
N4 Ni2 N4 180.0 . 2_776 ?
N5 Ni2 O4 87.94(18) 2_776 . ?
N5 Ni2 O4 92.06(18) . . ?
N4 Ni2 O4 87.4(2) . . ?
N4 Ni2 O4 92.6(2) 2_776 . ?
N5 Ni2 O4 92.06(18) 2_776 2_776 ?
N5 Ni2 O4 87.94(18) . 2_776 ?
N4 Ni2 O4 92.6(2) . 2_776 ?
N4 Ni2 O4 87.4(2) 2_776 2_776 ?
O4 Ni2 O4 180.0(2) . 2_776 ?
N7 Ni3 N7 180.0 . 2_665 ?
N7 Ni3 N8 85.6(2) . 2_665 ?
N7 Ni3 N8 94.4(2) 2_665 2_665 ?
N7 Ni3 N8 94.4(2) . . ?
N7 Ni3 N8 85.6(2) 2_665 . ?
N8 Ni3 N8 180.0 2_665 . ?
N7 Ni3 O6 86.26(18) . 2_665 ?
N7 Ni3 O6 93.74(18) 2_665 2_665 ?
N8 Ni3 O6 88.52(19) 2_665 2_665 ?
N8 Ni3 O6 91.48(19) . 2_665 ?
N7 Ni3 O6 93.74(18) . . ?
N7 Ni3 O6 86.26(18) 2_665 . ?
N8 Ni3 O6 91.48(19) 2_665 . ?
N8 Ni3 O6 88.52(19) . . ?
O6 Ni3 O6 180.0 2_665 . ?
N10 Ni4 N10 180.0(2) 2_666 . ?
N10 Ni4 N11 86.0(2) 2_666 . ?
N10 Ni4 N11 94.0(2) . . ?
N10 Ni4 N11 94.0(2) 2_666 2_666 ?
N10 Ni4 N11 86.0(2) . 2_666 ?
N11 Ni4 N11 180.00(3) . 2_666 ?
N10 Ni4 O8 92.11(19) 2_666 . ?
N10 Ni4 O8 87.89(19) . . ?
N11 Ni4 O8 92.31(19) . . ?
N11 Ni4 O8 87.69(19) 2_666 . ?
N10 Ni4 O8 87.89(19) 2_666 2_666 ?
N10 Ni4 O8 92.11(19) . 2_666 ?
N11 Ni4 O8 87.69(19) . 2_666 ?
N11 Ni4 O8 92.31(19) 2_666 2_666 ?
O8 Ni4 O8 180.0(3) . 2_666 ?
C1 O2 Ni1 137.5(4) . . ?
C9 O4 Ni2 131.2(4) . . ?
C16 O6 Ni3 131.1(4) . . ?
C8 O8 Ni4 133.0(4) . . ?
C22 O9 H9 109.5 . . ?
C28 O10 H10A 109.5 . . ?
C34 O11 H11 109.5 . . ?
C40 O12 H12 109.5 . . ?
C20 N1 C18 113.7(5) . . ?
C20 N1 Ni1 115.1(4) . . ?
C18 N1 Ni1 104.9(4) . . ?
C20 N1 H1 107.6 . . ?
C18 N1 H1 107.6 . . ?
Ni1 N1 H1 107.6 . . ?
C19 N2 C17 112.9(5) . . ?
C19 N2 Ni1 114.4(4) . . ?
C17 N2 Ni1 104.6(4) . . ?
C19 N2 H2 108.2 . . ?
C17 N2 H2 108.2 . . ?
Ni1 N2 H2 108.2 . . ?
C19 N3 C20 114.0(6) . . ?
C19 N3 C21 112.9(5) . . ?
C20 N3 C21 109.1(6) . . ?
C23 N4 C26 114.9(6) . . ?
C23 N4 Ni2 106.4(5) . . ?
C26 N4 Ni2 113.4(4) . . ?
C23 N4 H4 107.3 . . ?
C26 N4 H4 107.3 . . ?
Ni2 N4 H4 107.3 . . ?
C24 N5 C25 115.0(6) . . ?
C24 N5 Ni2 106.3(4) . . ?
C25 N5 Ni2 115.0(4) . . ?
C24 N5 H5 106.6 . . ?
C25 N5 H5 106.6 . . ?
Ni2 N5 H5 106.6 . . ?
C25 N6 C26 115.9(6) . . ?
C25 N6 C27 117.9(6) . . ?
C26 N6 C27 112.9(7) . . ?
C29 N7 C31 114.1(5) . . ?
C29 N7 Ni3 107.3(4) . . ?
C31 N7 Ni3 113.4(4) . . ?
C29 N7 H7 107.2 . . ?
C31 N7 H7 107.2 . . ?
Ni3 N7 H7 107.2 . . ?
C30 N8 C32 113.8(5) . . ?
C30 N8 Ni3 105.4(4) . . ?
C32 N8 Ni3 112.8(4) . . ?
C30 N8 H8 108.2 . . ?
C32 N8 H8 108.2 . . ?
Ni3 N8 H8 108.2 . . ?
C31 N9 C32 116.5(6) . . ?
C31 N9 C33 114.0(6) . . ?
C32 N9 C33 115.7(5) . . ?
C35 N10 C37 114.7(6) . . ?
C35 N10 Ni4 105.6(4) . . ?
C37 N10 Ni4 114.4(4) . . ?
C35 N10 H10 107.3 . . ?
C37 N10 H10 107.3 . . ?
Ni4 N10 H10 107.3 . . ?
C38 N11 C36 116.0(5) . . ?
C38 N11 Ni4 114.8(5) . . ?
C36 N11 Ni4 104.9(4) . . ?
C38 N11 H11A 106.8 . . ?
C36 N11 H11A 106.8 . . ?
Ni4 N11 H11A 106.8 . . ?
C38 N12 C37 116.2(6) . . ?
C38 N12 C39 113.2(6) . . ?
C37 N12 C39 117.2(6) . . ?
O1 C1 O2 127.4(6) . . ?
O1 C1 C2 117.4(6) . . ?
O2 C1 C2 115.2(5) . . ?
C3 C2 C7 119.8(5) . . ?
C3 C2 C1 118.6(5) . . ?
C7 C2 C1 121.6(5) . . ?
C4 C3 C2 120.5(6) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.8(6) . . ?
C3 C4 H4A 119.6 . . ?
C5 C4 H4A 119.6 . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 C8 120.9(6) . . ?
C4 C5 C8 120.1(6) . . ?
C5 C6 C7 121.8(6) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 118.0(6) . . ?
C6 C7 C12 119.0(5) . . ?
C2 C7 C12 122.9(5) . . ?
O7 C8 O8 126.0(6) . . ?
O7 C8 C5 118.7(6) . . ?
O8 C8 C5 115.3(6) . . ?
O4 C9 O3 125.4(6) . . ?
O4 C9 C10 117.8(6) . . ?
O3 C9 C10 116.7(5) . . ?
C11 C10 C15 119.1(6) . . ?
C11 C10 C9 121.0(5) . . ?
C15 C10 C9 119.8(6) . . ?
C10 C11 C12 122.1(5) . . ?
C10 C11 H11B 119.0 . . ?
C12 C11 H11B 119.0 . . ?
C13 C12 C11 119.3(6) . . ?
C13 C12 C7 123.4(5) . . ?
C11 C12 C7 117.2(5) . . ?
C12 C13 C14 117.7(5) . . ?
C12 C13 C16 125.1(6) . . ?
C14 C13 C16 117.2(5) . . ?
C15 C14 C13 122.8(6) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
C14 C15 C10 119.0(6) . . ?
C14 C15 H15 120.5 . . ?
C10 C15 H15 120.5 . . ?
O5 C16 O6 124.2(6) . . ?
O5 C16 C13 117.5(6) . . ?
O6 C16 C13 118.3(5) . . ?
N2 C17 C18 109.0(5) . 2_675 ?
N2 C17 H17A 109.9 . . ?
C18 C17 H17A 109.9 2_675 . ?
N2 C17 H17B 109.9 . . ?
C18 C17 H17B 109.9 2_675 . ?
H17A C17 H17B 108.3 . . ?
N1 C18 C17 109.2(5) . 2_675 ?
N1 C18 H18A 109.8 . . ?
C17 C18 H18A 109.8 2_675 . ?
N1 C18 H18B 109.8 . . ?
C17 C18 H18B 109.8 2_675 . ?
H18A C18 H18B 108.3 . . ?
N3 C19 N2 111.0(5) . . ?
N3 C19 H19A 109.4 . . ?
N2 C19 H19A 109.4 . . ?
N3 C19 H19B 109.4 . . ?
N2 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N1 C20 N3 109.8(5) . . ?
N1 C20 H20A 109.7 . . ?
N3 C20 H20A 109.7 . . ?
N1 C20 H20B 109.7 . . ?
N3 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
N3 C21 C22 113.2(7) . . ?
N3 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
N3 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
O9 C22 C21 113.1(8) . . ?
O9 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
O9 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
N4 C23 C24 108.2(6) . 2_776 ?
N4 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 2_776 . ?
N4 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 2_776 . ?
H23A C23 H23B 108.4 . . ?
N5 C24 C23 108.9(6) . 2_776 ?
N5 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 2_776 . ?
N5 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 2_776 . ?
H24A C24 H24B 108.3 . . ?
N6 C25 N5 115.1(6) . . ?
N6 C25 H25A 108.5 . . ?
N5 C25 H25A 108.5 . . ?
N6 C25 H25B 108.5 . . ?
N5 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
N6 C26 N4 113.4(6) . . ?
N6 C26 H26A 108.9 . . ?
N4 C26 H26A 108.9 . . ?
N6 C26 H26B 108.9 . . ?
N4 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 N6 118.1(9) . . ?
C28 C27 H27A 107.8 . . ?
N6 C27 H27A 107.8 . . ?
C28 C27 H27B 107.8 . . ?
N6 C27 H27B 107.8 . . ?
H27A C27 H27B 107.1 . . ?
C27 C28 O10 113.1(9) . . ?
C27 C28 H28A 109.0 . . ?
O10 C28 H28A 109.0 . . ?
C27 C28 H28B 109.0 . . ?
O10 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
N7 C29 C30 109.1(6) . 2_665 ?
N7 C29 H29A 109.9 . . ?
C30 C29 H29A 109.9 2_665 . ?
N7 C29 H29B 109.9 . . ?
C30 C29 H29B 109.9 2_665 . ?
H29A C29 H29B 108.3 . . ?
N8 C30 C29 109.2(6) . 2_665 ?
N8 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 2_665 . ?
N8 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 2_665 . ?
H30A C30 H30B 108.3 . . ?
N9 C31 N7 114.7(5) . . ?
N9 C31 H31A 108.6 . . ?
N7 C31 H31A 108.6 . . ?
N9 C31 H31B 108.6 . . ?
N7 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
N9 C32 N8 114.2(5) . . ?
N9 C32 H32A 108.7 . . ?
N8 C32 H32A 108.7 . . ?
N9 C32 H32B 108.7 . . ?
N8 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
N9 C33 C34 114.1(6) . . ?
N9 C33 H33A 108.7 . . ?
C34 C33 H33A 108.7 . . ?
N9 C33 H33B 108.7 . . ?
C34 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
O11 C34 C33 114.2(6) . . ?
O11 C34 H34A 108.7 . . ?
C33 C34 H34A 108.7 . . ?
O11 C34 H34B 108.7 . . ?
C33 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
N10 C35 C36 110.0(6) . 2_666 ?
N10 C35 H35A 109.7 . . ?
C36 C35 H35A 109.7 2_666 . ?
N10 C35 H35B 109.7 . . ?
C36 C35 H35B 109.7 2_666 . ?
H35A C35 H35B 108.2 . . ?
N11 C36 C35 107.9(5) . 2_666 ?
N11 C36 H36A 110.1 . . ?
C35 C36 H36A 110.1 2_666 . ?
N11 C36 H36B 110.1 . . ?
C35 C36 H36B 110.1 2_666 . ?
H36A C36 H36B 108.4 . . ?
N12 C37 N10 113.7(6) . . ?
N12 C37 H37A 108.8 . . ?
N10 C37 H37A 108.8 . . ?
N12 C37 H37B 108.8 . . ?
N10 C37 H37B 108.8 . . ?
H37A C37 H37B 107.7 . . ?
N12 C38 N11 114.1(5) . . ?
N12 C38 H38A 108.7 . . ?
N11 C38 H38A 108.7 . . ?
N12 C38 H38B 108.7 . . ?
N11 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
C40 C39 N12 117.2(8) . . ?
C40 C39 H39A 108.0 . . ?
N12 C39 H39A 108.0 . . ?
C40 C39 H39B 108.0 . . ?
N12 C39 H39B 108.0 . . ?
H39A C39 H39B 107.2 . . ?
O12 C40 C39 111.2(8) . . ?
O12 C40 H40A 109.4 . . ?
C39 C40 H40A 109.4 . . ?
O12 C40 H40B 109.4 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 O1 7.4(11) . . . . ?
Ni1 O2 C1 C2 -170.9(4) . . . . ?
O1 C1 C2 C3 -59.6(8) . . . . ?
O2 C1 C2 C3 118.9(6) . . . . ?
O1 C1 C2 C7 121.8(7) . . . . ?
O2 C1 C2 C7 -59.7(8) . . . . ?
C7 C2 C3 C4 0.2(9) . . . . ?
C1 C2 C3 C4 -178.5(6) . . . . ?
C2 C3 C4 C5 -2.5(10) . . . . ?
C3 C4 C5 C6 2.7(9) . . . . ?
C3 C4 C5 C8 -176.3(6) . . . . ?
C4 C5 C6 C7 -0.5(9) . . . . ?
C8 C5 C6 C7 178.4(6) . . . . ?
C5 C6 C7 C2 -1.7(9) . . . . ?
C5 C6 C7 C12 174.5(6) . . . . ?
C3 C2 C7 C6 1.9(9) . . . . ?
C1 C2 C7 C6 -179.5(5) . . . . ?
C3 C2 C7 C12 -174.2(6) . . . . ?
C1 C2 C7 C12 4.4(9) . . . . ?
Ni4 O8 C8 O7 3.5(10) . . . . ?
Ni4 O8 C8 C5 -177.1(4) . . . . ?
C6 C5 C8 O7 165.0(6) . . . . ?
C4 C5 C8 O7 -16.0(9) . . . . ?
C6 C5 C8 O8 -14.5(9) . . . . ?
C4 C5 C8 O8 164.4(6) . . . . ?
Ni2 O4 C9 O3 -20.0(10) . . . . ?
Ni2 O4 C9 C10 161.5(4) . . . . ?
O4 C9 C10 C11 22.3(9) . . . . ?
O3 C9 C10 C11 -156.3(6) . . . . ?
O4 C9 C10 C15 -162.1(6) . . . . ?
O3 C9 C10 C15 19.2(9) . . . . ?
C15 C10 C11 C12 -1.9(9) . . . . ?
C9 C10 C11 C12 173.6(5) . . . . ?
C10 C11 C12 C13 1.2(9) . . . . ?
C10 C11 C12 C7 -174.9(5) . . . . ?
C6 C7 C12 C13 120.3(6) . . . . ?
C2 C7 C12 C13 -63.6(9) . . . . ?
C6 C7 C12 C11 -63.8(8) . . . . ?
C2 C7 C12 C11 112.2(7) . . . . ?
C11 C12 C13 C14 1.4(9) . . . . ?
C7 C12 C13 C14 177.2(6) . . . . ?
C11 C12 C13 C16 -179.8(6) . . . . ?
C7 C12 C13 C16 -4.0(9) . . . . ?
C12 C13 C14 C15 -3.4(9) . . . . ?
C16 C13 C14 C15 177.8(6) . . . . ?
C13 C14 C15 C10 2.7(9) . . . . ?
C11 C10 C15 C14 0.0(9) . . . . ?
C9 C10 C15 C14 -175.6(6) . . . . ?
Ni3 O6 C16 O5 9.8(11) . . . . ?
Ni3 O6 C16 C13 -167.9(4) . . . . ?
C12 C13 C16 O5 143.8(7) . . . . ?
C14 C13 C16 O5 -37.4(9) . . . . ?
C12 C13 C16 O6 -38.4(10) . . . . ?
C14 C13 C16 O6 140.4(6) . . . . ?
C19 N2 C17 C18 -167.1(5) . . . 2_675 ?
Ni1 N2 C17 C18 -42.1(5) . . . 2_675 ?
C20 N1 C18 C17 166.1(5) . . . 2_675 ?
Ni1 N1 C18 C17 39.5(6) . . . 2_675 ?
C20 N3 C19 N2 -76.1(7) . . . . ?
C21 N3 C19 N2 158.7(6) . . . . ?
C17 N2 C19 N3 178.5(5) . . . . ?
Ni1 N2 C19 N3 59.0(6) . . . . ?
C18 N1 C20 N3 178.6(5) . . . . ?
Ni1 N1 C20 N3 -60.4(6) . . . . ?
C19 N3 C20 N1 76.6(7) . . . . ?
C21 N3 C20 N1 -156.1(6) . . . . ?
C19 N3 C21 C22 -153.9(7) . . . . ?
C20 N3 C21 C22 78.2(8) . . . . ?
N3 C21 C22 O9 69.5(9) . . . . ?
C26 N4 C23 C24 166.8(6) . . . 2_776 ?
Ni2 N4 C23 C24 40.4(7) . . . 2_776 ?
C25 N5 C24 C23 -169.8(5) . . . 2_776 ?
Ni2 N5 C24 C23 -41.3(6) . . . 2_776 ?
C26 N6 C25 N5 -69.9(7) . . . . ?
C27 N6 C25 N5 68.3(8) . . . . ?
C24 N5 C25 N6 178.0(5) . . . . ?
Ni2 N5 C25 N6 54.0(7) . . . . ?
C25 N6 C26 N4 72.1(8) . . . . ?
C27 N6 C26 N4 -68.2(9) . . . . ?
C23 N4 C26 N6 180.0(6) . . . . ?
Ni2 N4 C26 N6 -57.4(7) . . . . ?
C25 N6 C27 C28 44.3(11) . . . . ?
C26 N6 C27 C28 -176.2(8) . . . . ?
N6 C27 C28 O10 -74.4(11) . . . . ?
C31 N7 C29 C30 -165.5(6) . . . 2_665 ?
Ni3 N7 C29 C30 -39.0(7) . . . 2_665 ?
C32 N8 C30 C29 164.6(6) . . . 2_665 ?
Ni3 N8 C30 C29 40.5(7) . . . 2_665 ?
C32 N9 C31 N7 -70.6(7) . . . . ?
C33 N9 C31 N7 68.2(7) . . . . ?
C29 N7 C31 N9 -180.0(6) . . . . ?
Ni3 N7 C31 N9 56.8(7) . . . . ?
C31 N9 C32 N8 70.6(8) . . . . ?
C33 N9 C32 N8 -67.5(8) . . . . ?
C30 N8 C32 N9 -176.6(6) . . . . ?
Ni3 N8 C32 N9 -56.5(7) . . . . ?
C31 N9 C33 C34 156.7(5) . . . . ?
C32 N9 C33 C34 -64.2(7) . . . . ?
N9 C33 C34 O11 80.9(7) . . . . ?
C37 N10 C35 C36 -169.7(5) . . . 2_666 ?
Ni4 N10 C35 C36 -42.9(6) . . . 2_666 ?
C38 N11 C36 C35 167.8(6) . . . 2_666 ?
Ni4 N11 C36 C35 40.0(7) . . . 2_666 ?
C38 N12 C37 N10 -70.9(7) . . . . ?
C39 N12 C37 N10 67.3(8) . . . . ?
C35 N10 C37 N12 178.0(5) . . . . ?
Ni4 N10 C37 N12 55.8(7) . . . . ?
C37 N12 C38 N11 71.1(8) . . . . ?
C39 N12 C38 N11 -68.8(9) . . . . ?
C36 N11 C38 N12 -178.2(6) . . . . ?
Ni4 N11 C38 N12 -55.5(7) . . . . ?
C38 N12 C39 C40 -175.1(7) . . . . ?
C37 N12 C39 C40 45.5(11) . . . . ?
N12 C39 C40 O12 -75.2(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O9 H9 O5 0.84 1.81 2.602(7) 155.4 . yes
O10 H10A O3 0.84 1.91 2.743(8) 171.4 . yes
O11 H11 O1 0.84 1.95 2.786(6) 179.6 . yes
O12 H12 O9 0.84 1.91 2.686(8) 152.9 2_665 yes
N2 H2 O1 1.00 2.29 3.111(7) 139.0 . yes
N5 H5 O3 1.00 1.90 2.831(6) 154.7 . yes
N5 H5 O10 1.00 2.45 3.157(9) 127.6 . yes
N7 H7 O5 1.00 1.93 2.846(7) 150.7 . yes
N8 H8 O1 1.00 2.37 3.361(8) 171.2 . yes
N10 H10 O12 1.00 2.40 3.088(8) 125.4 . yes
N11 H11A O7 1.00 1.96 2.867(7) 150.3 . yes

_refine_diff_density_max         0.918
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.094




# start Validation Reply Form
_vrf_PLAT029_cp_OH_sq            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.920 Why?
RESPONSE: Since the Pohang Accelerator Laboratory 2D-SMC beamline
goniostat has only one omega-axis, diffrn_measured_fraction_theta_full value is not
fully covered as 0.920, especially for the low symmetry such as the monoclinic and
triclinic system. As this is an inherent problem, other shelx OMIT command were not
helpful to improve the completeness.
;
# 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_cp_CH2_sq
_database_code_depnum_ccdc_archive 'CCDC 1908261'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        cp-flexMOF(CH2)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H132 N24 Ni4 O16'
_chemical_formula_sum            'C88 H132 N24 Ni4 O16'
_chemical_formula_weight         2017.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.829(3)
_cell_length_b                   14.867(3)
_cell_length_c                   16.595(4)
_cell_angle_alpha                90.112(7)
_cell_angle_beta                 78.434(10)
_cell_angle_gamma                87.888(10)
_cell_volume                     2374.0(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    37673
_cell_measurement_theta_min      1.820
_cell_measurement_theta_max      33.225

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_F_000             1068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.821
_shelx_estimated_absorpt_T_min   0.960
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15074
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.199
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 0.921
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.921
_reflns_number_total             8042
_reflns_number_gt                3997
_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       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018>(Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  CIFTAB
_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)+(0.1536P)²] 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         8042
_refine_ls_number_parameters     601
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.2702
_refine_ls_wR_factor_gt          0.2236
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.974
_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 0.500000 0.500000 0.000000 0.0544(4) Uani 1 2 d S U P . .
Ni2 Ni 1.000000 0.000000 0.000000 0.0555(4) Uani 1 2 d S U P . .
Ni3 Ni 0.500000 0.500000 0.500000 0.0626(5) Uani 1 2 d S U P . .
Ni4 Ni 0.500000 0.000000 0.500000 0.0669(5) Uani 1 2 d S U P . .
O1 O 0.2355(7) 0.3732(4) 0.1145(3) 0.0668(15) Uani 1 1 d . U . . .
O2 O 0.4653(6) 0.3955(4) 0.0868(3) 0.0604(14) Uani 1 1 d . U . . .
O3 O 1.0607(7) 0.0338(4) 0.1978(3) 0.0777(18) Uani 1 1 d . U . . .
O4 O 0.9060(6) 0.0630(4) 0.1170(3) 0.0632(14) Uani 1 1 d . U . . .
O5 O 0.6796(8) 0.2936(5) 0.5093(4) 0.096(2) Uani 1 1 d . U . . .
O6 O 0.5889(6) 0.3841(4) 0.4253(3) 0.0652(15) Uani 1 1 d . U . . .
O7 O 0.3350(7) 0.2170(4) 0.4990(3) 0.0816(19) Uani 1 1 d . U . . .
O8 O 0.4906(7) 0.1180(4) 0.4279(3) 0.0750(17) Uani 1 1 d . U . . .
N1 N 0.2900(7) 0.5267(4) 0.0104(4) 0.0601(16) Uani 1 1 d . U . . .
H1 H 0.240288 0.487538 0.054852 0.072 Uiso 1 1 calc R U . . .
N2 N 0.5214(7) 0.5805(5) 0.0972(4) 0.0635(17) Uani 1 1 d . U . . .
H2 H 0.488225 0.545510 0.148331 0.076 Uiso 1 1 calc R U . . .
N3 N 0.2878(8) 0.6511(5) 0.1094(4) 0.0659(17) Uani 1 1 d . U . . .
N4 N 1.0554(8) 0.1290(4) -0.0382(4) 0.0657(17) Uani 1 1 d . U . . .
H4 H 1.039536 0.168723 0.011757 0.079 Uiso 1 1 calc R U . . .
N5 N 1.1797(7) -0.0298(4) 0.0364(4) 0.0604(16) Uani 1 1 d . U . . .
H5 H 1.172192 -0.002323 0.092207 0.073 Uiso 1 1 calc R U . . .
N6 N 1.2991(8) 0.1012(5) -0.0292(5) 0.0741(19) Uani 1 1 d . U . . .
N7 N 0.5761(8) 0.4556(5) 0.5993(4) 0.0663(17) Uani 1 1 d . U . . .
H7 H 0.613759 0.392529 0.587452 0.080 Uiso 1 1 calc R U . . .
N8 N 0.3176(8) 0.4331(5) 0.5330(4) 0.0716(18) Uani 1 1 d . U . . .
H8 H 0.337529 0.368255 0.517249 0.086 Uiso 1 1 calc R U . . .
N9 N 0.3500(9) 0.4036(5) 0.6739(4) 0.077(2) Uani 1 1 d . U . . .
N10 N 0.6835(10) 0.0443(6) 0.5245(5) 0.093(2) Uani 1 1 d . U . . .
H10 H 0.687403 0.109764 0.510771 0.112 Uiso 1 1 calc R U . . .
N11 N 0.3868(9) 0.0561(5) 0.6048(5) 0.088(2) Uani 1 1 d . U . . .
H11 H 0.369037 0.121049 0.593321 0.106 Uiso 1 1 calc R U . . .
N12 N 0.5868(12) 0.0924(7) 0.6603(6) 0.113(3) Uani 1 1 d . U . . .
C1 C 0.3547(9) 0.3674(5) 0.1315(5) 0.0543(18) Uani 1 1 d . U . . .
C2 C 0.3722(9) 0.3230(5) 0.2103(4) 0.0541(18) Uani 1 1 d . U . . .
C3 C 0.2541(9) 0.3013(5) 0.2695(5) 0.0546(18) Uani 1 1 d . U . . .
H3 H 0.163122 0.314384 0.260332 0.066 Uiso 1 1 calc R U . . .
C4 C 0.2741(9) 0.2606(5) 0.3414(5) 0.061(2) Uani 1 1 d . U . . .
H4A H 0.194795 0.247471 0.382094 0.074 Uiso 1 1 calc R U . . .
C5 C 0.4047(9) 0.2381(5) 0.3564(4) 0.0570(18) Uani 1 1 d . U . . .
C6 C 0.5248(8) 0.2587(5) 0.2968(4) 0.0540(17) Uani 1 1 d . U . . .
C7 C 0.5036(8) 0.3033(5) 0.2258(4) 0.0510(17) Uani 1 1 d . U . . .
H7A H 0.582420 0.320783 0.186722 0.061 Uiso 1 1 calc R U . . .
C8 C 0.4111(10) 0.1873(6) 0.4352(5) 0.066(2) Uani 1 1 d . U . . .
C9 C 0.6576(10) 0.3174(6) 0.4404(5) 0.066(2) Uani 1 1 d . U . . .
C10 C 0.7311(9) 0.2572(5) 0.3681(5) 0.0584(19) Uani 1 1 d . U . . .
C11 C 0.6698(8) 0.2326(5) 0.3038(4) 0.0523(17) Uani 1 1 d . U . . .
C12 C 0.7458(8) 0.1764(5) 0.2407(4) 0.0519(18) Uani 1 1 d . U . . .
H12 H 0.705287 0.160412 0.195514 0.062 Uiso 1 1 calc R U . . .
C13 C 0.8791(8) 0.1439(5) 0.2436(4) 0.0542(18) Uani 1 1 d . U . . .
C14 C 0.9417(9) 0.1696(6) 0.3079(5) 0.063(2) Uani 1 1 d . U . . .
H14 H 1.033435 0.149030 0.310306 0.075 Uiso 1 1 calc R U . . .
C15 C 0.8653(10) 0.2265(6) 0.3684(5) 0.067(2) Uani 1 1 d . U . . .
H15 H 0.907448 0.245160 0.412102 0.080 Uiso 1 1 calc R U . . .
C16 C 0.9559(10) 0.0739(6) 0.1813(5) 0.062(2) Uani 1 1 d . U . . .
C17 C 0.2567(10) 0.4968(6) -0.0667(5) 0.072(2) Uani 1 1 d . U . . .
H17A H 0.286454 0.541806 -0.110024 0.086 Uiso 1 1 calc R U . . .
H17B H 0.155097 0.490908 -0.059970 0.086 Uiso 1 1 calc R U . . .
C18 C 0.6707(9) 0.5914(6) 0.0915(5) 0.069(2) Uani 1 1 d . U . . .
H18A H 0.688856 0.610925 0.145263 0.082 Uiso 1 1 calc R U . . .
H18B H 0.704758 0.637567 0.050166 0.082 Uiso 1 1 calc R U . . .
C19 C 0.2462(10) 0.6234(5) 0.0342(5) 0.064(2) Uani 1 1 d . U . . .
H19A H 0.287914 0.663278 -0.011046 0.077 Uiso 1 1 calc R U . . .
H19B H 0.143860 0.630620 0.041610 0.077 Uiso 1 1 calc R U . . .
C20 C 0.4315(10) 0.6645(6) 0.1039(5) 0.068(2) Uani 1 1 d . U . . .
H20A H 0.443222 0.698782 0.153074 0.082 Uiso 1 1 calc R U . . .
H20B H 0.464773 0.702066 0.055181 0.082 Uiso 1 1 calc R U . . .
C21 C 0.2254(10) 0.5996(6) 0.1830(5) 0.074(2) Uani 1 1 d . U . . .
H21A H 0.260140 0.536150 0.175543 0.089 Uiso 1 1 calc R U . . .
H21B H 0.256245 0.624260 0.231505 0.089 Uiso 1 1 calc R U . . .
C22 C 0.0730(11) 0.6020(7) 0.1991(5) 0.084(3) Uani 1 1 d . U . . .
H22 H 0.026896 0.659561 0.207749 0.101 Uiso 1 1 calc R U . . .
C23 C -0.0052(11) 0.5322(8) 0.2028(5) 0.084(3) Uani 1 1 d . U . . .
H23A H 0.036297 0.473278 0.194536 0.101 Uiso 1 1 calc R U . . .
H23B H -0.103552 0.540359 0.213621 0.101 Uiso 1 1 calc R U . . .
C24 C 0.9530(10) 0.1569(6) -0.0878(5) 0.072(2) Uani 1 1 d . U . . .
H24A H 0.953806 0.222886 -0.095374 0.086 Uiso 1 1 calc R U . . .
H24B H 0.977624 0.127710 -0.142758 0.086 Uiso 1 1 calc R U . . .
C25 C 1.1852(9) -0.1311(6) 0.0465(5) 0.067(2) Uani 1 1 d . U . . .
H25A H 1.211739 -0.161309 -0.007889 0.081 Uiso 1 1 calc R U . . .
H25B H 1.254681 -0.148830 0.079838 0.081 Uiso 1 1 calc R U . . .
C26 C 1.3047(9) 0.0040(6) -0.0161(6) 0.068(2) Uani 1 1 d . U . . .
H26A H 1.319734 -0.027105 -0.070117 0.081 Uiso 1 1 calc R U . . .
H26B H 1.385579 -0.011520 0.009155 0.081 Uiso 1 1 calc R U . . .
C27 C 1.2037(10) 0.1330(6) -0.0784(6) 0.073(2) Uani 1 1 d . U . . .
H27A H 1.219703 0.096888 -0.129851 0.088 Uiso 1 1 calc R U . . .
H27B H 1.223995 0.196159 -0.093668 0.088 Uiso 1 1 calc R U . . .
C28 C 1.2914(10) 0.1550(7) 0.0485(6) 0.082(3) Uani 1 1 d . U . . .
H28A H 1.292173 0.219831 0.035047 0.098 Uiso 1 1 calc R U . . .
H28B H 1.202462 0.143797 0.086466 0.098 Uiso 1 1 calc R U . . .
C29 C 1.4087(11) 0.1325(7) 0.0909(7) 0.089(3) Uani 1 1 d . U . . .
H29 H 1.500191 0.144340 0.062681 0.106 Uiso 1 1 calc R U . . .
C30 C 1.3936(12) 0.0976(8) 0.1642(7) 0.095(3) Uani 1 1 d . U . . .
H30A H 1.303434 0.084946 0.194101 0.114 Uiso 1 1 calc R U . . .
H30B H 1.472684 0.084942 0.187655 0.114 Uiso 1 1 calc R U . . .
C31 C 0.6914(10) 0.5119(6) 0.6036(5) 0.073(2) Uani 1 1 d . U . . .
H31A H 0.752342 0.482014 0.637127 0.088 Uiso 1 1 calc R U . . .
H31B H 0.656008 0.569976 0.630483 0.088 Uiso 1 1 calc R U . . .
C32 C 0.2259(11) 0.4712(7) 0.4818(5) 0.076(2) Uani 1 1 d . U . . .
H32A H 0.181849 0.528481 0.506455 0.092 Uiso 1 1 calc R U . . .
H32B H 0.151444 0.429073 0.478587 0.092 Uiso 1 1 calc R U . . .
C33 C 0.4718(10) 0.4554(7) 0.6773(5) 0.077(2) Uani 1 1 d . U . . .
H33A H 0.516807 0.430625 0.721185 0.092 Uiso 1 1 calc R U . . .
H33B H 0.440917 0.518345 0.692679 0.092 Uiso 1 1 calc R U . . .
C34 C 0.2564(10) 0.4378(7) 0.6232(5) 0.079(2) Uani 1 1 d . U . . .
H34A H 0.229593 0.501260 0.638887 0.095 Uiso 1 1 calc R U . . .
H34B H 0.170863 0.402901 0.634226 0.095 Uiso 1 1 calc R U . . .
C35 C 0.3750(12) 0.3051(7) 0.6719(6) 0.092(3) Uani 1 1 d . U . . .
H35A H 0.454712 0.288852 0.697870 0.110 Uiso 1 1 calc R U . . .
H35B H 0.396310 0.282706 0.614349 0.110 Uiso 1 1 calc R U . . .
C36 C 0.2442(14) 0.2634(8) 0.7188(8) 0.109(4) Uani 1 1 d . U . . .
H36 H 0.226403 0.267933 0.777093 0.131 Uiso 1 1 calc R U . . .
C37 C 0.1516(14) 0.2208(9) 0.6848(8) 0.124(4) Uani 1 1 d . U . . .
H37A H 0.165383 0.214767 0.626662 0.149 Uiso 1 1 calc R U . . .
H37B H 0.072119 0.196564 0.718759 0.149 Uiso 1 1 calc R U . . .
C38 C 0.6945(13) 0.0367(8) 0.6079(7) 0.104(3) Uani 1 1 d . U . . .
H38A H 0.787102 0.055853 0.614433 0.125 Uiso 1 1 calc R U . . .
H38B H 0.685251 -0.026915 0.624896 0.125 Uiso 1 1 calc R U . . .
C39 C 0.4483(14) 0.0527(9) 0.6769(6) 0.108(3) Uani 1 1 d . U . . .
H39A H 0.457351 -0.010698 0.693876 0.129 Uiso 1 1 calc R U . . .
H39B H 0.386868 0.086024 0.722645 0.129 Uiso 1 1 calc R U . . .
C40 C 0.7907(12) -0.0022(8) 0.4648(7) 0.096(3) Uani 1 1 d . U . . .
H40A H 0.809501 -0.062833 0.485638 0.115 Uiso 1 1 calc R U . . .
H40B H 0.877370 0.031285 0.457887 0.115 Uiso 1 1 calc R U . . .
C41 C 0.2502(11) 0.0114(7) 0.6167(7) 0.093(3) Uani 1 1 d . U . . .
H41A H 0.258383 -0.048782 0.641108 0.112 Uiso 1 1 calc R U . . .
H41B H 0.178430 0.047831 0.654568 0.112 Uiso 1 1 calc R U . . .
C42 C 0.6324(18) 0.1218(11) 0.7355(9) 0.177(6) Uani 1 1 d D U . . .
H42A H 0.549415 0.146681 0.774171 0.213 Uiso 1 1 calc R U . . .
H42B H 0.665522 0.067545 0.761418 0.213 Uiso 1 1 calc R U . . .
C43 C 0.739(2) 0.1875(11) 0.7284(10) 0.181(7) Uani 1 1 d D U . . .
H43 H 0.778367 0.197228 0.775512 0.217 Uiso 1 1 calc R U . . .
C44 C 0.788(2) 0.2357(13) 0.6614(10) 0.213(9) Uani 1 1 d D U . . .
H44A H 0.752134 0.228226 0.612889 0.255 Uiso 1 1 calc R U . . .
H44B H 0.858714 0.277456 0.662400 0.255 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 N2 2.057(6) 2_665 ?
Ni1 N2 2.057(6) . ?
Ni1 N1 2.061(7) . ?
Ni1 N1 2.061(7) 2_665 ?
Ni1 O2 2.111(5) 2_665 ?
Ni1 O2 2.111(5) . ?
Ni2 N5 2.012(7) . ?
Ni2 N5 2.012(7) 2_755 ?
Ni2 N4 2.078(7) 2_755 ?
Ni2 N4 2.078(7) . ?
Ni2 O4 2.170(5) 2_755 ?
Ni2 O4 2.170(5) . ?
Ni3 N7 2.043(7) 2_666 ?
Ni3 N7 2.043(7) . ?
Ni3 N8 2.060(8) 2_666 ?
Ni3 N8 2.060(8) . ?
Ni3 O6 2.171(5) . ?
Ni3 O6 2.171(5) 2_666 ?
Ni4 N11 2.027(7) 2_656 ?
Ni4 N11 2.027(7) . ?
Ni4 N10 2.058(9) 2_656 ?
Ni4 N10 2.058(9) . ?
Ni4 O8 2.135(6) 2_656 ?
Ni4 O8 2.135(6) . ?
O1 C1 1.258(9) . ?
O2 C1 1.273(9) . ?
O3 C16 1.249(10) . ?
O4 C16 1.273(9) . ?
O5 C9 1.254(10) . ?
O6 C9 1.234(10) . ?
O7 C8 1.238(9) . ?
O8 C8 1.261(9) . ?
N1 C17 1.455(10) . ?
N1 C19 1.515(10) . ?
N1 H1 1.0000 . ?
N2 C18 1.466(11) . ?
N2 C20 1.494(10) . ?
N2 H2 1.0000 . ?
N3 C20 1.418(11) . ?
N3 C19 1.453(10) . ?
N3 C21 1.480(11) . ?
N4 C24 1.471(11) . ?
N4 C27 1.480(11) . ?
N4 H4 1.0000 . ?
N5 C26 1.462(10) . ?
N5 C25 1.516(10) . ?
N5 H5 1.0000 . ?
N6 C27 1.430(12) . ?
N6 C26 1.463(11) . ?
N6 C28 1.503(11) . ?
N7 C31 1.446(11) . ?
N7 C33 1.481(10) . ?
N7 H7 1.0000 . ?
N8 C32 1.460(11) . ?
N8 C34 1.497(10) . ?
N8 H8 1.0000 . ?
N9 C34 1.446(12) . ?
N9 C33 1.458(12) . ?
N9 C35 1.475(12) . ?
N10 C38 1.414(13) . ?
N10 C40 1.447(12) . ?
N10 H10 1.0000 . ?
N11 C39 1.445(13) . ?
N11 C41 1.498(13) . ?
N11 H11 1.0000 . ?
N12 C38 1.457(14) . ?
N12 C42 1.478(16) . ?
N12 C39 1.479(16) . ?
C1 C2 1.504(11) . ?
C2 C7 1.388(11) . ?
C2 C3 1.410(10) . ?
C3 C4 1.384(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(11) . ?
C4 H4A 0.9500 . ?
C5 C6 1.423(11) . ?
C5 C8 1.521(11) . ?
C6 C7 1.401(10) . ?
C6 C11 1.490(11) . ?
C7 H7A 0.9500 . ?
C9 C10 1.538(10) . ?
C10 C15 1.381(11) . ?
C10 C11 1.381(11) . ?
C11 C12 1.411(10) . ?
C12 C13 1.389(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(11) . ?
C13 C16 1.531(10) . ?
C14 C15 1.391(11) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.486(12) 2_665 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.467(13) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.310(14) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9500 . ?
C23 H23B 0.9500 . ?
C24 C25 1.459(12) 2_755 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.494(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.307(15) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9500 . ?
C30 H30B 0.9500 . ?
C31 C32 1.512(12) 2_666 ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.517(15) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.340(17) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9500 . ?
C37 H37B 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.493(15) 2_656 ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.449(12) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.34(2) . ?
C43 H43 0.9500 . ?
C44 H44A 0.9500 . ?
C44 H44B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2 180.0(4) 2_665 . ?
N2 Ni1 N1 84.1(3) 2_665 . ?
N2 Ni1 N1 95.9(3) . . ?
N2 Ni1 N1 95.9(3) 2_665 2_665 ?
N2 Ni1 N1 84.1(3) . 2_665 ?
N1 Ni1 N1 180.0 . 2_665 ?
N2 Ni1 O2 85.8(2) 2_665 2_665 ?
N2 Ni1 O2 94.2(2) . 2_665 ?
N1 Ni1 O2 87.9(2) . 2_665 ?
N1 Ni1 O2 92.1(2) 2_665 2_665 ?
N2 Ni1 O2 94.2(2) 2_665 . ?
N2 Ni1 O2 85.8(2) . . ?
N1 Ni1 O2 92.1(2) . . ?
N1 Ni1 O2 87.9(2) 2_665 . ?
O2 Ni1 O2 180.0 2_665 . ?
N5 Ni2 N5 180.0 . 2_755 ?
N5 Ni2 N4 85.6(3) . 2_755 ?
N5 Ni2 N4 94.4(3) 2_755 2_755 ?
N5 Ni2 N4 94.4(3) . . ?
N5 Ni2 N4 85.6(3) 2_755 . ?
N4 Ni2 N4 180.0 2_755 . ?
N5 Ni2 O4 87.1(2) . 2_755 ?
N5 Ni2 O4 92.9(2) 2_755 2_755 ?
N4 Ni2 O4 85.7(2) 2_755 2_755 ?
N4 Ni2 O4 94.3(2) . 2_755 ?
N5 Ni2 O4 92.9(2) . . ?
N5 Ni2 O4 87.1(2) 2_755 . ?
N4 Ni2 O4 94.3(2) 2_755 . ?
N4 Ni2 O4 85.7(2) . . ?
O4 Ni2 O4 180.0 2_755 . ?
N7 Ni3 N7 180.0 2_666 . ?
N7 Ni3 N8 93.7(3) 2_666 2_666 ?
N7 Ni3 N8 86.3(3) . 2_666 ?
N7 Ni3 N8 86.3(3) 2_666 . ?
N7 Ni3 N8 93.7(3) . . ?
N8 Ni3 N8 180.0(4) 2_666 . ?
N7 Ni3 O6 87.2(2) 2_666 . ?
N7 Ni3 O6 92.8(2) . . ?
N8 Ni3 O6 91.2(2) 2_666 . ?
N8 Ni3 O6 88.8(2) . . ?
N7 Ni3 O6 92.8(2) 2_666 2_666 ?
N7 Ni3 O6 87.2(2) . 2_666 ?
N8 Ni3 O6 88.8(2) 2_666 2_666 ?
N8 Ni3 O6 91.2(2) . 2_666 ?
O6 Ni3 O6 180.0 . 2_666 ?
N11 Ni4 N11 180.0 2_656 . ?
N11 Ni4 N10 92.5(4) 2_656 2_656 ?
N11 Ni4 N10 87.5(4) . 2_656 ?
N11 Ni4 N10 87.5(4) 2_656 . ?
N11 Ni4 N10 92.5(4) . . ?
N10 Ni4 N10 180.0 2_656 . ?
N11 Ni4 O8 94.8(3) 2_656 2_656 ?
N11 Ni4 O8 85.2(3) . 2_656 ?
N10 Ni4 O8 87.7(3) 2_656 2_656 ?
N10 Ni4 O8 92.3(3) . 2_656 ?
N11 Ni4 O8 85.2(3) 2_656 . ?
N11 Ni4 O8 94.8(3) . . ?
N10 Ni4 O8 92.3(3) 2_656 . ?
N10 Ni4 O8 87.7(3) . . ?
O8 Ni4 O8 180.0 2_656 . ?
C1 O2 Ni1 132.0(5) . . ?
C16 O4 Ni2 129.9(5) . . ?
C9 O6 Ni3 131.8(5) . . ?
C8 O8 Ni4 133.9(5) . . ?
C17 N1 C19 114.8(7) . . ?
C17 N1 Ni1 106.0(5) . . ?
C19 N1 Ni1 113.2(5) . . ?
C17 N1 H1 107.5 . . ?
C19 N1 H1 107.5 . . ?
Ni1 N1 H1 107.5 . . ?
C18 N2 C20 117.0(7) . . ?
C18 N2 Ni1 107.0(5) . . ?
C20 N2 Ni1 112.4(5) . . ?
C18 N2 H2 106.6 . . ?
C20 N2 H2 106.6 . . ?
Ni1 N2 H2 106.6 . . ?
C20 N3 C19 116.4(7) . . ?
C20 N3 C21 113.0(7) . . ?
C19 N3 C21 114.3(7) . . ?
C24 N4 C27 116.7(7) . . ?
C24 N4 Ni2 104.2(5) . . ?
C27 N4 Ni2 112.5(5) . . ?
C24 N4 H4 107.7 . . ?
C27 N4 H4 107.7 . . ?
Ni2 N4 H4 107.7 . . ?
C26 N5 C25 113.2(6) . . ?
C26 N5 Ni2 115.7(6) . . ?
C25 N5 Ni2 105.9(5) . . ?
C26 N5 H5 107.2 . . ?
C25 N5 H5 107.2 . . ?
Ni2 N5 H5 107.2 . . ?
C27 N6 C26 115.9(8) . . ?
C27 N6 C28 113.7(7) . . ?
C26 N6 C28 113.0(8) . . ?
C31 N7 C33 112.7(7) . . ?
C31 N7 Ni3 105.5(5) . . ?
C33 N7 Ni3 114.4(6) . . ?
C31 N7 H7 108.0 . . ?
C33 N7 H7 108.0 . . ?
Ni3 N7 H7 108.0 . . ?
C32 N8 C34 113.6(7) . . ?
C32 N8 Ni3 105.1(6) . . ?
C34 N8 Ni3 113.8(6) . . ?
C32 N8 H8 108.0 . . ?
C34 N8 H8 108.0 . . ?
Ni3 N8 H8 108.0 . . ?
C34 N9 C33 117.5(8) . . ?
C34 N9 C35 115.8(8) . . ?
C33 N9 C35 114.7(8) . . ?
C38 N10 C40 116.5(10) . . ?
C38 N10 Ni4 114.1(8) . . ?
C40 N10 Ni4 104.6(7) . . ?
C38 N10 H10 107.1 . . ?
C40 N10 H10 107.1 . . ?
Ni4 N10 H10 107.1 . . ?
C39 N11 C41 113.2(8) . . ?
C39 N11 Ni4 117.0(7) . . ?
C41 N11 Ni4 104.4(6) . . ?
C39 N11 H11 107.3 . . ?
C41 N11 H11 107.3 . . ?
Ni4 N11 H11 107.3 . . ?
C38 N12 C42 111.3(12) . . ?
C38 N12 C39 114.0(10) . . ?
C42 N12 C39 113.5(10) . . ?
O1 C1 O2 125.5(8) . . ?
O1 C1 C2 118.9(7) . . ?
O2 C1 C2 115.6(8) . . ?
C7 C2 C3 119.4(7) . . ?
C7 C2 C1 120.8(7) . . ?
C3 C2 C1 119.9(8) . . ?
C4 C3 C2 118.3(8) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 122.8(7) . . ?
C3 C4 H4A 118.6 . . ?
C5 C4 H4A 118.6 . . ?
C4 C5 C6 119.4(7) . . ?
C4 C5 C8 117.2(7) . . ?
C6 C5 C8 123.2(8) . . ?
C7 C6 C5 117.3(8) . . ?
C7 C6 C11 118.4(7) . . ?
C5 C6 C11 124.3(7) . . ?
C2 C7 C6 122.6(7) . . ?
C2 C7 H7A 118.7 . . ?
C6 C7 H7A 118.7 . . ?
O7 C8 O8 127.1(8) . . ?
O7 C8 C5 116.6(8) . . ?
O8 C8 C5 116.4(7) . . ?
O6 C9 O5 127.2(7) . . ?
O6 C9 C10 118.2(7) . . ?
O5 C9 C10 114.5(8) . . ?
C15 C10 C11 119.0(7) . . ?
C15 C10 C9 117.5(7) . . ?
C11 C10 C9 123.5(8) . . ?
C10 C11 C12 119.0(7) . . ?
C10 C11 C6 124.6(7) . . ?
C12 C11 C6 116.3(7) . . ?
C13 C12 C11 121.0(7) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.0(7) . . ?
C12 C13 C16 121.5(7) . . ?
C14 C13 C16 118.3(8) . . ?
C15 C14 C13 117.7(8) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
C10 C15 C14 123.2(8) . . ?
C10 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
O3 C16 O4 126.4(7) . . ?
O3 C16 C13 117.6(7) . . ?
O4 C16 C13 116.0(8) . . ?
N1 C17 C18 109.4(7) . 2_665 ?
N1 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 2_665 . ?
N1 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 2_665 . ?
H17A C17 H17B 108.2 . . ?
N2 C18 C17 108.0(7) . 2_665 ?
N2 C18 H18A 110.1 . . ?
C17 C18 H18A 110.1 2_665 . ?
N2 C18 H18B 110.1 . . ?
C17 C18 H18B 110.1 2_665 . ?
H18A C18 H18B 108.4 . . ?
N3 C19 N1 112.6(7) . . ?
N3 C19 H19A 109.1 . . ?
N1 C19 H19A 109.1 . . ?
N3 C19 H19B 109.1 . . ?
N1 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
N3 C20 N2 115.2(7) . . ?
N3 C20 H20A 108.5 . . ?
N2 C20 H20A 108.5 . . ?
N3 C20 H20B 108.5 . . ?
N2 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C22 C21 N3 113.4(8) . . ?
C22 C21 H21A 108.9 . . ?
N3 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
N3 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C21 126.0(10) . . ?
C23 C22 H22 117.0 . . ?
C21 C22 H22 117.0 . . ?
C22 C23 H23A 120.0 . . ?
C22 C23 H23B 120.0 . . ?
H23A C23 H23B 120.0 . . ?
C25 C24 N4 109.7(7) 2_755 . ?
C25 C24 H24A 109.7 2_755 . ?
N4 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 2_755 . ?
N4 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C24 C25 N5 107.3(7) 2_755 . ?
C24 C25 H25A 110.3 2_755 . ?
N5 C25 H25A 110.3 . . ?
C24 C25 H25B 110.3 2_755 . ?
N5 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N5 C26 N6 114.0(7) . . ?
N5 C26 H26A 108.7 . . ?
N6 C26 H26A 108.7 . . ?
N5 C26 H26B 108.7 . . ?
N6 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
N6 C27 N4 114.7(7) . . ?
N6 C27 H27A 108.6 . . ?
N4 C27 H27A 108.6 . . ?
N6 C27 H27B 108.6 . . ?
N4 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C29 C28 N6 112.9(7) . . ?
C29 C28 H28A 109.0 . . ?
N6 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
N6 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C30 C29 C28 124.3(11) . . ?
C30 C29 H29 117.8 . . ?
C28 C29 H29 117.9 . . ?
C29 C30 H30A 120.0 . . ?
C29 C30 H30B 120.0 . . ?
H30A C30 H30B 120.0 . . ?
N7 C31 C32 110.3(7) . 2_666 ?
N7 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 2_666 . ?
N7 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 2_666 . ?
H31A C31 H31B 108.1 . . ?
N8 C32 C31 109.7(7) . 2_666 ?
N8 C32 H32A 109.7 . . ?
C31 C32 H32A 109.7 2_666 . ?
N8 C32 H32B 109.7 . . ?
C31 C32 H32B 109.7 2_666 . ?
H32A C32 H32B 108.2 . . ?
N9 C33 N7 114.3(7) . . ?
N9 C33 H33A 108.7 . . ?
N7 C33 H33A 108.7 . . ?
N9 C33 H33B 108.7 . . ?
N7 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
N9 C34 N8 113.3(7) . . ?
N9 C34 H34A 108.9 . . ?
N8 C34 H34A 108.9 . . ?
N9 C34 H34B 108.9 . . ?
N8 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
N9 C35 C36 107.7(9) . . ?
N9 C35 H35A 110.2 . . ?
C36 C35 H35A 110.2 . . ?
N9 C35 H35B 110.2 . . ?
C36 C35 H35B 110.2 . . ?
H35A C35 H35B 108.5 . . ?
C37 C36 C35 125.4(12) . . ?
C37 C36 H36 117.3 . . ?
C35 C36 H36 117.3 . . ?
C36 C37 H37A 120.0 . . ?
C36 C37 H37B 120.0 . . ?
H37A C37 H37B 120.0 . . ?
N10 C38 N12 110.7(10) . . ?
N10 C38 H38A 109.5 . . ?
N12 C38 H38A 109.5 . . ?
N10 C38 H38B 109.5 . . ?
N12 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
N11 C39 N12 111.0(9) . . ?
N11 C39 H39A 109.4 . . ?
N12 C39 H39A 109.4 . . ?
N11 C39 H39B 109.4 . . ?
N12 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
N10 C40 C41 111.9(10) . 2_656 ?
N10 C40 H40A 109.2 . . ?
C41 C40 H40A 109.2 2_656 . ?
N10 C40 H40B 109.2 . . ?
C41 C40 H40B 109.2 2_656 . ?
H40A C40 H40B 107.9 . . ?
C40 C41 N11 109.0(9) 2_656 . ?
C40 C41 H41A 109.9 2_656 . ?
N11 C41 H41A 109.9 . . ?
C40 C41 H41B 109.9 2_656 . ?
N11 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C43 C42 N12 118.9(14) . . ?
C43 C42 H42A 107.6 . . ?
N12 C42 H42A 107.6 . . ?
C43 C42 H42B 107.6 . . ?
N12 C42 H42B 107.6 . . ?
H42A C42 H42B 107.0 . . ?
C44 C43 C42 125.8(17) . . ?
C44 C43 H43 117.1 . . ?
C42 C43 H43 117.1 . . ?
C43 C44 H44A 120.0 . . ?
C43 C44 H44B 120.0 . . ?
H44A C44 H44B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C1 O1 27.6(11) . . . . ?
Ni1 O2 C1 C2 -153.1(5) . . . . ?
O1 C1 C2 C7 170.5(7) . . . . ?
O2 C1 C2 C7 -8.9(10) . . . . ?
O1 C1 C2 C3 -9.8(11) . . . . ?
O2 C1 C2 C3 170.9(7) . . . . ?
C7 C2 C3 C4 -0.2(11) . . . . ?
C1 C2 C3 C4 -180.0(7) . . . . ?
C2 C3 C4 C5 -1.8(11) . . . . ?
C3 C4 C5 C6 1.1(12) . . . . ?
C3 C4 C5 C8 -175.5(7) . . . . ?
C4 C5 C6 C7 1.6(11) . . . . ?
C8 C5 C6 C7 178.0(7) . . . . ?
C4 C5 C6 C11 -175.9(7) . . . . ?
C8 C5 C6 C11 0.5(12) . . . . ?
C3 C2 C7 C6 3.0(11) . . . . ?
C1 C2 C7 C6 -177.3(7) . . . . ?
C5 C6 C7 C2 -3.6(10) . . . . ?
C11 C6 C7 C2 174.0(7) . . . . ?
Ni4 O8 C8 O7 20.7(16) . . . . ?
Ni4 O8 C8 C5 -157.3(6) . . . . ?
C4 C5 C8 O7 -47.1(12) . . . . ?
C6 C5 C8 O7 136.4(9) . . . . ?
C4 C5 C8 O8 131.0(9) . . . . ?
C6 C5 C8 O8 -45.5(12) . . . . ?
Ni3 O6 C9 O5 10.0(16) . . . . ?
Ni3 O6 C9 C10 -167.2(5) . . . . ?
O6 C9 C10 C15 137.4(9) . . . . ?
O5 C9 C10 C15 -40.2(12) . . . . ?
O6 C9 C10 C11 -42.7(13) . . . . ?
O5 C9 C10 C11 139.8(9) . . . . ?
C15 C10 C11 C12 0.5(12) . . . . ?
C9 C10 C11 C12 -179.4(7) . . . . ?
C15 C10 C11 C6 178.2(8) . . . . ?
C9 C10 C11 C6 -1.7(13) . . . . ?
C7 C6 C11 C10 124.5(8) . . . . ?
C5 C6 C11 C10 -58.1(11) . . . . ?
C7 C6 C11 C12 -57.8(9) . . . . ?
C5 C6 C11 C12 119.7(8) . . . . ?
C10 C11 C12 C13 1.6(11) . . . . ?
C6 C11 C12 C13 -176.3(7) . . . . ?
C11 C12 C13 C14 -2.4(12) . . . . ?
C11 C12 C13 C16 172.5(7) . . . . ?
C12 C13 C14 C15 1.2(12) . . . . ?
C16 C13 C14 C15 -173.9(8) . . . . ?
C11 C10 C15 C14 -1.8(13) . . . . ?
C9 C10 C15 C14 178.2(8) . . . . ?
C13 C14 C15 C10 0.9(13) . . . . ?
Ni2 O4 C16 O3 -16.4(13) . . . . ?
Ni2 O4 C16 C13 163.0(5) . . . . ?
C12 C13 C16 O3 -164.8(8) . . . . ?
C14 C13 C16 O3 10.1(12) . . . . ?
C12 C13 C16 O4 15.7(11) . . . . ?
C14 C13 C16 O4 -169.3(7) . . . . ?
C19 N1 C17 C18 168.6(7) . . . 2_665 ?
Ni1 N1 C17 C18 42.8(8) . . . 2_665 ?
C20 N2 C18 C17 -167.5(7) . . . 2_665 ?
Ni1 N2 C18 C17 -40.3(8) . . . 2_665 ?
C20 N3 C19 N1 72.6(9) . . . . ?
C21 N3 C19 N1 -62.0(10) . . . . ?
C17 N1 C19 N3 -177.1(7) . . . . ?
Ni1 N1 C19 N3 -55.1(8) . . . . ?
C19 N3 C20 N2 -73.8(9) . . . . ?
C21 N3 C20 N2 61.3(9) . . . . ?
C18 N2 C20 N3 -179.9(7) . . . . ?
Ni1 N2 C20 N3 55.6(8) . . . . ?
C20 N3 C21 C22 167.5(7) . . . . ?
C19 N3 C21 C22 -56.4(10) . . . . ?
N3 C21 C22 C23 121.0(10) . . . . ?
C27 N4 C24 C25 167.9(7) . . . 2_755 ?
Ni2 N4 C24 C25 43.2(7) . . . 2_755 ?
C26 N5 C25 C24 -170.6(7) . . . 2_755 ?
Ni2 N5 C25 C24 -42.8(7) . . . 2_755 ?
C25 N5 C26 N6 177.7(7) . . . . ?
Ni2 N5 C26 N6 55.3(9) . . . . ?
C27 N6 C26 N5 -69.2(10) . . . . ?
C28 N6 C26 N5 64.5(10) . . . . ?
C26 N6 C27 N4 71.2(9) . . . . ?
C28 N6 C27 N4 -62.2(10) . . . . ?
C24 N4 C27 N6 -177.1(7) . . . . ?
Ni2 N4 C27 N6 -56.8(8) . . . . ?
C27 N6 C28 C29 -169.0(9) . . . . ?
C26 N6 C28 C29 56.2(11) . . . . ?
N6 C28 C29 C30 -116.8(11) . . . . ?
C33 N7 C31 C32 -165.5(7) . . . 2_666 ?
Ni3 N7 C31 C32 -40.0(8) . . . 2_666 ?
C34 N8 C32 C31 163.8(8) . . . 2_666 ?
Ni3 N8 C32 C31 38.7(8) . . . 2_666 ?
C34 N9 C33 N7 -68.4(10) . . . . ?
C35 N9 C33 N7 72.8(10) . . . . ?
C31 N7 C33 N9 176.6(8) . . . . ?
Ni3 N7 C33 N9 56.0(9) . . . . ?
C33 N9 C34 N8 68.8(10) . . . . ?
C35 N9 C34 N8 -72.0(11) . . . . ?
C32 N8 C34 N9 -177.4(8) . . . . ?
Ni3 N8 C34 N9 -57.1(9) . . . . ?
C34 N9 C35 C36 -72.3(11) . . . . ?
C33 N9 C35 C36 145.9(9) . . . . ?
N9 C35 C36 C37 104.9(14) . . . . ?
C40 N10 C38 N12 175.5(10) . . . . ?
Ni4 N10 C38 N12 -62.5(11) . . . . ?
C42 N12 C38 N10 -151.9(11) . . . . ?
C39 N12 C38 N10 78.1(13) . . . . ?
C41 N11 C39 N12 176.3(9) . . . . ?
Ni4 N11 C39 N12 54.9(11) . . . . ?
C38 N12 C39 N11 -72.6(13) . . . . ?
C42 N12 C39 N11 158.6(11) . . . . ?
C38 N10 C40 C41 164.3(10) . . . 2_656 ?
Ni4 N10 C40 C41 37.4(10) . . . 2_656 ?
C39 N11 C41 C40 -168.8(9) . . . 2_656 ?
Ni4 N11 C41 C40 -40.6(9) . . . 2_656 ?
C38 N12 C42 C43 70.5(19) . . . . ?
C39 N12 C42 C43 -159.3(15) . . . . ?
N12 C42 C43 C44 11(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 1.00 1.97 2.866(9) 148.4 . yes
N5 H5 O3 1.00 1.93 2.844(8) 149.9 . yes
N7 H7 O5 1.00 1.96 2.876(9) 150.5 . yes
N8 H8 O7 1.00 2.27 3.253(10) 167.2 . yes
N11 H11 O7 1.00 2.19 3.058(10) 144.7 . yes

_refine_diff_density_max         0.781
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.103




# start Validation Reply Form
_vrf_PLAT029_cp_CH2_sq           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.921 Why?
RESPONSE: Since the Pohang Accelerator Laboratory 2D-SMC beamline
goniostat has only one omega-axis, diffrn_measured_fraction_theta_full value is not
fully covered as 0.921, especially for the low symmetry such as the monoclinic and
triclinic system. As this is an inherent problem, other shelx OMIT command were not
helpful to improve the completeness.

;
# 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_asflex_OH_sq
_database_code_depnum_ccdc_archive 'CCDC 1898506'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        as-flexMOF(OH)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H130 N24 Ni4 O24, 2(C3 H7 N O)'
_chemical_formula_sum            'C86 H146 N26 Ni4 O26'
_chemical_formula_weight         2195.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   15.210(3)
_cell_length_b                   15.650(3)
_cell_length_c                   17.099(3)
_cell_angle_alpha                82.34(3)
_cell_angle_beta                 65.07(3)
_cell_angle_gamma                75.54(3)
_cell_volume                     3572.3(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    119301
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28016
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.294
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             14057
_reflns_number_gt                5993
_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       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  CIFTAB
_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)+(0.1367P)²] 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         14057
_refine_ls_number_parameters     676
_refine_ls_number_restraints     648
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2303
_refine_ls_wR_factor_gt          0.2121
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.919
_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 0.500000 1.000000 0.000000 0.0740(3) Uani 1 2 d S U P . .
N1 N 0.6118(3) 0.9624(3) -0.1187(2) 0.0774(11) Uani 1 1 d . U . . .
H1 H 0.634535 0.897409 -0.116673 0.093 Uiso 1 1 calc R U . . .
N2 N 0.4965(4) 0.9517(3) -0.1824(2) 0.0902(12) Uani 1 1 d . U . . .
N3 N 0.3942(3) 0.9651(3) -0.0255(2) 0.0810(11) Uani 1 1 d . U . . .
H3 H 0.402701 0.900159 -0.017330 0.097 Uiso 1 1 calc R U . . .
C1 C 0.6925(4) 1.0019(4) -0.1266(3) 0.0872(14) Uani 1 1 d . U . . .
H1A H 0.679306 1.064117 -0.144831 0.105 Uiso 1 1 calc R U . . .
H1B H 0.754640 0.971809 -0.171087 0.105 Uiso 1 1 calc R U . . .
C2 C 0.5805(4) 0.9862(4) -0.1908(3) 0.0904(15) Uani 1 1 d . U . . .
H2A H 0.563469 1.050698 -0.196430 0.108 Uiso 1 1 calc R U . . .
H2B H 0.636961 0.964726 -0.244166 0.108 Uiso 1 1 calc R U . . .
C3 C 0.3989(4) 0.9884(4) -0.1154(3) 0.0971(16) Uani 1 1 d . U . . .
H3A H 0.347933 0.965964 -0.122197 0.116 Uiso 1 1 calc R U . . .
H3B H 0.384193 1.052770 -0.123245 0.116 Uiso 1 1 calc R U . . .
C4 C 0.2962(4) 1.0050(4) 0.0403(3) 0.0893(15) Uani 1 1 d . U . . .
H4A H 0.246021 0.973301 0.045071 0.107 Uiso 1 1 calc R U . . .
H4B H 0.275571 1.066967 0.024517 0.107 Uiso 1 1 calc R U . . .
C5 C 0.5206(5) 0.8561(4) -0.1928(4) 0.1045(17) Uani 1 1 d . U . . .
H5A H 0.510172 0.826681 -0.136249 0.125 Uiso 1 1 calc R U . . .
H5B H 0.591247 0.838187 -0.230237 0.125 Uiso 1 1 calc R U . . .
C6 C 0.4592(8) 0.8229(7) -0.2315(6) 0.178(4) Uani 1 1 d . U . . .
H6A H 0.480477 0.758688 -0.237079 0.214 Uiso 1 1 calc R U . . .
H6B H 0.388565 0.836892 -0.193042 0.214 Uiso 1 1 calc R U . . .
O1 O 0.4733(9) 0.8621(6) -0.3088(5) 0.274(5) Uani 1 1 d . U . . .
Ni2 Ni 0.500000 0.500000 0.500000 0.0714(3) Uani 1 2 d S U P . .
N4 N 0.6371(3) 0.4899(3) 0.5014(2) 0.0820(11) Uani 1 1 d . U . . .
H4 H 0.678267 0.516576 0.446415 0.098 Uiso 1 1 calc R U . . .
N5 N 0.5842(4) 0.6305(3) 0.5750(3) 0.1033(13) Uani 1 1 d D U . . .
N6 N 0.4487(3) 0.6303(3) 0.5338(3) 0.0835(11) Uani 1 1 d . U . . .
H6 H 0.477470 0.666946 0.481453 0.100 Uiso 1 1 calc R U . . .
C7 C 0.6828(4) 0.3949(4) 0.5016(3) 0.0909(15) Uani 1 1 d . U . . .
H7A H 0.655329 0.368873 0.559900 0.109 Uiso 1 1 calc R U . . .
H7B H 0.754691 0.386523 0.482937 0.109 Uiso 1 1 calc R U . . .
C8 C 0.6325(4) 0.5390(4) 0.5738(3) 0.0934(15) Uani 1 1 d . U . . .
H8A H 0.597068 0.510409 0.628989 0.112 Uiso 1 1 calc R U . . .
H8B H 0.700269 0.534729 0.568339 0.112 Uiso 1 1 calc R U . . .
C9 C 0.4773(5) 0.6512(4) 0.5996(4) 0.0998(16) Uani 1 1 d . U . . .
H9A H 0.451685 0.714231 0.611345 0.120 Uiso 1 1 calc R U . . .
H9B H 0.446001 0.618153 0.653106 0.120 Uiso 1 1 calc R U . . .
C10 C 0.3390(4) 0.6491(4) 0.5594(3) 0.0949(16) Uani 1 1 d . U . . .
H10A H 0.313227 0.712978 0.557485 0.114 Uiso 1 1 calc R U . . .
H10B H 0.306232 0.626775 0.618477 0.114 Uiso 1 1 calc R U . . .
C11A C 0.6383(13) 0.6857(11) 0.5031(8) 0.111(4) Uani 0.496(11) 1 d D U P A 1
H11A H 0.595826 0.704166 0.471184 0.133 Uiso 0.496(11) 1 calc R U P A 1
H11B H 0.696264 0.643518 0.466278 0.133 Uiso 0.496(11) 1 calc R U P A 1
C12A C 0.680(2) 0.7697(15) 0.4978(10) 0.227(9) Uani 0.496(11) 1 d D U P A 1
H12A H 0.752719 0.754009 0.477128 0.273 Uiso 0.496(11) 1 calc R U P A 1
H12B H 0.662377 0.814724 0.458269 0.273 Uiso 0.496(11) 1 calc R U P A 1
O2A O 0.6368(11) 0.8015(11) 0.5826(9) 0.204(7) Uani 0.496(11) 1 d D U P A 1
H2A1 H 0.673808 0.819633 0.596321 0.306 Uiso 0.496(11) 1 d . U P A 1
C11B C 0.6402(15) 0.6863(14) 0.5055(11) 0.183(7) Uani 0.504(11) 1 d D U P A 2
H11C H 0.600395 0.746709 0.509930 0.219 Uiso 0.504(11) 1 calc R U P A 2
H11D H 0.653906 0.664194 0.449642 0.219 Uiso 0.504(11) 1 calc R U P A 2
C12B C 0.7381(15) 0.6871(16) 0.5103(11) 0.213(8) Uani 0.504(11) 1 d D U P A 2
H12C H 0.778597 0.626989 0.498779 0.255 Uiso 0.504(11) 1 calc R U P A 2
H12D H 0.771951 0.724750 0.461849 0.255 Uiso 0.504(11) 1 calc R U P A 2
O2B O 0.7427(16) 0.7134(14) 0.5833(11) 0.266(9) Uani 0.504(11) 1 d D U P A 2
H2B1 H 0.792907 0.711137 0.580709 0.399 Uiso 0.504(11) 1 d . U P A 2
Ni3 Ni 0.500000 0.500000 0.000000 0.0787(3) Uani 1 2 d S U P . .
N7 N 0.4844(3) 0.5627(3) -0.1091(2) 0.0867(12) Uani 1 1 d . U . . .
H7 H 0.471953 0.627180 -0.103191 0.104 Uiso 1 1 calc R U . . .
N8 N 0.6662(4) 0.5491(3) -0.1902(3) 0.1000(13) Uani 1 1 d . U . . .
N9 N 0.6454(3) 0.5091(3) -0.0417(3) 0.0910(12) Uani 1 1 d . U . . .
H9 H 0.645212 0.570369 -0.032602 0.109 Uiso 1 1 calc R U . . .
C13 C 0.3934(4) 0.5418(4) -0.1077(3) 0.0948(15) Uani 1 1 d . U . . .
H13A H 0.408442 0.481565 -0.126806 0.114 Uiso 1 1 calc R U . . .
H13B H 0.370119 0.582568 -0.147120 0.114 Uiso 1 1 calc R U . . .
C14 C 0.5729(5) 0.5376(4) -0.1895(3) 0.1054(17) Uani 1 1 d . U . . .
H14A H 0.580450 0.475460 -0.199594 0.126 Uiso 1 1 calc R U . . .
H14B H 0.561692 0.572796 -0.237570 0.126 Uiso 1 1 calc R U . . .
C15 C 0.7059(5) 0.4917(4) -0.1351(3) 0.1018(16) Uani 1 1 d . U . . .
H15A H 0.773449 0.498695 -0.150085 0.122 Uiso 1 1 calc R U . . .
H15B H 0.709907 0.430471 -0.145345 0.122 Uiso 1 1 calc R U . . .
C16 C 0.6857(4) 0.4496(4) 0.0175(3) 0.0961(16) Uani 1 1 d . U . . .
H16A H 0.704508 0.388272 -0.000063 0.115 Uiso 1 1 calc R U . . .
H16B H 0.744757 0.466419 0.014952 0.115 Uiso 1 1 calc R U . . .
C17 C 0.6679(5) 0.6430(4) -0.1951(4) 0.1087(18) Uani 1 1 d . U . . .
H17A H 0.616331 0.670636 -0.142088 0.130 Uiso 1 1 calc R U . . .
H17B H 0.651921 0.671479 -0.243474 0.130 Uiso 1 1 calc R U . . .
C18 C 0.7662(6) 0.6591(5) -0.2067(5) 0.133(2) Uani 1 1 d . U . . .
H18A H 0.819211 0.619009 -0.250022 0.160 Uiso 1 1 calc R U . . .
H18B H 0.769851 0.719580 -0.229471 0.160 Uiso 1 1 calc R U . . .
O3 O 0.7846(4) 0.6471(3) -0.1284(3) 0.1383(16) Uani 1 1 d . U . . .
H3C H 0.741162 0.681893 -0.091686 0.208 Uiso 1 1 calc R U . . .
Ni4 Ni 0.000000 1.000000 0.500000 0.0861(3) Uani 1 2 d S U P . .
N10 N 0.0724(3) 1.1007(3) 0.4427(3) 0.1002(13) Uani 1 1 d . U . . .
H10 H 0.028592 1.155860 0.471351 0.120 Uiso 1 1 calc R U . . .
N11 N 0.0079(4) 1.1295(4) 0.3275(3) 0.1146(15) Uani 1 1 d D U . . .
N12 N -0.0870(3) 1.0265(3) 0.4312(3) 0.0949(13) Uani 1 1 d . U . . .
H12 H -0.142688 1.076189 0.459253 0.114 Uiso 1 1 calc R U . . .
C19 C 0.1604(5) 1.0809(5) 0.4640(4) 0.120(2) Uani 1 1 d . U . . .
H19A H 0.187001 1.134056 0.454812 0.144 Uiso 1 1 calc R U . . .
H19B H 0.212236 1.035149 0.426475 0.144 Uiso 1 1 calc R U . . .
C20 C 0.0941(5) 1.1137(5) 0.3483(4) 0.121(2) Uani 1 1 d . U . . .
H20A H 0.126571 1.163848 0.325781 0.145 Uiso 1 1 calc R U . . .
H20B H 0.141315 1.061154 0.318462 0.145 Uiso 1 1 calc R U . . .
C21 C -0.0354(5) 1.0549(5) 0.3386(3) 0.1134(18) Uani 1 1 d . U . . .
H21A H 0.016974 1.005236 0.308036 0.136 Uiso 1 1 calc R U . . .
H21B H -0.083290 1.069259 0.311977 0.136 Uiso 1 1 calc R U . . .
C22 C -0.1295(5) 0.9509(5) 0.4419(4) 0.113(2) Uani 1 1 d . U . . .
H22A H -0.080624 0.903971 0.403945 0.136 Uiso 1 1 calc R U . . .
H22B H -0.187337 0.967127 0.427118 0.136 Uiso 1 1 calc R U . . .
C23 C -0.0657(5) 1.2125(4) 0.3564(4) 0.144(2) Uani 1 1 d D U . . .
H23A H -0.096330 1.208570 0.419563 0.173 Uiso 1 1 calc R U . . .
H23B H -0.117798 1.213564 0.336623 0.173 Uiso 1 1 calc R U . . .
C24 C -0.0367(10) 1.3035(7) 0.3309(5) 0.228(5) Uani 1 1 d D U . . .
H24A H 0.014887 1.303574 0.272203 0.273 Uiso 1 1 calc R U . . .
H24B H -0.094505 1.350426 0.334448 0.273 Uiso 1 1 calc R U . . .
O4 O 0.0007(10) 1.3152(8) 0.3949(9) 0.352(6) Uani 1 1 d D U . . .
H4C H 0.000000 1.371084 0.403353 0.528 Uiso 1 1 d . U . . .
O5 O 0.5241(2) 0.8693(2) 0.05706(18) 0.0805(9) Uani 1 1 d . U . . .
O6 O 0.6492(3) 0.7860(2) -0.04414(19) 0.0941(11) Uani 1 1 d . U . . .
O7 O 0.5521(2) 0.5463(2) 0.36987(18) 0.0768(9) Uani 1 1 d . U . . .
O8 O 0.7177(3) 0.5293(3) 0.3097(2) 0.1088(12) Uani 1 1 d . U . . .
O9 O 0.4623(3) 0.6227(2) 0.05955(19) 0.0844(9) Uani 1 1 d . U . . .
O10 O 0.4013(3) 0.7365(2) -0.0131(2) 0.0892(10) Uani 1 1 d . U . . .
O11 O 0.1025(3) 0.9114(3) 0.4006(2) 0.0966(11) Uani 1 1 d . U . . .
O12 O 0.2293(3) 0.8532(3) 0.4361(2) 0.1075(12) Uani 1 1 d . U . . .
C25 C 0.5890(4) 0.7989(3) 0.0329(3) 0.0737(12) Uani 1 1 d . U . . .
C26 C 0.5953(4) 0.7302(3) 0.0996(3) 0.0694(12) Uani 1 1 d . U . . .
C27 C 0.5111(3) 0.7133(3) 0.1736(3) 0.0674(11) Uani 1 1 d . U . . .
C28 C 0.5286(4) 0.6547(3) 0.2376(3) 0.0694(12) Uani 1 1 d . U . . .
H28 H 0.473457 0.641899 0.286038 0.083 Uiso 1 1 calc R U . . .
C29 C 0.6224(4) 0.6148(3) 0.2337(3) 0.0749(12) Uani 1 1 d . U . . .
C30 C 0.7053(4) 0.6284(3) 0.1593(3) 0.0791(13) Uani 1 1 d . U . . .
H30 H 0.769944 0.600282 0.153367 0.095 Uiso 1 1 calc R U . . .
C31 C 0.6889(4) 0.6848(3) 0.0943(3) 0.0775(13) Uani 1 1 d . U . . .
H31 H 0.744360 0.692831 0.043710 0.093 Uiso 1 1 calc R U . . .
C32 C 0.6317(4) 0.5586(3) 0.3101(3) 0.0765(13) Uani 1 1 d . U . . .
C33 C 0.4128(4) 0.6998(4) 0.0531(3) 0.0762(13) Uani 1 1 d . U . . .
C34 C 0.3589(4) 0.7495(3) 0.1363(3) 0.0726(12) Uani 1 1 d . U . . .
C35 C 0.4072(3) 0.7527(3) 0.1910(2) 0.0644(11) Uani 1 1 d . U . . .
C36 C 0.3452(4) 0.7927(3) 0.2714(3) 0.0689(11) Uani 1 1 d . U . . .
H36 H 0.374893 0.795741 0.309000 0.083 Uiso 1 1 calc R U . . .
C37 C 0.2475(4) 0.8264(3) 0.2978(3) 0.0707(12) Uani 1 1 d . U . . .
C38 C 0.2021(4) 0.8244(3) 0.2430(3) 0.0759(13) Uani 1 1 d . U . . .
H38 H 0.133722 0.848256 0.260460 0.091 Uiso 1 1 calc R U . . .
C39 C 0.2571(4) 0.7872(3) 0.1620(3) 0.0761(13) Uani 1 1 d . U . . .
H39 H 0.226080 0.787250 0.124698 0.091 Uiso 1 1 calc R U . . .
C40 C 0.1868(4) 0.8680(4) 0.3849(3) 0.0838(14) Uani 1 1 d . U . . .
O1S O 0.7764(7) 0.9660(6) 0.2743(6) 0.235(4) Uani 1 1 d . U . . .
N1S N 0.6944(7) 0.8586(6) 0.2779(6) 0.185(3) Uani 1 1 d . U . . .
C1S C 0.6965(10) 0.9374(8) 0.2942(8) 0.190(4) Uani 1 1 d . U . . .
H1S H 0.635341 0.976129 0.322485 0.228 Uiso 1 1 calc R U . . .
C2S C 0.6014(8) 0.8365(7) 0.2921(6) 0.197(4) Uani 1 1 d . U . . .
H2S1 H 0.550132 0.890033 0.301279 0.296 Uiso 1 1 calc R U . . .
H2S2 H 0.582420 0.797253 0.342496 0.296 Uiso 1 1 calc R U . . .
H2S3 H 0.609723 0.807455 0.242003 0.296 Uiso 1 1 calc R U . . .
C3S C 0.7838(12) 0.7935(11) 0.2387(16) 0.401(13) Uani 1 1 d . U . . .
H3S1 H 0.812763 0.779781 0.191792 0.601 Uiso 1 1 d . U . . .
H3S2 H 0.773746 0.735723 0.285625 0.601 Uiso 1 1 d . U . . .
H3S3 H 0.835302 0.810049 0.264991 0.601 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 2.043(4) . ?
Ni1 N3 2.043(4) 2_675 ?
Ni1 N1 2.066(4) . ?
Ni1 N1 2.066(4) 2_675 ?
Ni1 O5 2.159(3) . ?
Ni1 O5 2.159(3) 2_675 ?
N1 C1 1.456(6) . ?
N1 C2 1.472(6) . ?
N1 H1 0.9900 . ?
N2 C2 1.454(7) . ?
N2 C5 1.464(7) . ?
N2 C3 1.470(7) . ?
N3 C4 1.479(6) . ?
N3 C3 1.507(6) . ?
N3 H3 0.9900 . ?
C1 C4 1.545(7) 2_675 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.561(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 O1 1.334(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
Ni2 N6 2.060(4) 2_666 ?
Ni2 N6 2.060(4) . ?
Ni2 N4 2.062(4) . ?
Ni2 N4 2.062(4) 2_666 ?
Ni2 O7 2.115(3) . ?
Ni2 O7 2.115(3) 2_666 ?
N4 C7 1.476(6) . ?
N4 C8 1.511(6) . ?
N4 H4 0.9900 . ?
N5 C8 1.435(7) . ?
N5 C9 1.458(7) . ?
N5 C11B 1.463(9) . ?
N5 C11A 1.467(9) . ?
N6 C9 1.463(6) . ?
N6 C10 1.495(7) . ?
N6 H6 0.9900 . ?
C7 C10 1.505(7) 2_666 ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11A C12A 1.575(9) . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C12A O2A 1.416(9) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
O2A H2A1 0.814(13) . ?
C11B C12B 1.528(10) . ?
C11B H11C 0.9800 . ?
C11B H11D 0.9800 . ?
C12B O2B 1.400(9) . ?
C12B H12C 0.9800 . ?
C12B H12D 0.9800 . ?
O2B H2B1 0.74(2) . ?
Ni3 N9 2.055(5) . ?
Ni3 N9 2.055(5) 2_665 ?
Ni3 N7 2.067(4) . ?
Ni3 N7 2.067(4) 2_665 ?
Ni3 O9 2.129(3) 2_665 ?
Ni3 O9 2.129(3) . ?
N7 C14 1.475(7) . ?
N7 C13 1.488(7) . ?
N7 H7 0.9900 . ?
N8 C15 1.429(7) . ?
N8 C17 1.466(7) . ?
N8 C14 1.469(7) . ?
N9 C15 1.491(6) . ?
N9 C16 1.502(7) . ?
N9 H9 0.9900 . ?
C13 C16 1.501(7) 2_665 ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.503(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 O3 1.460(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
O3 H3C 0.8300 . ?
Ni4 N10 2.050(5) 2_576 ?
Ni4 N10 2.050(5) . ?
Ni4 N12 2.054(4) 2_576 ?
Ni4 N12 2.054(4) . ?
Ni4 O11 2.135(3) . ?
Ni4 O11 2.135(3) 2_576 ?
N10 C19 1.481(8) . ?
N10 C20 1.499(7) . ?
N10 H10 0.9900 . ?
N11 C21 1.432(8) . ?
N11 C20 1.455(8) . ?
N11 C23 1.470(6) . ?
N12 C22 1.440(7) . ?
N12 C21 1.503(7) . ?
N12 H12 0.9900 . ?
C19 C22 1.525(9) 2_576 ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C24 1.549(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 O4 1.479(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
O4 H4C 0.902(10) . ?
O5 C25 1.263(5) . ?
O6 C25 1.255(5) . ?
O7 C32 1.253(6) . ?
O8 C32 1.271(6) . ?
O9 C33 1.272(6) . ?
O10 C33 1.259(6) . ?
O11 C40 1.225(6) . ?
O12 C40 1.260(6) . ?
C25 C26 1.477(6) . ?
C26 C31 1.393(6) . ?
C26 C27 1.423(6) . ?
C27 C28 1.402(6) . ?
C27 C35 1.460(6) . ?
C28 C29 1.385(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.401(6) . ?
C29 C32 1.513(7) . ?
C30 C31 1.393(6) . ?
C30 H30 0.9400 . ?
C31 H31 0.9400 . ?
C33 C34 1.516(6) . ?
C34 C39 1.406(6) . ?
C34 C35 1.424(6) . ?
C35 C36 1.418(6) . ?
C36 C37 1.341(6) . ?
C36 H36 0.9400 . ?
C37 C38 1.386(6) . ?
C37 C40 1.515(6) . ?
C38 C39 1.397(6) . ?
C38 H38 0.9400 . ?
C39 H39 0.9400 . ?
O1S C1S 1.294(12) . ?
N1S C1S 1.311(11) . ?
N1S C3S 1.435(15) . ?
N1S C2S 1.453(11) . ?
C1S H1S 0.9400 . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
C2S H2S3 0.9700 . ?
C3S H3S1 0.76(2) . ?
C3S H3S2 1.12(2) . ?
C3S H3S3 1.146(19) . ?

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
N3 Ni1 N3 180.0 . 2_675 ?
N3 Ni1 N1 93.77(16) . . ?
N3 Ni1 N1 86.23(16) 2_675 . ?
N3 Ni1 N1 86.23(16) . 2_675 ?
N3 Ni1 N1 93.77(16) 2_675 2_675 ?
N1 Ni1 N1 180.0 . 2_675 ?
N3 Ni1 O5 87.51(14) . . ?
N3 Ni1 O5 92.49(15) 2_675 . ?
N1 Ni1 O5 92.74(14) . . ?
N1 Ni1 O5 87.26(14) 2_675 . ?
N3 Ni1 O5 92.49(15) . 2_675 ?
N3 Ni1 O5 87.51(15) 2_675 2_675 ?
N1 Ni1 O5 87.26(14) . 2_675 ?
N1 Ni1 O5 92.74(14) 2_675 2_675 ?
O5 Ni1 O5 180.0 . 2_675 ?
C1 N1 C2 113.8(4) . . ?
C1 N1 Ni1 104.9(3) . . ?
C2 N1 Ni1 113.7(3) . . ?
C1 N1 H1 108.1 . . ?
C2 N1 H1 108.1 . . ?
Ni1 N1 H1 108.1 . . ?
C2 N2 C5 113.3(5) . . ?
C2 N2 C3 117.6(4) . . ?
C5 N2 C3 116.3(5) . . ?
C4 N3 C3 111.2(4) . . ?
C4 N3 Ni1 107.6(3) . . ?
C3 N3 Ni1 115.4(3) . . ?
C4 N3 H3 107.5 . . ?
C3 N3 H3 107.5 . . ?
Ni1 N3 H3 107.5 . . ?
N1 C1 C4 111.3(4) . 2_675 ?
N1 C1 H1A 109.4 . . ?
C4 C1 H1A 109.4 2_675 . ?
N1 C1 H1B 109.4 . . ?
C4 C1 H1B 109.4 2_675 . ?
H1A C1 H1B 108.0 . . ?
N2 C2 N1 115.0(4) . . ?
N2 C2 H2A 108.5 . . ?
N1 C2 H2A 108.5 . . ?
N2 C2 H2B 108.5 . . ?
N1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N2 C3 N3 112.5(4) . . ?
N2 C3 H3A 109.1 . . ?
N3 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
N3 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N3 C4 C1 106.9(4) . 2_675 ?
N3 C4 H4A 110.3 . . ?
C1 C4 H4A 110.3 2_675 . ?
N3 C4 H4B 110.3 . . ?
C1 C4 H4B 110.3 2_675 . ?
H4A C4 H4B 108.6 . . ?
N2 C5 C6 115.0(6) . . ?
N2 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
O1 C6 C5 109.1(8) . . ?
O1 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O1 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N6 Ni2 N6 180.0 2_666 . ?
N6 Ni2 N4 85.28(17) 2_666 . ?
N6 Ni2 N4 94.72(17) . . ?
N6 Ni2 N4 94.72(17) 2_666 2_666 ?
N6 Ni2 N4 85.29(17) . 2_666 ?
N4 Ni2 N4 180.0 . 2_666 ?
N6 Ni2 O7 92.76(14) 2_666 . ?
N6 Ni2 O7 87.24(14) . . ?
N4 Ni2 O7 90.91(14) . . ?
N4 Ni2 O7 89.09(14) 2_666 . ?
N6 Ni2 O7 87.24(14) 2_666 2_666 ?
N6 Ni2 O7 92.76(14) . 2_666 ?
N4 Ni2 O7 89.09(14) . 2_666 ?
N4 Ni2 O7 90.91(14) 2_666 2_666 ?
O7 Ni2 O7 180.0 . 2_666 ?
C7 N4 C8 114.1(4) . . ?
C7 N4 Ni2 107.0(3) . . ?
C8 N4 Ni2 113.2(3) . . ?
C7 N4 H4 107.4 . . ?
C8 N4 H4 107.4 . . ?
Ni2 N4 H4 107.4 . . ?
C8 N5 C9 117.4(5) . . ?
C8 N5 C11B 115.3(11) . . ?
C9 N5 C11B 115.7(10) . . ?
C8 N5 C11A 115.2(9) . . ?
C9 N5 C11A 114.2(8) . . ?
C9 N6 C10 114.0(4) . . ?
C9 N6 Ni2 113.5(3) . . ?
C10 N6 Ni2 105.8(3) . . ?
C9 N6 H6 107.8 . . ?
C10 N6 H6 107.8 . . ?
Ni2 N6 H6 107.8 . . ?
N4 C7 C10 108.2(4) . 2_666 ?
N4 C7 H7A 110.1 . . ?
C10 C7 H7A 110.1 2_666 . ?
N4 C7 H7B 110.1 . . ?
C10 C7 H7B 110.1 2_666 . ?
H7A C7 H7B 108.4 . . ?
N5 C8 N4 113.5(4) . . ?
N5 C8 H8A 108.9 . . ?
N4 C8 H8A 108.9 . . ?
N5 C8 H8B 108.9 . . ?
N4 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N5 C9 N6 113.6(5) . . ?
N5 C9 H9A 108.8 . . ?
N6 C9 H9A 108.8 . . ?
N5 C9 H9B 108.8 . . ?
N6 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N6 C10 C7 109.4(4) . 2_666 ?
N6 C10 H10A 109.8 . . ?
C7 C10 H10A 109.8 2_666 . ?
N6 C10 H10B 109.8 . . ?
C7 C10 H10B 109.8 2_666 . ?
H10A C10 H10B 108.2 . . ?
N5 C11A C12A 133.4(11) . . ?
N5 C11A H11A 103.9 . . ?
C12A C11A H11A 103.9 . . ?
N5 C11A H11B 103.9 . . ?
C12A C11A H11B 103.9 . . ?
H11A C11A H11B 105.4 . . ?
O2A C12A C11A 106.4(11) . . ?
O2A C12A H12A 110.5 . . ?
C11A C12A H12A 110.5 . . ?
O2A C12A H12B 110.5 . . ?
C11A C12A H12B 110.5 . . ?
H12A C12A H12B 108.6 . . ?
C12A O2A H2A1 114.7(16) . . ?
N5 C11B C12B 110.9(12) . . ?
N5 C11B H11C 109.4 . . ?
C12B C11B H11C 109.4 . . ?
N5 C11B H11D 109.4 . . ?
C12B C11B H11D 109.4 . . ?
H11C C11B H11D 108.0 . . ?
O2B C12B C11B 122.8(15) . . ?
O2B C12B H12C 106.6 . . ?
C11B C12B H12C 106.6 . . ?
O2B C12B H12D 106.6 . . ?
C11B C12B H12D 106.6 . . ?
H12C C12B H12D 106.6 . . ?
C12B O2B H2B1 116(2) . . ?
N9 Ni3 N9 180.0 . 2_665 ?
N9 Ni3 N7 94.31(18) . . ?
N9 Ni3 N7 85.69(18) 2_665 . ?
N9 Ni3 N7 85.69(18) . 2_665 ?
N9 Ni3 N7 94.31(18) 2_665 2_665 ?
N7 Ni3 N7 180.0 . 2_665 ?
N9 Ni3 O9 93.66(16) . 2_665 ?
N9 Ni3 O9 86.34(15) 2_665 2_665 ?
N7 Ni3 O9 88.32(14) . 2_665 ?
N7 Ni3 O9 91.68(14) 2_665 2_665 ?
N9 Ni3 O9 86.34(15) . . ?
N9 Ni3 O9 93.66(15) 2_665 . ?
N7 Ni3 O9 91.68(14) . . ?
N7 Ni3 O9 88.32(14) 2_665 . ?
O9 Ni3 O9 180.0 2_665 . ?
C14 N7 C13 113.3(4) . . ?
C14 N7 Ni3 113.3(4) . . ?
C13 N7 Ni3 105.3(3) . . ?
C14 N7 H7 108.2 . . ?
C13 N7 H7 108.2 . . ?
Ni3 N7 H7 108.2 . . ?
C15 N8 C17 118.0(5) . . ?
C15 N8 C14 117.7(5) . . ?
C17 N8 C14 111.0(5) . . ?
C15 N9 C16 114.1(4) . . ?
C15 N9 Ni3 114.0(4) . . ?
C16 N9 Ni3 106.5(3) . . ?
C15 N9 H9 107.3 . . ?
C16 N9 H9 107.3 . . ?
Ni3 N9 H9 107.3 . . ?
N7 C13 C16 109.1(4) . 2_665 ?
N7 C13 H13A 109.9 . . ?
C16 C13 H13A 109.9 2_665 . ?
N7 C13 H13B 109.9 . . ?
C16 C13 H13B 109.9 2_665 . ?
H13A C13 H13B 108.3 . . ?
N8 C14 N7 115.0(4) . . ?
N8 C14 H14A 108.5 . . ?
N7 C14 H14A 108.5 . . ?
N8 C14 H14B 108.5 . . ?
N7 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
N8 C15 N9 113.1(5) . . ?
N8 C15 H15A 109.0 . . ?
N9 C15 H15A 109.0 . . ?
N8 C15 H15B 109.0 . . ?
N9 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C13 C16 N9 108.4(5) 2_665 . ?
C13 C16 H16A 110.0 2_665 . ?
N9 C16 H16A 110.0 . . ?
C13 C16 H16B 110.0 2_665 . ?
N9 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
N8 C17 C18 113.6(6) . . ?
N8 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
N8 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
O3 C18 C17 114.9(5) . . ?
O3 C18 H18A 108.5 . . ?
C17 C18 H18A 108.5 . . ?
O3 C18 H18B 108.5 . . ?
C17 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C18 O3 H3C 109.5 . . ?
N10 Ni4 N10 180.0 2_576 . ?
N10 Ni4 N12 94.9(2) 2_576 2_576 ?
N10 Ni4 N12 85.1(2) . 2_576 ?
N10 Ni4 N12 85.1(2) 2_576 . ?
N10 Ni4 N12 94.9(2) . . ?
N12 Ni4 N12 180.0 2_576 . ?
N10 Ni4 O11 87.68(16) 2_576 . ?
N10 Ni4 O11 92.32(16) . . ?
N12 Ni4 O11 93.64(15) 2_576 . ?
N12 Ni4 O11 86.36(15) . . ?
N10 Ni4 O11 92.32(16) 2_576 2_576 ?
N10 Ni4 O11 87.68(16) . 2_576 ?
N12 Ni4 O11 86.35(15) 2_576 2_576 ?
N12 Ni4 O11 93.65(15) . 2_576 ?
O11 Ni4 O11 180.0 . 2_576 ?
C19 N10 C20 115.3(5) . . ?
C19 N10 Ni4 105.3(4) . . ?
C20 N10 Ni4 113.0(4) . . ?
C19 N10 H10 107.6 . . ?
C20 N10 H10 107.6 . . ?
Ni4 N10 H10 107.6 . . ?
C21 N11 C20 115.7(6) . . ?
C21 N11 C23 113.6(5) . . ?
C20 N11 C23 116.9(6) . . ?
C22 N12 C21 113.8(5) . . ?
C22 N12 Ni4 107.5(4) . . ?
C21 N12 Ni4 114.4(4) . . ?
C22 N12 H12 106.9 . . ?
C21 N12 H12 106.9 . . ?
Ni4 N12 H12 106.9 . . ?
N10 C19 C22 108.8(5) . 2_576 ?
N10 C19 H19A 109.9 . . ?
C22 C19 H19A 109.9 2_576 . ?
N10 C19 H19B 109.9 . . ?
C22 C19 H19B 109.9 2_576 . ?
H19A C19 H19B 108.3 . . ?
N11 C20 N10 115.0(5) . . ?
N11 C20 H20A 108.5 . . ?
N10 C20 H20A 108.5 . . ?
N11 C20 H20B 108.5 . . ?
N10 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
N11 C21 N12 114.1(5) . . ?
N11 C21 H21A 108.7 . . ?
N12 C21 H21A 108.7 . . ?
N11 C21 H21B 108.7 . . ?
N12 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N12 C22 C19 107.6(5) . 2_576 ?
N12 C22 H22A 110.2 . . ?
C19 C22 H22A 110.2 2_576 . ?
N12 C22 H22B 110.2 . . ?
C19 C22 H22B 110.2 2_576 . ?
H22A C22 H22B 108.5 . . ?
N11 C23 C24 121.9(7) . . ?
N11 C23 H23A 106.9 . . ?
C24 C23 H23A 106.9 . . ?
N11 C23 H23B 106.9 . . ?
C24 C23 H23B 106.9 . . ?
H23A C23 H23B 106.7 . . ?
O4 C24 C23 104.0(7) . . ?
O4 C24 H24A 111.0 . . ?
C23 C24 H24A 111.0 . . ?
O4 C24 H24B 111.0 . . ?
C23 C24 H24B 111.0 . . ?
H24A C24 H24B 109.0 . . ?
C24 O4 H4C 116.6(12) . . ?
C25 O5 Ni1 134.7(3) . . ?
C32 O7 Ni2 138.9(3) . . ?
C33 O9 Ni3 135.8(3) . . ?
C40 O11 Ni4 133.4(3) . . ?
O6 C25 O5 123.1(4) . . ?
O6 C25 C26 119.1(4) . . ?
O5 C25 C26 117.7(4) . . ?
C31 C26 C27 117.8(4) . . ?
C31 C26 C25 118.6(4) . . ?
C27 C26 C25 123.3(4) . . ?
C28 C27 C26 117.5(4) . . ?
C28 C27 C35 116.0(4) . . ?
C26 C27 C35 126.5(4) . . ?
C29 C28 C27 123.8(4) . . ?
C29 C28 H28 118.1 . . ?
C27 C28 H28 118.1 . . ?
C28 C29 C30 118.7(4) . . ?
C28 C29 C32 118.8(4) . . ?
C30 C29 C32 122.5(5) . . ?
C31 C30 C29 118.0(5) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C30 C31 C26 124.0(4) . . ?
C30 C31 H31 118.0 . . ?
C26 C31 H31 118.0 . . ?
O7 C32 O8 125.5(5) . . ?
O7 C32 C29 116.1(5) . . ?
O8 C32 C29 118.4(5) . . ?
O10 C33 O9 127.1(4) . . ?
O10 C33 C34 118.0(5) . . ?
O9 C33 C34 114.8(4) . . ?
C39 C34 C35 120.2(4) . . ?
C39 C34 C33 118.2(4) . . ?
C35 C34 C33 121.4(4) . . ?
C36 C35 C34 115.4(4) . . ?
C36 C35 C27 118.9(4) . . ?
C34 C35 C27 125.6(4) . . ?
C37 C36 C35 125.0(4) . . ?
C37 C36 H36 117.5 . . ?
C35 C36 H36 117.5 . . ?
C36 C37 C38 118.8(4) . . ?
C36 C37 C40 121.5(5) . . ?
C38 C37 C40 119.7(5) . . ?
C37 C38 C39 120.5(5) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C34 120.0(5) . . ?
C38 C39 H39 120.0 . . ?
C34 C39 H39 120.0 . . ?
O11 C40 O12 125.6(5) . . ?
O11 C40 C37 119.3(5) . . ?
O12 C40 C37 115.1(5) . . ?
C1S N1S C3S 121.7(11) . . ?
C1S N1S C2S 120.9(10) . . ?
C3S N1S C2S 117.2(10) . . ?
O1S C1S N1S 125.0(12) . . ?
O1S C1S H1S 117.5 . . ?
N1S C1S H1S 117.5 . . ?
N1S C2S H2S1 109.5 . . ?
N1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
N1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S C3S H3S1 131(3) . . ?
N1S C3S H3S2 103.7(16) . . ?
H3S1 C3S H3S2 112.9(15) . . ?
N1S C3S H3S3 101.9(12) . . ?
H3S1 C3S H3S3 110.5(18) . . ?
H3S2 C3S H3S3 88.6(18) . . ?

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
C2 N1 C1 C4 165.3(4) . . . 2_675 ?
Ni1 N1 C1 C4 40.4(5) . . . 2_675 ?
C5 N2 C2 N1 -71.1(5) . . . . ?
C3 N2 C2 N1 69.2(6) . . . . ?
C1 N1 C2 N2 -176.8(4) . . . . ?
Ni1 N1 C2 N2 -56.7(5) . . . . ?
C2 N2 C3 N3 -66.9(6) . . . . ?
C5 N2 C3 N3 72.2(6) . . . . ?
C4 N3 C3 N2 178.4(4) . . . . ?
Ni1 N3 C3 N2 55.5(5) . . . . ?
C3 N3 C4 C1 -165.6(4) . . . 2_675 ?
Ni1 N3 C4 C1 -38.4(5) . . . 2_675 ?
C2 N2 C5 C6 -149.6(6) . . . . ?
C3 N2 C5 C6 69.5(7) . . . . ?
N2 C5 C6 O1 58.7(10) . . . . ?
C8 N4 C7 C10 166.8(4) . . . 2_666 ?
Ni2 N4 C7 C10 40.8(5) . . . 2_666 ?
C9 N5 C8 N4 70.3(6) . . . . ?
C11B N5 C8 N4 -71.4(10) . . . . ?
C11A N5 C8 N4 -68.7(7) . . . . ?
C7 N4 C8 N5 -177.6(5) . . . . ?
Ni2 N4 C8 N5 -54.9(5) . . . . ?
C8 N5 C9 N6 -72.2(6) . . . . ?
C11B N5 C9 N6 69.4(11) . . . . ?
C11A N5 C9 N6 67.2(9) . . . . ?
C10 N6 C9 N5 178.5(4) . . . . ?
Ni2 N6 C9 N5 57.3(5) . . . . ?
C9 N6 C10 C7 -166.0(4) . . . 2_666 ?
Ni2 N6 C10 C7 -40.5(5) . . . 2_666 ?
C8 N5 C11A C12A -121(2) . . . . ?
C9 N5 C11A C12A 99(2) . . . . ?
N5 C11A C12A O2A -13(4) . . . . ?
C8 N5 C11B C12B -61.8(18) . . . . ?
C9 N5 C11B C12B 155.9(13) . . . . ?
N5 C11B C12B O2B -58(3) . . . . ?
C14 N7 C13 C16 167.3(5) . . . 2_665 ?
Ni3 N7 C13 C16 42.9(5) . . . 2_665 ?
C15 N8 C14 N7 69.1(7) . . . . ?
C17 N8 C14 N7 -71.2(6) . . . . ?
C13 N7 C14 N8 -174.4(5) . . . . ?
Ni3 N7 C14 N8 -54.4(6) . . . . ?
C17 N8 C15 N9 67.9(7) . . . . ?
C14 N8 C15 N9 -69.6(6) . . . . ?
C16 N9 C15 N8 180.0(5) . . . . ?
Ni3 N9 C15 N8 57.4(6) . . . . ?
C15 N9 C16 C13 -166.0(5) . . . 2_665 ?
Ni3 N9 C16 C13 -39.4(5) . . . 2_665 ?
C15 N8 C17 C18 46.7(7) . . . . ?
C14 N8 C17 C18 -173.1(5) . . . . ?
N8 C17 C18 O3 -78.0(7) . . . . ?
C20 N10 C19 C22 -167.2(5) . . . 2_576 ?
Ni4 N10 C19 C22 -41.9(5) . . . 2_576 ?
C21 N11 C20 N10 -71.5(7) . . . . ?
C23 N11 C20 N10 66.5(8) . . . . ?
C19 N10 C20 N11 177.6(6) . . . . ?
Ni4 N10 C20 N11 56.4(7) . . . . ?
C20 N11 C21 N12 70.0(6) . . . . ?
C23 N11 C21 N12 -69.4(7) . . . . ?
C22 N12 C21 N11 -179.4(5) . . . . ?
Ni4 N12 C21 N11 -55.3(6) . . . . ?
C21 N12 C22 C19 168.9(5) . . . 2_576 ?
Ni4 N12 C22 C19 41.1(5) . . . 2_576 ?
C21 N11 C23 C24 -165.2(6) . . . . ?
C20 N11 C23 C24 55.9(8) . . . . ?
N11 C23 C24 O4 -83.6(11) . . . . ?
Ni1 O5 C25 O6 -14.7(8) . . . . ?
Ni1 O5 C25 C26 163.3(3) . . . . ?
O6 C25 C26 C31 39.0(7) . . . . ?
O5 C25 C26 C31 -139.0(5) . . . . ?
O6 C25 C26 C27 -146.9(5) . . . . ?
O5 C25 C26 C27 35.0(7) . . . . ?
C31 C26 C27 C28 2.6(6) . . . . ?
C25 C26 C27 C28 -171.5(4) . . . . ?
C31 C26 C27 C35 -179.2(4) . . . . ?
C25 C26 C27 C35 6.7(7) . . . . ?
C26 C27 C28 C29 1.7(7) . . . . ?
C35 C27 C28 C29 -176.7(4) . . . . ?
C27 C28 C29 C30 -4.4(7) . . . . ?
C27 C28 C29 C32 175.2(4) . . . . ?
C28 C29 C30 C31 2.7(7) . . . . ?
C32 C29 C30 C31 -176.8(4) . . . . ?
C29 C30 C31 C26 1.6(7) . . . . ?
C27 C26 C31 C30 -4.3(7) . . . . ?
C25 C26 C31 C30 170.1(4) . . . . ?
Ni2 O7 C32 O8 13.0(8) . . . . ?
Ni2 O7 C32 C29 -165.7(3) . . . . ?
C28 C29 C32 O7 5.6(7) . . . . ?
C30 C29 C32 O7 -174.8(4) . . . . ?
C28 C29 C32 O8 -173.1(4) . . . . ?
C30 C29 C32 O8 6.4(7) . . . . ?
Ni3 O9 C33 O10 -30.0(8) . . . . ?
Ni3 O9 C33 C34 147.0(4) . . . . ?
O10 C33 C34 C39 48.7(6) . . . . ?
O9 C33 C34 C39 -128.5(5) . . . . ?
O10 C33 C34 C35 -136.1(5) . . . . ?
O9 C33 C34 C35 46.7(6) . . . . ?
C39 C34 C35 C36 2.1(6) . . . . ?
C33 C34 C35 C36 -173.0(4) . . . . ?
C39 C34 C35 C27 177.4(4) . . . . ?
C33 C34 C35 C27 2.3(7) . . . . ?
C28 C27 C35 C36 50.2(6) . . . . ?
C26 C27 C35 C36 -128.0(5) . . . . ?
C28 C27 C35 C34 -125.0(5) . . . . ?
C26 C27 C35 C34 56.7(7) . . . . ?
C34 C35 C36 C37 0.0(7) . . . . ?
C27 C35 C36 C37 -175.7(4) . . . . ?
C35 C36 C37 C38 -1.3(7) . . . . ?
C35 C36 C37 C40 -180.0(4) . . . . ?
C36 C37 C38 C39 0.6(7) . . . . ?
C40 C37 C38 C39 179.3(5) . . . . ?
C37 C38 C39 C34 1.4(7) . . . . ?
C35 C34 C39 C38 -2.8(7) . . . . ?
C33 C34 C39 C38 172.4(4) . . . . ?
Ni4 O11 C40 O12 13.8(9) . . . . ?
Ni4 O11 C40 C37 -167.0(3) . . . . ?
C36 C37 C40 O11 167.4(5) . . . . ?
C38 C37 C40 O11 -11.3(8) . . . . ?
C36 C37 C40 O12 -13.4(7) . . . . ?
C38 C37 C40 O12 168.0(5) . . . . ?
C3S N1S C1S O1S 3(2) . . . . ?
C2S N1S C1S O1S -171.6(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O6 0.99 2.02 2.909(5) 147.8 . yes
N3 H3 O10 0.99 2.56 3.532(5) 168.0 . yes
N4 H4 O8 0.99 2.15 3.013(5) 144.9 . yes
N7 H7 O10 0.99 2.20 3.068(5) 145.5 . yes
N9 H9 O3 0.99 2.54 3.182(7) 122.6 . yes
O3 H3C O6 0.83 1.88 2.672(6) 159.7 . yes
N12 H12 O12 0.99 1.99 2.888(5) 149.3 2_576 yes

_refine_diff_density_max         0.789
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.069























####################################################################### 
# 
# 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_asflex_CN_sq
_database_code_depnum_ccdc_archive 'CCDC 1898507'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        as-flexMOF(CN)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H62 N16 Ni2 O8'
_chemical_formula_sum            'C44 H62 N16 Ni2 O8'
_chemical_formula_weight         1060.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0875 '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                   21.799(4)
_cell_length_b                   25.727(5)
_cell_length_c                   15.630(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.86(3)
_cell_angle_gamma                90
_cell_volume                     8746(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    88099
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       block
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.805
_exptl_crystal_F_000             2232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    0.449
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35918
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.718
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9987
_reflns_number_gt                7287
_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       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2015b)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  CIFTAB
_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)+(0.0956P)²] 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         9987
_refine_ls_number_parameters     319
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1676
_refine_ls_wR_factor_gt          0.1618
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.111
_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
N8 N 0.4330(2) 0.2277(3) 0.6175(4) 0.219(3) Uani 1 1 d . . . . .
Ni1 Ni 0.500000 0.500000 0.000000 0.03756(12) Uani 1 2 d S . P . .
Ni2 Ni 0.750000 0.250000 0.500000 0.04603(13) Uani 1 2 d S . P . .
O1 O 0.51857(7) 0.46793(6) 0.12358(8) 0.0444(3) Uani 1 1 d . . . . .
O2 O 0.57801(7) 0.52118(6) 0.20663(9) 0.0510(4) Uani 1 1 d . . . . .
O3 O 0.69322(7) 0.30212(6) 0.42609(10) 0.0533(4) Uani 1 1 d . . . . .
O4 O 0.60756(9) 0.25871(7) 0.38797(13) 0.0738(6) Uani 1 1 d . . . . .
N1 N 0.53673(8) 0.57059(7) 0.03665(10) 0.0447(4) Uani 1 1 d . . . . .
H1 H 0.545731 0.570102 0.099577 0.054 Uiso 1 1 calc R U . . .
N2 N 0.43627(10) 0.61057(8) 0.05339(12) 0.0574(5) Uani 1 1 d . . . . .
N3 N 0.41363(8) 0.51734(7) 0.03869(11) 0.0472(4) Uani 1 1 d . . . . .
H3 H 0.414942 0.512728 0.101668 0.057 Uiso 1 1 calc R U . . .
N4 N 0.40612(15) 0.67020(13) 0.33686(18) 0.1044(10) Uani 1 1 d . . . . .
N5 N 0.69469(9) 0.18747(7) 0.46701(13) 0.0552(5) Uani 1 1 d . . . . .
H5 H 0.656416 0.201704 0.438390 0.066 Uiso 1 1 calc R U . . .
N6 N 0.64748(11) 0.18573(9) 0.60453(16) 0.0704(6) Uani 1 1 d . . . . .
N7 N 0.70526(10) 0.26834(8) 0.60771(13) 0.0580(5) Uani 1 1 d . . . . .
H7 H 0.667769 0.288219 0.589383 0.070 Uiso 1 1 calc R U . . .
C1 C 0.59519(11) 0.57436(10) -0.00425(14) 0.0548(6) Uani 1 1 d . . . . .
H1A H 0.621217 0.600857 0.024965 0.066 Uiso 1 1 calc R U . . .
H1AB H 0.587395 0.584893 -0.064255 0.066 Uiso 1 1 calc R U . . .
C2 C 0.49444(12) 0.61433(9) 0.01520(14) 0.0536(6) Uani 1 1 d . . . . .
H2A H 0.514565 0.646815 0.034053 0.064 Uiso 1 1 calc R U . . .
H2AB H 0.486851 0.616053 -0.047252 0.064 Uiso 1 1 calc R U . . .
C3 C 0.39397(12) 0.57183(10) 0.01969(15) 0.0571(6) Uani 1 1 d . . . . .
H3A H 0.388350 0.576170 -0.042639 0.069 Uiso 1 1 calc R U . . .
H3AB H 0.354034 0.577685 0.043332 0.069 Uiso 1 1 calc R U . . .
C4 C 0.37184(10) 0.47759(10) 0.00014(14) 0.0557(6) Uani 1 1 d . . . . .
H4A H 0.360018 0.486584 -0.059628 0.067 Uiso 1 1 calc R U . . .
H4AB H 0.334484 0.475683 0.031551 0.067 Uiso 1 1 calc R U . . .
C5 C 0.44035(14) 0.61678(10) 0.14605(15) 0.0657(7) Uani 1 1 d . . . . .
H5A H 0.479667 0.633212 0.164139 0.079 Uiso 1 1 calc R U . . .
H5AB H 0.439443 0.582441 0.173074 0.079 Uiso 1 1 calc R U . . .
C6 C 0.39004(19) 0.64842(17) 0.1754(2) 0.1061(12) Uani 1 1 d . U . . .
H6A H 0.387480 0.680888 0.142595 0.127 Uiso 1 1 calc R U . . .
H6B H 0.351180 0.629708 0.164136 0.127 Uiso 1 1 calc R U . . .
C7 C 0.39796(17) 0.66054(15) 0.2658(2) 0.0967(12) Uani 1 1 d . . . . .
C8 C 0.72558(14) 0.15846(10) 0.40167(18) 0.0704(8) Uani 1 1 d . . . . .
H8A H 0.696007 0.135949 0.369490 0.084 Uiso 1 1 calc R U . . .
H8AB H 0.758062 0.136564 0.428987 0.084 Uiso 1 1 calc R U . . .
C9 C 0.67621(13) 0.15599(10) 0.53998(19) 0.0683(8) Uani 1 1 d . . . . .
H9A H 0.647573 0.128948 0.518266 0.082 Uiso 1 1 calc R U . . .
H9AB H 0.712689 0.138641 0.566634 0.082 Uiso 1 1 calc R U . . .
C10 C 0.68617(14) 0.22158(11) 0.65593(17) 0.0697(7) Uani 1 1 d . . . . .
H10A H 0.723104 0.203090 0.678467 0.084 Uiso 1 1 calc R U . . .
H10B H 0.663862 0.233027 0.704952 0.084 Uiso 1 1 calc R U . . .
C11 C 0.74710(14) 0.30327(11) 0.65811(17) 0.0693(7) Uani 1 1 d . . . . .
H11A H 0.779895 0.283057 0.688419 0.083 Uiso 1 1 calc R U . . .
H11B H 0.724490 0.321871 0.700755 0.083 Uiso 1 1 calc R U . . .
C12 C 0.58522(14) 0.20376(14) 0.5804(2) 0.0862(9) Uani 1 1 d . . . . .
H12A H 0.585919 0.241505 0.572077 0.103 Uiso 1 1 calc R U . . .
H12B H 0.570988 0.187804 0.525687 0.103 Uiso 1 1 calc R U . . .
C13 C 0.5424(2) 0.1914(2) 0.6439(4) 0.166(2) Uani 1 1 d . . . . .
H13A H 0.539147 0.153484 0.647866 0.199 Uiso 1 1 calc R U . . .
H13B H 0.559358 0.204092 0.699697 0.199 Uiso 1 1 calc R U . . .
C14 C 0.4816(3) 0.2125(3) 0.6280(4) 0.172(3) Uani 1 1 d . . . . .
C15 C 0.55531(9) 0.47788(8) 0.18773(12) 0.0388(4) Uani 1 1 d . . . . .
C16 C 0.57408(9) 0.43116(8) 0.24239(11) 0.0358(4) Uani 1 1 d . . . . .
C17 C 0.63652(9) 0.42665(8) 0.26898(12) 0.0424(5) Uani 1 1 d . . . . .
H17 H 0.663675 0.453501 0.256170 0.051 Uiso 1 1 calc R U . . .
C18 C 0.65907(10) 0.38357(9) 0.31365(12) 0.0443(5) Uani 1 1 d . . . . .
H18 H 0.701101 0.381430 0.331136 0.053 Uiso 1 1 calc R U . . .
C19 C 0.61982(10) 0.34367(8) 0.33259(12) 0.0401(5) Uani 1 1 d . . . . .
C20 C 0.55757(10) 0.34769(7) 0.30602(11) 0.0380(4) Uani 1 1 d . . . . .
H20 H 0.530843 0.320417 0.318275 0.046 Uiso 1 1 calc R U . . .
C21 C 0.53412(8) 0.39102(7) 0.26188(10) 0.0335(4) Uani 1 1 d . . . . .
C22 C 0.64168(11) 0.29749(9) 0.38628(13) 0.0484(5) 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
N8 C14 1.132(6) . ?
Ni1 N1 2.0507(18) 5_665 ?
Ni1 N1 2.0507(18) . ?
Ni1 N3 2.0644(19) 5_665 ?
Ni1 N3 2.0645(19) . ?
Ni1 O1 2.1143(13) 5_665 ?
Ni1 O1 2.1143(13) . ?
Ni2 N5 2.0550(19) 7_656 ?
Ni2 N5 2.0550(19) . ?
Ni2 N7 2.056(2) . ?
Ni2 N7 2.056(2) 7_656 ?
Ni2 O3 2.1148(14) . ?
Ni2 O3 2.1148(14) 7_656 ?
O1 C15 1.267(2) . ?
O2 C15 1.246(2) . ?
O3 C22 1.253(2) . ?
O4 C22 1.246(3) . ?
N1 C1 1.467(3) . ?
N1 C2 1.479(3) . ?
N1 H1 0.9900 . ?
N2 C3 1.434(3) . ?
N2 C2 1.441(3) . ?
N2 C5 1.454(3) . ?
N3 C4 1.471(3) . ?
N3 C3 1.490(3) . ?
N3 H3 0.9900 . ?
N4 C7 1.140(4) . ?
N5 C8 1.465(3) . ?
N5 C9 1.477(3) . ?
N5 H5 0.9900 . ?
N6 C9 1.442(4) . ?
N6 C10 1.455(4) . ?
N6 C12 1.460(4) . ?
N7 C11 1.471(3) . ?
N7 C10 1.493(3) . ?
N7 H7 0.9900 . ?
C1 C4 1.517(3) 5_665 ?
C1 H1A 0.9800 . ?
C1 H1AB 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2AB 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3AB 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4AB 0.9800 . ?
C5 C6 1.464(4) . ?
C5 H5A 0.9800 . ?
C5 H5AB 0.9800 . ?
C6 C7 1.446(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C8 C11 1.507(4) 7_656 ?
C8 H8A 0.9800 . ?
C8 H8AB 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9AB 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.443(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 C14 1.438(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C15 C16 1.515(3) . ?
C16 C21 1.398(3) . ?
C16 C17 1.401(3) . ?
C17 C18 1.383(3) . ?
C17 H17 0.9400 . ?
C18 C19 1.381(3) . ?
C18 H18 0.9400 . ?
C19 C20 1.396(3) . ?
C19 C22 1.513(3) . ?
C20 C21 1.390(2) . ?
C20 H20 0.9400 . ?
C21 C21 1.509(3) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 5_665 . ?
N1 Ni1 N3 94.21(8) 5_665 5_665 ?
N1 Ni1 N3 85.79(8) . 5_665 ?
N1 Ni1 N3 85.79(8) 5_665 . ?
N1 Ni1 N3 94.21(8) . . ?
N3 Ni1 N3 180.0 5_665 . ?
N1 Ni1 O1 92.47(6) 5_665 5_665 ?
N1 Ni1 O1 87.52(6) . 5_665 ?
N3 Ni1 O1 86.50(7) 5_665 5_665 ?
N3 Ni1 O1 93.50(7) . 5_665 ?
N1 Ni1 O1 87.53(6) 5_665 . ?
N1 Ni1 O1 92.47(6) . . ?
N3 Ni1 O1 93.50(7) 5_665 . ?
N3 Ni1 O1 86.51(7) . . ?
O1 Ni1 O1 180.0 5_665 . ?
N5 Ni2 N5 180.0 7_656 . ?
N5 Ni2 N7 85.27(9) 7_656 . ?
N5 Ni2 N7 94.73(9) . . ?
N5 Ni2 N7 94.73(9) 7_656 7_656 ?
N5 Ni2 N7 85.27(9) . 7_656 ?
N7 Ni2 N7 180.0 . 7_656 ?
N5 Ni2 O3 87.29(7) 7_656 . ?
N5 Ni2 O3 92.71(7) . . ?
N7 Ni2 O3 90.53(7) . . ?
N7 Ni2 O3 89.47(7) 7_656 . ?
N5 Ni2 O3 92.71(7) 7_656 7_656 ?
N5 Ni2 O3 87.29(7) . 7_656 ?
N7 Ni2 O3 89.47(7) . 7_656 ?
N7 Ni2 O3 90.53(7) 7_656 7_656 ?
O3 Ni2 O3 180.0 . 7_656 ?
C15 O1 Ni1 135.76(13) . . ?
C22 O3 Ni2 133.11(15) . . ?
C1 N1 C2 113.42(17) . . ?
C1 N1 Ni1 105.72(14) . . ?
C2 N1 Ni1 112.64(13) . . ?
C1 N1 H1 108.3 . . ?
C2 N1 H1 108.3 . . ?
Ni1 N1 H1 108.3 . . ?
C3 N2 C2 117.18(19) . . ?
C3 N2 C5 115.9(2) . . ?
C2 N2 C5 114.1(2) . . ?
C4 N3 C3 114.23(17) . . ?
C4 N3 Ni1 106.36(14) . . ?
C3 N3 Ni1 113.62(15) . . ?
C4 N3 H3 107.4 . . ?
C3 N3 H3 107.4 . . ?
Ni1 N3 H3 107.4 . . ?
C8 N5 C9 114.9(2) . . ?
C8 N5 Ni2 106.52(17) . . ?
C9 N5 Ni2 114.92(16) . . ?
C8 N5 H5 106.6 . . ?
C9 N5 H5 106.6 . . ?
Ni2 N5 H5 106.6 . . ?
C9 N6 C10 117.4(2) . . ?
C9 N6 C12 115.3(2) . . ?
C10 N6 C12 115.8(3) . . ?
C11 N7 C10 113.9(2) . . ?
C11 N7 Ni2 105.52(17) . . ?
C10 N7 Ni2 113.08(16) . . ?
C11 N7 H7 108.0 . . ?
C10 N7 H7 108.0 . . ?
Ni2 N7 H7 108.0 . . ?
N1 C1 C4 110.27(18) . 5_665 ?
N1 C1 H1A 109.6 . . ?
C4 C1 H1A 109.6 5_665 . ?
N1 C1 H1AB 109.6 . . ?
C4 C1 H1AB 109.6 5_665 . ?
H1A C1 H1AB 108.1 . . ?
N2 C2 N1 114.06(18) . . ?
N2 C2 H2A 108.7 . . ?
N1 C2 H2A 108.7 . . ?
N2 C2 H2AB 108.7 . . ?
N1 C2 H2AB 108.7 . . ?
H2A C2 H2AB 107.6 . . ?
N2 C3 N3 114.30(18) . . ?
N2 C3 H3A 108.7 . . ?
N3 C3 H3A 108.7 . . ?
N2 C3 H3AB 108.7 . . ?
N3 C3 H3AB 108.7 . . ?
H3A C3 H3AB 107.6 . . ?
N3 C4 C1 108.45(18) . 5_665 ?
N3 C4 H4A 110.0 . . ?
C1 C4 H4A 110.0 5_665 . ?
N3 C4 H4AB 110.0 . . ?
C1 C4 H4AB 110.0 5_665 . ?
H4A C4 H4AB 108.4 . . ?
N2 C5 C6 112.1(2) . . ?
N2 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N2 C5 H5AB 109.2 . . ?
C6 C5 H5AB 109.2 . . ?
H5A C5 H5AB 107.9 . . ?
C7 C6 C5 112.6(3) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N4 C7 C6 177.9(5) . . ?
N5 C8 C11 108.6(2) . 7_656 ?
N5 C8 H8A 110.0 . . ?
C11 C8 H8A 110.0 7_656 . ?
N5 C8 H8AB 110.0 . . ?
C11 C8 H8AB 110.0 7_656 . ?
H8A C8 H8AB 108.4 . . ?
N6 C9 N5 113.8(2) . . ?
N6 C9 H9A 108.8 . . ?
N5 C9 H9A 108.8 . . ?
N6 C9 H9AB 108.8 . . ?
N5 C9 H9AB 108.8 . . ?
H9A C9 H9AB 107.7 . . ?
N6 C10 N7 113.8(2) . . ?
N6 C10 H10A 108.8 . . ?
N7 C10 H10A 108.8 . . ?
N6 C10 H10B 108.8 . . ?
N7 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N7 C11 C8 108.9(2) . 7_656 ?
N7 C11 H11A 109.9 . . ?
C8 C11 H11A 109.9 7_656 . ?
N7 C11 H11B 109.9 . . ?
C8 C11 H11B 109.9 7_656 . ?
H11A C11 H11B 108.3 . . ?
C13 C12 N6 112.7(3) . . ?
C13 C12 H12A 109.1 . . ?
N6 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
N6 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C14 C13 C12 115.4(5) . . ?
C14 C13 H13A 108.4 . . ?
C12 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
N8 C14 C13 177.4(7) . . ?
O2 C15 O1 126.02(18) . . ?
O2 C15 C16 119.19(16) . . ?
O1 C15 C16 114.74(17) . . ?
C21 C16 C17 118.78(17) . . ?
C21 C16 C15 124.09(16) . . ?
C17 C16 C15 116.94(18) . . ?
C18 C17 C16 121.4(2) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C19 C18 C17 119.98(19) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 119.01(18) . . ?
C18 C19 C22 121.73(18) . . ?
C20 C19 C22 119.1(2) . . ?
C21 C20 C19 121.65(19) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C16 119.13(17) . . ?
C20 C21 C21 116.47(14) . 2_655 ?
C16 C21 C21 124.40(12) . 2_655 ?
O4 C22 O3 125.6(2) . . ?
O4 C22 C19 118.33(19) . . ?
O3 C22 C19 116.1(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
C2 N1 C1 C4 -164.32(17) . . . 5_665 ?
Ni1 N1 C1 C4 -40.42(19) . . . 5_665 ?
C3 N2 C2 N1 -71.6(2) . . . . ?
C5 N2 C2 N1 68.6(3) . . . . ?
C1 N1 C2 N2 178.69(18) . . . . ?
Ni1 N1 C2 N2 58.6(2) . . . . ?
C2 N2 C3 N3 68.9(3) . . . . ?
C5 N2 C3 N3 -70.6(3) . . . . ?
C4 N3 C3 N2 -176.87(19) . . . . ?
Ni1 N3 C3 N2 -54.6(2) . . . . ?
C3 N3 C4 C1 165.30(19) . . . 5_665 ?
Ni1 N3 C4 C1 39.15(19) . . . 5_665 ?
C3 N2 C5 C6 -80.3(3) . . . . ?
C2 N2 C5 C6 138.9(3) . . . . ?
N2 C5 C6 C7 -172.4(3) . . . . ?
C9 N5 C8 C11 -168.5(2) . . . 7_656 ?
Ni2 N5 C8 C11 -40.0(2) . . . 7_656 ?
C10 N6 C9 N5 -69.5(3) . . . . ?
C12 N6 C9 N5 72.5(3) . . . . ?
C8 N5 C9 N6 178.3(2) . . . . ?
Ni2 N5 C9 N6 54.2(3) . . . . ?
C9 N6 C10 N7 71.4(3) . . . . ?
C12 N6 C10 N7 -70.4(3) . . . . ?
C11 N7 C10 N6 -176.9(2) . . . . ?
Ni2 N7 C10 N6 -56.4(3) . . . . ?
C10 N7 C11 C8 167.0(2) . . . 7_656 ?
Ni2 N7 C11 C8 42.4(2) . . . 7_656 ?
C9 N6 C12 C13 129.5(4) . . . . ?
C10 N6 C12 C13 -87.9(4) . . . . ?
N6 C12 C13 C14 174.2(5) . . . . ?
Ni1 O1 C15 O2 26.5(3) . . . . ?
Ni1 O1 C15 C16 -150.74(15) . . . . ?
O2 C15 C16 C21 143.2(2) . . . . ?
O1 C15 C16 C21 -39.4(3) . . . . ?
O2 C15 C16 C17 -41.9(3) . . . . ?
O1 C15 C16 C17 135.6(2) . . . . ?
C21 C16 C17 C18 0.1(3) . . . . ?
C15 C16 C17 C18 -175.18(18) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C17 C18 C19 C20 0.0(3) . . . . ?
C17 C18 C19 C22 -175.93(19) . . . . ?
C18 C19 C20 C21 -0.7(3) . . . . ?
C22 C19 C20 C21 175.33(17) . . . . ?
C19 C20 C21 C16 1.1(3) . . . . ?
C19 C20 C21 C21 -178.96(18) . . . 2_655 ?
C17 C16 C21 C20 -0.8(3) . . . . ?
C15 C16 C21 C20 174.12(17) . . . . ?
C17 C16 C21 C21 179.29(19) . . . 2_655 ?
C15 C16 C21 C21 -5.8(3) . . . 2_655 ?
Ni2 O3 C22 O4 7.0(4) . . . . ?
Ni2 O3 C22 C19 -173.50(14) . . . . ?
C18 C19 C22 O4 -167.0(2) . . . . ?
C20 C19 C22 O4 17.1(3) . . . . ?
C18 C19 C22 O3 13.5(3) . . . . ?
C20 C19 C22 O3 -162.44(19) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O2 0.99 2.17 3.027(2) 143.6 . yes
N5 H5 O4 0.99 1.95 2.859(3) 152.0 . yes
N7 H7 N4 0.99 2.31 3.071(3) 133.3 5_666 yes

_refine_diff_density_max         0.670
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.056























####################################################################### 
# 
# 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_asflex_CH2_sq
_database_code_depnum_ccdc_archive 'CCDC 1908259'
loop_
_audit_author_name
_audit_author_address
'Sungeun Jeoung'
;Ulsan National Institute of Science and Technology (UNIST)
South Korea
;
_audit_update_record             
;
2019-05-17 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        as-flexMOF(CH2)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H66 N12 Ni2 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H72 N14 Ni2 O8'
_chemical_formula_weight         1090.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0019 0.0011 '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 0.0040 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0074 0.0043 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3348 0.8487 '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                   12.920(3)
_cell_length_b                   32.634(7)
_cell_length_c                   15.617(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.16(3)
_cell_angle_gamma                90
_cell_volume                     6355(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    92121
_cell_measurement_theta_min      0.350
_cell_measurement_theta_max      33.679

_exptl_crystal_description       block
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_F_000             2312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.105
_exptl_absorpt_coefficient_mu    0.428
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.956
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.610
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31733
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.500
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        21.469
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             8742
_reflns_number_gt                6808
_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       
'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2015b)'
_computing_molecular_graphics    'DIAMOND 4(Putz&Brandenburg, 2014)'
_computing_publication_material  'publCIF(Westrip, 2010)'
_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)+(0.1896P)²+1.3860P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0024(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8742
_refine_ls_number_parameters     321
_refine_ls_number_restraints     296
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2778
_refine_ls_wR_factor_gt          0.2657
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.145
_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 0.750000 0.750000 0.500000 0.05298(19) Uani 1 2 d S U P . .
N1 N 0.82988(19) 0.77184(7) 0.41097(16) 0.0632(5) Uani 1 1 d . U . . .
H1 H 0.841144 0.748775 0.373214 0.076 Uiso 1 1 calc R U . . .
N2 N 1.0095(2) 0.76256(10) 0.5150(2) 0.0711(6) Uani 1 1 d . U . . .
N3 N 0.88630(18) 0.72588(6) 0.58423(15) 0.0585(5) Uani 1 1 d . U . . .
H3 H 0.901388 0.699482 0.558663 0.070 Uiso 1 1 calc R U . . .
C1 C 0.7543(3) 0.80126(11) 0.3547(2) 0.0732(8) Uani 1 1 d . U . . .
H1A H 0.775740 0.806627 0.300036 0.088 Uiso 1 1 calc R U . . .
H1B H 0.755643 0.827258 0.386408 0.088 Uiso 1 1 calc R U . . .
C2 C 0.9370(2) 0.79040(10) 0.4547(2) 0.0715(7) Uani 1 1 d . U . . .
H2A H 0.971013 0.799288 0.408618 0.086 Uiso 1 1 calc R U . . .
H2B H 0.925853 0.814777 0.487842 0.086 Uiso 1 1 calc R U . . .
C3 C 0.9828(2) 0.75200(8) 0.5956(2) 0.0642(7) Uani 1 1 d . U . . .
H3A H 0.971565 0.777340 0.625661 0.077 Uiso 1 1 calc R U . . .
H3B H 1.043993 0.737716 0.634496 0.077 Uiso 1 1 calc R U . . .
C4 C 0.8582(2) 0.71673(10) 0.6676(2) 0.0686(7) Uani 1 1 d . U . . .
H4A H 0.860704 0.741857 0.702486 0.082 Uiso 1 1 calc R U . . .
H4B H 0.909436 0.697123 0.702841 0.082 Uiso 1 1 calc R U . . .
C5 C 1.0519(3) 0.72913(14) 0.4701(3) 0.0841(9) Uani 1 1 d . U . . .
H5A H 1.070625 0.740200 0.417738 0.101 Uiso 1 1 calc R U . . .
H5B H 0.995753 0.708484 0.449716 0.101 Uiso 1 1 calc R U . . .
C6 C 1.1475(4) 0.70930(18) 0.5285(4) 0.1067(14) Uani 1 1 d . U . . .
H6 H 1.205640 0.726583 0.553842 0.128 Uiso 1 1 calc R U . . .
C7 C 1.1599(6) 0.6713(2) 0.5484(5) 0.142(2) Uani 1 1 d . U . . .
H7A H 1.104326 0.652661 0.524887 0.170 Uiso 1 1 calc R U . . .
H7B H 1.224568 0.662078 0.586442 0.170 Uiso 1 1 calc R U . . .
Ni2 Ni 0.500000 0.500000 0.000000 0.0611(2) Uani 1 2 d S U P . .
N4 N 0.5795(4) 0.44892(10) 0.0569(2) 0.1029(11) Uani 1 1 d . U . . .
H4 H 0.599900 0.452954 0.121993 0.123 Uiso 1 1 calc R U . . .
N5 N 0.4419(5) 0.41253(15) 0.0706(3) 0.1392(17) Uani 1 1 d D U . . .
N6 N 0.3609(4) 0.48017(12) 0.0258(4) 0.1292(17) Uani 1 1 d . U . . .
H6A H 0.378714 0.489471 0.088262 0.155 Uiso 1 1 calc R U . . .
C8 C 0.6923(6) 0.4499(2) 0.0223(5) 0.145(2) Uani 1 1 d . U . . .
H8A H 0.751005 0.437420 0.067606 0.174 Uiso 1 1 calc R U . . .
H8B H 0.681648 0.433677 -0.032178 0.174 Uiso 1 1 calc R U . . .
C9 C 0.5340(7) 0.41094(16) 0.0397(4) 0.1377(19) Uani 1 1 d . U . . .
H9A H 0.583153 0.389686 0.070919 0.165 Uiso 1 1 calc R U . . .
H9B H 0.515448 0.405105 -0.024080 0.165 Uiso 1 1 calc R U . . .
C10 C 0.3553(6) 0.4390(2) 0.0438(7) 0.162(3) Uani 1 1 d . U . . .
H10A H 0.308484 0.426885 -0.009835 0.195 Uiso 1 1 calc R U . . .
H10B H 0.316068 0.437248 0.089627 0.195 Uiso 1 1 calc R U . . .
C11 C 0.2783(5) 0.5071(2) -0.0050(6) 0.141(2) Uani 1 1 d . U . . .
H11A H 0.235289 0.508127 0.038118 0.169 Uiso 1 1 calc R U . . .
H11B H 0.232408 0.496098 -0.060364 0.169 Uiso 1 1 calc R U . . .
C12 C 0.456182 0.409643 0.168292 0.181(3) Uani 1 1 d D U . A -1
H12A H 0.390755 0.419464 0.182164 0.217 Uiso 1 1 d . U . B -1
H12B H 0.515425 0.427608 0.198236 0.217 Uiso 1 1 d . U . C -1
C13 C 0.481050 0.363379 0.204247 0.225(5) Uani 1 1 d D U . A -1
H13 H 0.548985 0.353189 0.203900 0.270 Uiso 1 1 d . U . D -1
C14 C 0.420032 0.338156 0.233747 0.440(17) Uani 1 1 d D U . A -1
H14A H 0.351027 0.346350 0.235940 0.528 Uiso 1 1 d . U . E -1
H14B H 0.445065 0.311790 0.252809 0.528 Uiso 1 1 d . U . F -1
O1 O 0.71226(15) 0.69485(5) 0.42439(14) 0.0623(5) Uani 1 1 d . U . . .
O2 O 0.8617(2) 0.65829(8) 0.4673(2) 0.0994(10) Uani 1 1 d . U . . .
O3 O 0.5284(2) 0.53331(6) 0.12039(13) 0.0799(7) Uani 1 1 d . U . . .
O4 O 0.6234(4) 0.49146(8) 0.22527(19) 0.1357(17) Uani 1 1 d . U . . .
C15 C 0.7679(2) 0.66364(8) 0.4225(2) 0.0621(6) Uani 1 1 d . U . . .
C16 C 0.7166(2) 0.62908(7) 0.36114(16) 0.0544(5) Uani 1 1 d . U . . .
C17 C 0.7810(2) 0.59690(9) 0.3468(2) 0.0679(7) Uani 1 1 d . U . . .
H17 H 0.855282 0.597357 0.373162 0.081 Uiso 1 1 calc R U . . .
C18 C 0.7355(3) 0.56444(9) 0.2940(2) 0.0726(8) Uani 1 1 d . U . . .
H18 H 0.779628 0.543111 0.283795 0.087 Uiso 1 1 calc R U . . .
C19 C 0.6261(3) 0.56248(8) 0.25567(17) 0.0647(7) Uani 1 1 d . U . . .
C20 C 0.5587(2) 0.59430(6) 0.26888(14) 0.0524(5) Uani 1 1 d . U . . .
C21 C 0.60675(19) 0.62743(6) 0.32246(14) 0.0488(5) Uani 1 1 d . U . . .
H21 H 0.563272 0.649071 0.332384 0.059 Uiso 1 1 calc R U . . .
C22 C 0.5869(4) 0.52561(9) 0.1965(2) 0.0851(11) Uani 1 1 d . U . . .
N1S N 0.8067(7) 0.71847(19) 0.2295(4) 0.154(2) Uani 1 1 d . U . . .
C1S C 0.7559(5) 0.69340(18) 0.1840(4) 0.1071(13) Uani 1 1 d . U . . .
C2S C 0.6927(5) 0.66130(17) 0.1253(4) 0.1091(14) Uani 1 1 d . U . . .
H2S1 H 0.624727 0.672728 0.092035 0.164 Uiso 1 1 calc R U . . .
H2S2 H 0.679626 0.638561 0.161085 0.164 Uiso 1 1 calc R U . . .
H2S3 H 0.732437 0.651677 0.084431 0.164 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 N3 2.059(2) . ?
Ni1 N3 2.059(2) 7_666 ?
Ni1 N1 2.063(3) . ?
Ni1 N1 2.063(3) 7_666 ?
Ni1 O1 2.1376(17) . ?
Ni1 O1 2.1376(17) 7_666 ?
N1 C1 1.483(4) . ?
N1 C2 1.501(4) . ?
N1 H1 0.9900 . ?
N2 C3 1.432(5) . ?
N2 C2 1.459(4) . ?
N2 C5 1.478(5) . ?
N3 C4 1.472(4) . ?
N3 C3 1.482(4) . ?
N3 H3 0.9900 . ?
C1 C4 1.521(4) 7_666 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.479(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.277(8) . ?
C6 H6 0.9400 . ?
C7 H7A 0.9400 . ?
C7 H7B 0.9400 . ?
Ni2 N4 2.036(3) 5_665 ?
Ni2 N4 2.036(3) . ?
Ni2 N6 2.046(5) . ?
Ni2 N6 2.046(5) 5_665 ?
Ni2 O3 2.1190(19) 5_665 ?
Ni2 O3 2.1191(19) . ?
N4 C9 1.368(7) . ?
N4 C8 1.681(9) . ?
N4 H4 0.9900 . ?
N5 C10 1.390(9) . ?
N5 C9 1.397(10) . ?
N5 C12 1.492(5) . ?
N6 C11 1.370(8) . ?
N6 C10 1.378(7) . ?
N6 H6A 0.9900 . ?
C8 C11 1.497(10) 5_665 ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.6136(3) . ?
C12 H12A 0.97980(18) . ?
C12 H12B 0.9803(2) . ?
C13 C14 1.3043(2) . ?
C13 H13 0.93995(16) . ?
C14 H14A 0.93994(17) . ?
C14 H14B 0.93976(16) . ?
O1 C15 1.251(3) . ?
O2 C15 1.243(4) . ?
O3 C22 1.255(4) . ?
O4 C22 1.247(4) . ?
C15 C16 1.515(3) . ?
C16 C21 1.391(3) . ?
C16 C17 1.394(4) . ?
C17 C18 1.376(4) . ?
C17 H17 0.9400 . ?
C18 C19 1.384(5) . ?
C18 H18 0.9400 . ?
C19 C20 1.405(4) . ?
C19 C22 1.521(4) . ?
C20 C21 1.408(3) . ?
C20 C20 1.477(5) 2_655 ?
C21 H21 0.9400 . ?
N1S C1S 1.166(8) . ?
C1S C2S 1.488(8) . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
C2S H2S3 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
N3 Ni1 N3 180.0 . 7_666 ?
N3 Ni1 N1 93.88(10) . . ?
N3 Ni1 N1 86.12(10) 7_666 . ?
N3 Ni1 N1 86.13(10) . 7_666 ?
N3 Ni1 N1 93.87(10) 7_666 7_666 ?
N1 Ni1 N1 180.00(10) . 7_666 ?
N3 Ni1 O1 93.69(8) . . ?
N3 Ni1 O1 86.31(8) 7_666 . ?
N1 Ni1 O1 90.03(9) . . ?
N1 Ni1 O1 89.97(9) 7_666 . ?
N3 Ni1 O1 86.31(8) . 7_666 ?
N3 Ni1 O1 93.69(8) 7_666 7_666 ?
N1 Ni1 O1 89.97(9) . 7_666 ?
N1 Ni1 O1 90.03(9) 7_666 7_666 ?
O1 Ni1 O1 180.0 . 7_666 ?
C1 N1 C2 113.2(2) . . ?
C1 N1 Ni1 104.8(2) . . ?
C2 N1 Ni1 113.39(19) . . ?
C1 N1 H1 108.4 . . ?
C2 N1 H1 108.4 . . ?
Ni1 N1 H1 108.4 . . ?
C3 N2 C2 117.1(3) . . ?
C3 N2 C5 116.4(3) . . ?
C2 N2 C5 114.1(3) . . ?
C4 N3 C3 113.9(2) . . ?
C4 N3 Ni1 105.96(18) . . ?
C3 N3 Ni1 114.12(17) . . ?
C4 N3 H3 107.5 . . ?
C3 N3 H3 107.5 . . ?
Ni1 N3 H3 107.5 . . ?
N1 C1 C4 109.1(3) . 7_666 ?
N1 C1 H1A 109.9 . . ?
C4 C1 H1A 109.9 7_666 . ?
N1 C1 H1B 109.9 . . ?
C4 C1 H1B 109.9 7_666 . ?
H1A C1 H1B 108.3 . . ?
N2 C2 N1 113.7(3) . . ?
N2 C2 H2A 108.8 . . ?
N1 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
N1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N2 C3 N3 114.9(2) . . ?
N2 C3 H3A 108.5 . . ?
N3 C3 H3A 108.5 . . ?
N2 C3 H3B 108.5 . . ?
N3 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
N3 C4 C1 108.5(2) . 7_666 ?
N3 C4 H4A 110.0 . . ?
C1 C4 H4A 110.0 7_666 . ?
N3 C4 H4B 110.0 . . ?
C1 C4 H4B 110.0 7_666 . ?
H4A C4 H4B 108.4 . . ?
N2 C5 C6 112.5(4) . . ?
N2 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 C5 127.3(6) . . ?
C7 C6 H6 116.4 . . ?
C5 C6 H6 116.4 . . ?
C6 C7 H7A 120.0 . . ?
C6 C7 H7B 120.0 . . ?
H7A C7 H7B 120.0 . . ?
N4 Ni2 N4 180.0 5_665 . ?
N4 Ni2 N6 88.6(2) 5_665 . ?
N4 Ni2 N6 91.4(2) . . ?
N4 Ni2 N6 91.4(2) 5_665 5_665 ?
N4 Ni2 N6 88.6(2) . 5_665 ?
N6 Ni2 N6 180.0 . 5_665 ?
N4 Ni2 O3 94.71(11) 5_665 5_665 ?
N4 Ni2 O3 85.29(11) . 5_665 ?
N6 Ni2 O3 93.15(17) . 5_665 ?
N6 Ni2 O3 86.85(17) 5_665 5_665 ?
N4 Ni2 O3 85.28(11) 5_665 . ?
N4 Ni2 O3 94.72(11) . . ?
N6 Ni2 O3 86.85(17) . . ?
N6 Ni2 O3 93.15(17) 5_665 . ?
O3 Ni2 O3 180.00(14) 5_665 . ?
C9 N4 C8 108.5(4) . . ?
C9 N4 Ni2 120.9(4) . . ?
C8 N4 Ni2 103.0(3) . . ?
C9 N4 H4 107.9 . . ?
C8 N4 H4 107.9 . . ?
Ni2 N4 H4 107.9 . . ?
C10 N5 C9 127.7(6) . . ?
C10 N5 C12 102.8(5) . . ?
C9 N5 C12 117.5(5) . . ?
C11 N6 C10 128.3(6) . . ?
C11 N6 Ni2 111.8(5) . . ?
C10 N6 Ni2 116.4(4) . . ?
C11 N6 H6A 96.2 . . ?
C10 N6 H6A 96.2 . . ?
Ni2 N6 H6A 96.2 . . ?
C11 C8 N4 110.9(4) 5_665 . ?
C11 C8 H8A 109.5 5_665 . ?
N4 C8 H8A 109.5 . . ?
C11 C8 H8B 109.5 5_665 . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 108.0 . . ?
N4 C9 N5 105.1(4) . . ?
N4 C9 H9A 110.7 . . ?
N5 C9 H9A 110.7 . . ?
N4 C9 H9B 110.7 . . ?
N5 C9 H9B 110.7 . . ?
H9A C9 H9B 108.8 . . ?
N6 C10 N5 125.9(6) . . ?
N6 C10 H10A 105.8 . . ?
N5 C10 H10A 105.8 . . ?
N6 C10 H10B 105.8 . . ?
N5 C10 H10B 105.8 . . ?
H10A C10 H10B 106.2 . . ?
N6 C11 C8 117.0(6) . 5_665 ?
N6 C11 H11A 108.0 . . ?
C8 C11 H11A 108.0 5_665 . ?
N6 C11 H11B 108.0 . . ?
C8 C11 H11B 108.0 5_665 . ?
H11A C11 H11B 107.3 . . ?
N5 C12 C13 112.04(19) . . ?
N5 C12 H12A 108.8(2) . . ?
C13 C12 H12A 109.506(11) . . ?
N5 C12 H12B 108.8(2) . . ?
C13 C12 H12B 109.511(19) . . ?
H12A C12 H12B 108.062(14) . . ?
C14 C13 C12 129.026(9) . . ?
C14 C13 H13 115.489(14) . . ?
C12 C13 H13 115.485(10) . . ?
C13 C14 H14A 120.000(14) . . ?
C13 C14 H14B 119.997(11) . . ?
H14A C14 H14B 120.003(9) . . ?
C15 O1 Ni1 130.48(16) . . ?
C22 O3 Ni2 131.20(19) . . ?
O2 C15 O1 125.6(2) . . ?
O2 C15 C16 116.8(2) . . ?
O1 C15 C16 117.6(2) . . ?
C21 C16 C17 119.0(2) . . ?
C21 C16 C15 122.1(2) . . ?
C17 C16 C15 118.8(2) . . ?
C18 C17 C16 119.8(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 121.5(3) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C20 120.3(2) . . ?
C18 C19 C22 116.1(3) . . ?
C20 C19 C22 123.6(3) . . ?
C19 C20 C21 117.5(2) . . ?
C19 C20 C20 123.57(17) . 2_655 ?
C21 C20 C20 118.96(19) . 2_655 ?
C16 C21 C20 121.9(2) . . ?
C16 C21 H21 119.0 . . ?
C20 C21 H21 119.0 . . ?
O4 C22 O3 126.7(3) . . ?
O4 C22 C19 116.9(3) . . ?
O3 C22 C19 116.0(2) . . ?
N1S C1S C2S 179.0(6) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
C2 N1 C1 C4 -166.1(3) . . . 7_666 ?
Ni1 N1 C1 C4 -42.0(3) . . . 7_666 ?
C3 N2 C2 N1 -69.4(4) . . . . ?
C5 N2 C2 N1 71.4(4) . . . . ?
C1 N1 C2 N2 176.0(3) . . . . ?
Ni1 N1 C2 N2 56.8(3) . . . . ?
C2 N2 C3 N3 69.0(3) . . . . ?
C5 N2 C3 N3 -71.0(3) . . . . ?
C4 N3 C3 N2 -177.8(3) . . . . ?
Ni1 N3 C3 N2 -56.0(3) . . . . ?
C3 N3 C4 C1 166.8(2) . . . 7_666 ?
Ni1 N3 C4 C1 40.6(3) . . . 7_666 ?
C3 N2 C5 C6 -55.9(5) . . . . ?
C2 N2 C5 C6 162.9(4) . . . . ?
N2 C5 C6 C7 123.6(6) . . . . ?
C9 N4 C8 C11 157.3(6) . . . 5_665 ?
Ni2 N4 C8 C11 27.9(6) . . . 5_665 ?
C8 N4 C9 N5 179.6(4) . . . . ?
Ni2 N4 C9 N5 -61.8(6) . . . . ?
C10 N5 C9 N4 59.1(8) . . . . ?
C12 N5 C9 N4 -76.8(5) . . . . ?
C11 N6 C10 N5 176.3(9) . . . . ?
Ni2 N6 C10 N5 19.3(12) . . . . ?
C9 N5 C10 N6 -40.3(13) . . . . ?
C12 N5 C10 N6 100.4(9) . . . . ?
C10 N6 C11 C8 -177.7(8) . . . 5_665 ?
Ni2 N6 C11 C8 -19.8(9) . . . 5_665 ?
C10 N5 C12 C13 138.4(4) . . . . ?
C9 N5 C12 C13 -76.0(5) . . . . ?
N5 C12 C13 C14 -109.5(3) . . . . ?
Ni1 O1 C15 O2 0.3(5) . . . . ?
Ni1 O1 C15 C16 179.60(18) . . . . ?
O2 C15 C16 C21 165.9(3) . . . . ?
O1 C15 C16 C21 -13.5(4) . . . . ?
O2 C15 C16 C17 -10.7(5) . . . . ?
O1 C15 C16 C17 169.9(3) . . . . ?
C21 C16 C17 C18 0.9(5) . . . . ?
C15 C16 C17 C18 177.6(3) . . . . ?
C16 C17 C18 C19 -1.2(5) . . . . ?
C17 C18 C19 C20 1.0(5) . . . . ?
C17 C18 C19 C22 178.1(3) . . . . ?
C18 C19 C20 C21 -0.5(4) . . . . ?
C22 C19 C20 C21 -177.3(3) . . . . ?
C18 C19 C20 C20 -179.3(3) . . . 2_655 ?
C22 C19 C20 C20 3.8(5) . . . 2_655 ?
C17 C16 C21 C20 -0.4(4) . . . . ?
C15 C16 C21 C20 -176.9(2) . . . . ?
C19 C20 C21 C16 0.1(4) . . . . ?
C20 C20 C21 C16 179.0(2) 2_655 . . . ?
Ni2 O3 C22 O4 -19.0(8) . . . . ?
Ni2 O3 C22 C19 154.2(3) . . . . ?
C18 C19 C22 O4 45.5(6) . . . . ?
C20 C19 C22 O4 -137.5(4) . . . . ?
C18 C19 C22 O3 -128.4(4) . . . . ?
C20 C19 C22 O3 48.6(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 N1S 0.99 2.39 3.272(6) 148.8 . yes
N3 H3 O2 0.99 1.93 2.828(3) 149.5 . yes
N4 H4 O4 0.99 2.00 2.895(4) 148.6 . yes
N6 H6A O3 0.99 2.35 2.864(5) 111.3 . yes

_refine_diff_density_max         1.270
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.095



# start Validation Reply Form
_vrf_PLAT410_asflex_CH2_sq       
;
PROBLEM: Short Intra H...H Contact H10B ..H12A . 1.62 Ang.
x,y,z = 1_555
Short Intra H...H Contact H12B ..H12B . 1.76 Ang.
1-x,y,1/2-z = 2_655 Check
RESPONSE: When we examine closely the crystal structure, we can see that the adjacent
-CH=CH2 arm parts are pi-pi interaction by packing. However, crystallographically, the
reason why occurs Alert A is very close distance of hydrogen atoms.
;
_vrf_PLAT412_asflex_CH2_sq       
;
PROBLEM: Short Intra XH3 .. XHn H13 ..H14A . 1.40 Ang.
1-x,y,1/2-z = 2_655 Check
Short Intra XH3 .. XHn H13 ..H14B . 1.50 Ang.
1-x,y,1/2-z = 2_655 Check
Short Intra XH3 .. XHn H14B ..H14B . 1.44 Ang.
1-x,y,1/2-z = 2_655 Check
RESPONSE: When we examine closely the crystal structure, we can see that the adjacent
-CH=CH2 arm parts are pi-pi interaction by packing. However, crystallographically, the
reason why occurs Alert A is very close distance of hydrogen atoms.
;
# end Validation Reply Form




















