#------------------------------------------------------------------------------
#$Date: 2018-09-01 16:06:14 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210299 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309386.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4309386
loop_
_publ_author_name
'Ghosh, Sujit K.'
'Bharadwaj, Parimal K.'
_publ_section_title
;
 Metal--Organic Framework H-Bonded Like a Polycatenane: Coexistence of
 Acyclic Water Trimer and Nonamer
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   16
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5553
_journal_page_last               5555
_journal_paper_doi               10.1021/ic050727u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C78 H84 N12 Ni3 O39'
_chemical_formula_sum            'C26 H28 N4 Ni O13'
_chemical_formula_weight         663.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 104.832(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            12
_cell_length_a                   24.730(5)
_cell_length_b                   19.895(2)
_cell_length_c                   17.257(4)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.04
_cell_volume                     8208(3)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54336
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        <0.05
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.8843
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flake type'
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         20256
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0659P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                15698
_reflns_number_total             20256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050727usi20050509_123607.cif
_cod_data_source_block           {(3dpeH2)_[Ni(pdc)2]3.15H2O}1
_cod_depositor_comments
;
The following automatic conversions were performed:
_cell_measurement_temperature value '100K' changed to '100' - value
should be numeric, i.e.'FLOAT or 'INT' without temperature
units.
_diffrn_ambient_temperature value '100K' changed to '100' -
value should be numeric, i.e.'FLOAT or 'INT' without temperature
units.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_original_cell_volume        8208(4)
_cod_database_code               4309386
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.932034(8) 0.118329(11) 1.129642(12) 0.00938(6) Uani 1 1 d . . .
Ni2 Ni 0.595872(8) 0.111914(11) 0.802395(12) 0.00996(6) Uani 1 1 d . . .
Ni3 Ni 0.736258(8) -0.108295(11) 0.546355(12) 0.00932(6) Uani 1 1 d . . .
O1 O 0.80317(5) 0.25481(6) 1.11018(7) 0.0160(3) Uani 1 1 d . . .
O2 O 0.87518(5) 0.19847(6) 1.08338(7) 0.0128(2) Uani 1 1 d . . .
O3 O 0.96000(5) -0.00738(6) 1.32632(7) 0.0159(3) Uani 1 1 d . . .
O4 O 0.96839(5) 0.04064(6) 1.21185(7) 0.0128(2) Uani 1 1 d . . .
O5 O 0.99476(5) 0.18917(6) 1.18202(7) 0.0135(2) Uani 1 1 d . . .
O6 O 1.07306(5) 0.23575(6) 1.16167(7) 0.0189(3) Uani 1 1 d . . .
O7 O 0.88939(4) 0.04649(6) 1.04255(7) 0.0127(2) Uani 1 1 d . . .
O8 O 0.89529(5) -0.00199(6) 0.92754(7) 0.0140(2) Uani 1 1 d . . .
O9 O 0.47178(5) 0.25289(6) 0.77984(7) 0.0206(3) Uani 1 1 d . . .
O10 O 0.53777(5) 0.18789(6) 0.75062(7) 0.0149(3) Uani 1 1 d . . .
O11 O 0.62565(5) -0.00871(6) 1.00305(7) 0.0159(3) Uani 1 1 d . . .
O12 O 0.63278(5) 0.03653(6) 0.88675(7) 0.0131(2) Uani 1 1 d . . .
O13 O 0.65538(5) 0.18634(6) 0.85173(7) 0.0143(2) Uani 1 1 d . . .
O14 O 0.72469(5) 0.24584(6) 0.82266(7) 0.0197(3) Uani 1 1 d . . .
O15 O 0.55644(5) 0.03432(6) 0.71828(7) 0.0130(2) Uani 1 1 d . . .
O16 O 0.56102(5) -0.01029(6) 0.60045(7) 0.0134(2) Uani 1 1 d . . .
O17 O 0.77967(5) -0.03756(6) 0.63455(7) 0.0128(2) Uani 1 1 d . . .
O18 O 0.77457(5) 0.01001(6) 0.75037(7) 0.0140(2) Uani 1 1 d . . .
O19 O 0.59283(5) -0.21916(6) 0.50916(7) 0.0167(3) Uani 1 1 d . . .
O20 O 0.67378(5) -0.17757(6) 0.49324(7) 0.0129(2) Uani 1 1 d . . .
O21 O 0.69931(5) -0.03023(6) 0.46442(7) 0.0134(2) Uani 1 1 d . . .
O22 O 0.70659(5) 0.01678(6) 0.34873(7) 0.0174(3) Uani 1 1 d . . .
O23 O 0.79195(5) -0.18968(6) 0.59125(7) 0.0121(2) Uani 1 1 d . . .
O24 O 0.86092(5) -0.24950(6) 0.56086(7) 0.0151(3) Uani 1 1 d . . .
OW1 O 0.57732(6) -0.29832(7) 0.37642(9) 0.0234(3) Uani 1 1 d D . .
OW2 O 0.66582(6) -0.36920(8) 0.47158(10) 0.0271(3) Uani 1 1 d D . .
OW3 O 0.73236(6) -0.31151(8) 0.60107(9) 0.0223(3) Uani 1 1 d D . .
OW4 O 0.80614(7) -0.41105(7) 0.65296(9) 0.0247(3) Uani 1 1 d D . .
OW5 O 0.89544(6) -0.31527(7) 0.70525(8) 0.0184(3) Uani 1 1 d D . .
OW6 O 1.00031(6) 0.12759(8) 1.70629(10) 0.0290(3) Uani 1 1 d D . .
OW7 O 0.93449(7) 0.18132(8) 1.57247(9) 0.0254(3) Uani 1 1 d D . .
OW8 O 0.85757(7) 0.08604(7) 1.51235(9) 0.0275(3) Uani 1 1 d D . .
OW9 O 0.76863(6) 0.17884(7) 0.46721(8) 0.0225(3) Uani 1 1 d D . .
OW10 O 0.65190(6) 0.13720(8) 0.31832(9) 0.0240(3) Uani 1 1 d D . .
OW11 O 0.55388(6) 0.16192(8) 0.20702(8) 0.0269(3) Uani 1 1 d D . .
OW12 O 0.50563(6) -0.45438(7) 0.32399(8) 0.0233(3) Uani 1 1 d D . .
OW13 O 1.08316(5) 0.02709(8) 1.22087(8) 0.0215(3) Uani 1 1 d D . .
OW14 O 0.74885(6) 0.03926(8) 0.89352(8) 0.0233(3) Uani 1 1 d D . .
OW15 O 0.58225(5) -0.03052(7) 0.45002(8) 0.0194(3) Uani 1 1 d D . .
N1 N 0.88488(6) 0.12034(7) 1.20559(8) 0.0095(3) Uani 1 1 d . . .
N2 N 0.97802(5) 0.11811(7) 1.05234(8) 0.0095(3) Uani 1 1 d . . .
N3 N 0.55032(6) 0.11748(7) 0.88005(8) 0.0101(3) Uani 1 1 d . . .
N4 N 0.64129(5) 0.11258(7) 0.72450(8) 0.0094(3) Uani 1 1 d . . .
N5 N 0.69124(5) -0.10912(7) 0.62483(8) 0.0096(3) Uani 1 1 d . . .
N6 N 0.78130(5) -0.11224(7) 0.46800(8) 0.0095(3) Uani 1 1 d . . .
N7 N 0.84560(6) 0.38633(7) 1.28824(9) 0.0149(3) Uani 1 1 d . . .
H7 H 0.8255 0.4206 1.2685 0.018 Uiso 1 1 calc R . .
N8 N 1.09006(6) 0.03167(7) 1.45798(8) 0.0133(3) Uani 1 1 d . . .
H8 H 1.1099 -0.0033 1.4753 0.016 Uiso 1 1 calc R . .
N9 N 0.51683(6) 0.39092(7) 0.95383(9) 0.0142(3) Uani 1 1 d . . .
H9 H 0.4965 0.4244 0.9322 0.017 Uiso 1 1 calc R . .
N10 N 0.75427(6) 0.03081(7) 1.12962(8) 0.0135(3) Uani 1 1 d . . .
H10 H 0.7735 -0.0046 1.1471 0.016 Uiso 1 1 calc R . .
N11 N 0.57686(6) -0.04479(7) 0.21157(8) 0.0140(3) Uani 1 1 d . . .
H11 H 0.5546 -0.0124 0.1915 0.017 Uiso 1 1 calc R . .
N12 N 0.82371(6) -0.39533(7) 0.38835(9) 0.0147(3) Uani 1 1 d . . .
H12 H 0.8429 -0.4303 0.4078 0.018 Uiso 1 1 calc R . .
C1 C 0.83963(7) 0.21062(8) 1.12389(9) 0.0112(3) Uani 1 1 d . . .
C2 C 0.84385(6) 0.16563(8) 1.19615(9) 0.0106(3) Uani 1 1 d . . .
C3 C 0.81068(7) 0.16930(8) 1.24947(9) 0.0118(3) Uani 1 1 d . . .
H3 H 0.7823 0.2011 1.2428 0.014 Uiso 1 1 calc R . .
C4 C 0.82082(7) 0.12422(9) 1.31350(10) 0.0148(3) Uani 1 1 d . . .
H4 H 0.7988 0.1252 1.3498 0.018 Uiso 1 1 calc R . .
C5 C 0.86410(7) 0.07786(9) 1.32266(10) 0.0139(3) Uani 1 1 d . . .
H5 H 0.8716 0.0477 1.3653 0.017 Uiso 1 1 calc R . .
C6 C 0.89579(6) 0.07739(8) 1.26710(9) 0.0108(3) Uani 1 1 d . . .
C7 C 0.94558(7) 0.03232(8) 1.26906(10) 0.0117(3) Uani 1 1 d . . .
C8 C 0.91161(6) 0.03710(8) 0.98543(9) 0.0109(3) Uani 1 1 d . . .
C9 C 0.96360(6) 0.07897(8) 0.98751(9) 0.0105(3) Uani 1 1 d . . .
C10 C 0.99416(7) 0.07998(9) 0.93039(10) 0.0133(3) Uani 1 1 d . . .
H10 H 0.9846 0.0520 0.8858 0.016 Uiso 1 1 calc R . .
C11 C 1.03928(7) 0.12357(9) 0.94128(10) 0.0142(3) Uani 1 1 d . . .
H11 H 1.0600 0.1255 0.9033 0.017 Uiso 1 1 calc R . .
C12 C 1.05355(7) 0.16452(8) 1.00915(10) 0.0127(3) Uani 1 1 d . . .
H12 H 1.0835 0.1942 1.0170 0.015 Uiso 1 1 calc R . .
C13 C 1.02185(6) 0.15978(8) 1.06439(10) 0.0108(3) Uani 1 1 d . . .
C14 C 1.03103(7) 0.19884(8) 1.14259(10) 0.0130(3) Uani 1 1 d . . .
C15 C 0.50572(7) 0.20592(8) 0.79403(10) 0.0125(3) Uani 1 1 d . . .
C16 C 0.51087(7) 0.16499(8) 0.87011(10) 0.0115(3) Uani 1 1 d . . .
C17 C 0.48028(7) 0.17374(9) 0.92628(10) 0.0137(3) Uani 1 1 d . . .
H17 H 0.4534 0.2074 0.9200 0.016 Uiso 1 1 calc R . .
C18 C 0.49080(7) 0.13085(9) 0.99251(10) 0.0160(4) Uani 1 1 d . . .
H18 H 0.4702 0.1349 1.0304 0.019 Uiso 1 1 calc R . .
C19 C 0.53214(7) 0.08206(9) 1.00159(10) 0.0138(3) Uani 1 1 d . . .
H19 H 0.5397 0.0534 1.0456 0.017 Uiso 1 1 calc R . .
C20 C 0.56184(7) 0.07705(8) 0.94367(10) 0.0115(3) Uani 1 1 d . . .
C21 C 0.61076(6) 0.03024(8) 0.94534(10) 0.0119(3) Uani 1 1 d . . .
C22 C 0.68899(7) 0.20011(8) 0.80940(10) 0.0131(3) Uani 1 1 d . . .
C23 C 0.68294(7) 0.15725(8) 0.73453(10) 0.0115(3) Uani 1 1 d . . .
C24 C 0.71448(7) 0.16260(8) 0.67922(10) 0.0125(3) Uani 1 1 d . . .
H24 H 0.7431 0.1941 0.6859 0.015 Uiso 1 1 calc R . .
C25 C 0.70240(7) 0.11970(8) 0.61319(10) 0.0136(3) Uani 1 1 d . . .
H25 H 0.7234 0.1218 0.5756 0.016 Uiso 1 1 calc R . .
C26 C 0.65889(7) 0.07390(8) 0.60368(10) 0.0120(3) Uani 1 1 d . . .
H26 H 0.6504 0.0450 0.5599 0.014 Uiso 1 1 calc R . .
C27 C 0.62821(6) 0.07210(8) 0.66084(9) 0.0099(3) Uani 1 1 d . . .
C28 C 0.57775(6) 0.02774(8) 0.65910(9) 0.0108(3) Uani 1 1 d . . .
C29 C 0.75807(6) -0.02934(8) 0.69233(10) 0.0110(3) Uani 1 1 d . . .
C30 C 0.70692(6) -0.07225(8) 0.69150(10) 0.0105(3) Uani 1 1 d . . .
C31 C 0.67814(7) -0.07668(8) 0.75063(10) 0.0131(3) Uani 1 1 d . . .
H31 H 0.6888 -0.0509 0.7970 0.016 Uiso 1 1 calc R . .
C32 C 0.63301(7) -0.12066(8) 0.73890(10) 0.0138(3) Uani 1 1 d . . .
H32 H 0.6135 -0.1251 0.7781 0.017 Uiso 1 1 calc R . .
C33 C 0.61695(7) -0.15808(8) 0.66836(10) 0.0126(3) Uani 1 1 d . . .
H33 H 0.5867 -0.1874 0.6595 0.015 Uiso 1 1 calc R . .
C34 C 0.64727(6) -0.15041(8) 0.61219(10) 0.0108(3) Uani 1 1 d . . .
C35 C 0.63656(7) -0.18613(8) 0.53162(10) 0.0118(3) Uani 1 1 d . . .
C36 C 0.82581(6) -0.20385(8) 0.54860(9) 0.0111(3) Uani 1 1 d . . .
C37 C 0.82063(6) -0.15961(8) 0.47528(9) 0.0107(3) Uani 1 1 d . . .
C38 C 0.85142(7) -0.16623(8) 0.41926(10) 0.0124(3) Uani 1 1 d . . .
H38 H 0.8785 -0.1995 0.4243 0.015 Uiso 1 1 calc R . .
C39 C 0.84068(7) -0.12151(9) 0.35489(10) 0.0143(3) Uani 1 1 d . . .
H39 H 0.8613 -0.1241 0.3168 0.017 Uiso 1 1 calc R . .
C40 C 0.79916(7) -0.07307(9) 0.34773(10) 0.0140(3) Uani 1 1 d . . .
H40 H 0.7913 -0.0434 0.3046 0.017 Uiso 1 1 calc R . .
C41 C 0.76966(6) -0.06976(8) 0.40612(9) 0.0106(3) Uani 1 1 d . . .
C42 C 0.72121(7) -0.02288(8) 0.40595(10) 0.0121(3) Uani 1 1 d . . .
C43 C 1.09592(7) 0.06220(9) 1.39076(10) 0.0144(3) Uani 1 1 d . . .
H43 H 1.1216 0.0460 1.3644 0.017 Uiso 1 1 calc R . .
C44 C 1.06376(7) 0.11729(9) 1.36155(10) 0.0135(3) Uani 1 1 d . . .
H44 H 1.0677 0.1383 1.3152 0.016 Uiso 1 1 calc R . .
C45 C 1.02510(7) 0.14193(8) 1.40100(10) 0.0126(3) Uani 1 1 d . . .
C46 C 1.02117(7) 0.10944(9) 1.47213(10) 0.0139(3) Uani 1 1 d . . .
H46 H 0.9965 0.1252 1.5006 0.017 Uiso 1 1 calc R . .
C47 C 1.05407(7) 0.05441(9) 1.49867(10) 0.0152(3) Uani 1 1 d . . .
H47 H 1.0515 0.0326 1.5452 0.018 Uiso 1 1 calc R . .
C48 C 0.99008(7) 0.19894(8) 1.36563(10) 0.0137(3) Uani 1 1 d . . .
H48 H 0.9985 0.2205 1.3224 0.016 Uiso 1 1 calc R . .
C49 C 0.94673(7) 0.22241(9) 1.39080(10) 0.0141(3) Uani 1 1 d . . .
H49 H 0.9387 0.2019 1.4350 0.017 Uiso 1 1 calc R . .
C50 C 0.91106(7) 0.27850(8) 1.35293(10) 0.0126(3) Uani 1 1 d . . .
C51 C 0.91528(7) 0.30787(9) 1.28084(10) 0.0152(3) Uani 1 1 d . . .
H51 H 0.9403 0.2907 1.2539 0.018 Uiso 1 1 calc R . .
C52 C 0.88230(7) 0.36220(9) 1.25003(10) 0.0169(4) Uani 1 1 d . . .
H52 H 0.8855 0.3822 1.2027 0.020 Uiso 1 1 calc R . .
C53 C 0.87124(7) 0.30461(9) 1.38998(10) 0.0149(3) Uani 1 1 d . . .
H53 H 0.8666 0.2854 1.4370 0.018 Uiso 1 1 calc R . .
C54 C 0.83919(7) 0.35876(9) 1.35630(10) 0.0156(4) Uani 1 1 d . . .
H54 H 0.8129 0.3764 1.3808 0.019 Uiso 1 1 calc R . .
C55 C 0.76262(7) 0.06254(9) 1.06477(10) 0.0148(3) Uani 1 1 d . . .
H55 H 0.7892 0.0465 1.0397 0.018 Uiso 1 1 calc R . .
C56 C 0.73181(7) 0.11859(9) 1.03582(10) 0.0145(4) Uani 1 1 d . . .
H56 H 0.7377 0.1407 0.9912 0.017 Uiso 1 1 calc R . .
C57 C 0.69170(7) 0.14275(8) 1.07275(10) 0.0126(3) Uani 1 1 d . . .
C58 C 0.68489(7) 0.10871(9) 1.14119(10) 0.0146(3) Uani 1 1 d . . .
H58 H 0.6591 0.1239 1.1680 0.017 Uiso 1 1 calc R . .
C59 C 0.71666(7) 0.05304(9) 1.16777(10) 0.0153(3) Uani 1 1 d . . .
H59 H 0.7122 0.0303 1.2128 0.018 Uiso 1 1 calc R . .
C60 C 0.65861(7) 0.20141(8) 1.03752(10) 0.0137(3) Uani 1 1 d . . .
H60 H 0.6685 0.2228 0.9953 0.016 Uiso 1 1 calc R . .
C61 C 0.61526(7) 0.22671(9) 1.06113(10) 0.0136(3) Uani 1 1 d . . .
H61 H 0.6059 0.2068 1.1047 0.016 Uiso 1 1 calc R . .
C62 C 0.58177(7) 0.28386(8) 1.02240(10) 0.0130(3) Uani 1 1 d . . .
C63 C 0.54166(7) 0.31144(9) 1.05789(10) 0.0143(3) Uani 1 1 d . . .
H63 H 0.5367 0.2936 1.1054 0.017 Uiso 1 1 calc R . .
C64 C 0.50963(7) 0.36508(9) 1.02207(10) 0.0150(3) Uani 1 1 d . . .
H64 H 0.4830 0.3834 1.0454 0.018 Uiso 1 1 calc R . .
C65 C 0.58759(7) 0.31267(9) 0.95049(10) 0.0160(4) Uani 1 1 d . . .
H65 H 0.6136 0.2954 0.9252 0.019 Uiso 1 1 calc R . .
C66 C 0.55481(7) 0.36627(9) 0.91801(10) 0.0177(4) Uani 1 1 d . . .
H66 H 0.5589 0.3857 0.8708 0.021 Uiso 1 1 calc R . .
C67 C 0.61358(7) -0.06652(9) 0.17184(10) 0.0157(4) Uani 1 1 d . . .
H67 H 0.6145 -0.0466 0.1234 0.019 Uiso 1 1 calc R . .
C68 C 0.64974(7) -0.11802(9) 0.20235(10) 0.0149(4) Uani 1 1 d . . .
H68 H 0.6752 -0.1331 0.1749 0.018 Uiso 1 1 calc R . .
C69 C 0.64783(7) -0.14782(8) 0.27577(10) 0.0130(3) Uani 1 1 d . . .
C70 C 0.60890(7) -0.12325(9) 0.31506(10) 0.0140(3) Uani 1 1 d . . .
H70 H 0.6070 -0.1418 0.3638 0.017 Uiso 1 1 calc R . .
C71 C 0.57358(7) -0.07192(9) 0.28188(10) 0.0150(3) Uani 1 1 d . . .
H71 H 0.5475 -0.0559 0.3077 0.018 Uiso 1 1 calc R . .
C72 C 0.68417(7) -0.20303(9) 0.31337(10) 0.0140(3) Uani 1 1 d . . .
H72 H 0.6781 -0.2213 0.3600 0.017 Uiso 1 1 calc R . .
C73 C 0.72550(7) -0.22931(9) 0.28596(10) 0.0136(3) Uani 1 1 d . . .
H73 H 0.7324 -0.2108 0.2400 0.016 Uiso 1 1 calc R . .
C74 C 0.76051(7) -0.28568(8) 0.32437(10) 0.0129(3) Uani 1 1 d . . .
C75 C 0.79833(7) -0.31437(9) 0.28577(10) 0.0143(3) Uani 1 1 d . . .
H75 H 0.8023 -0.2965 0.2377 0.017 Uiso 1 1 calc R . .
C76 C 0.82954(7) -0.36912(9) 0.31927(10) 0.0151(3) Uani 1 1 d . . .
H76 H 0.8548 -0.3881 0.2940 0.018 Uiso 1 1 calc R . .
C77 C 0.75692(7) -0.31348(9) 0.39748(10) 0.0156(4) Uani 1 1 d . . .
H77 H 0.7330 -0.2947 0.4253 0.019 Uiso 1 1 calc R . .
C78 C 0.78872(7) -0.36843(9) 0.42787(10) 0.0172(4) Uani 1 1 d . . .
H78 H 0.7861 -0.3872 0.4761 0.021 Uiso 1 1 calc R . .
H112 H 0.4890(8) -0.4179(8) 0.3136(12) 0.018(6) Uiso 1 1 d D . .
H214 H 0.7510(10) 0.0270(12) 0.8530(11) 0.039(8) Uiso 1 1 d D . .
H1W9 H 0.7563(8) 0.2050(10) 0.4332(10) 0.024(6) Uiso 1 1 d D . .
H113 H 1.0521(6) 0.0256(12) 1.2191(13) 0.034(7) Uiso 1 1 d D . .
H215 H 0.6130(6) -0.0286(12) 0.4512(13) 0.032(7) Uiso 1 1 d D . .
H213 H 1.0843(9) 0.0163(12) 1.1801(10) 0.030(7) Uiso 1 1 d D . .
H2W2 H 0.6557(8) -0.4028(8) 0.4786(13) 0.025(7) Uiso 1 1 d D . .
H2W4 H 0.8347(7) -0.3983(13) 0.6710(15) 0.054(9) Uiso 1 1 d D . .
H1W8 H 0.8279(7) 0.0991(13) 1.4982(17) 0.067(10) Uiso 1 1 d D . .
H211 H 0.5882(6) 0.1644(11) 0.2406(12) 0.032(6) Uiso 1 1 d D . .
H2W3 H 0.7450(9) -0.2793(9) 0.5953(13) 0.039(8) Uiso 1 1 d D . .
H115 H 0.5813(9) -0.0228(13) 0.4919(10) 0.046(8) Uiso 1 1 d D . .
H2W1 H 0.5654(9) -0.2840(11) 0.3378(9) 0.031(7) Uiso 1 1 d D . .
H1W5 H 0.8863(9) -0.2952(11) 0.6658(10) 0.033(7) Uiso 1 1 d D . .
H1W2 H 0.6420(8) -0.3530(11) 0.4448(14) 0.048(9) Uiso 1 1 d D . .
H1W1 H 0.5793(9) -0.2719(10) 0.4060(10) 0.035(7) Uiso 1 1 d D . .
H114 H 0.7180(7) 0.0355(12) 0.8935(13) 0.037(7) Uiso 1 1 d D . .
H2W9 H 0.7782(10) 0.2004(11) 0.5070(9) 0.040(7) Uiso 1 1 d D . .
H2W8 H 0.8759(9) 0.1196(11) 1.5270(16) 0.057(9) Uiso 1 1 d D . .
H1W3 H 0.7135(10) -0.3196(13) 0.5624(12) 0.067(11) Uiso 1 1 d D . .
H1W4 H 0.7879(10) -0.3791(11) 0.6404(17) 0.064(10) Uiso 1 1 d D . .
H2W5 H 0.9040(9) -0.2903(11) 0.7383(11) 0.038(8) Uiso 1 1 d D . .
H212 H 0.5206(10) -0.4567(13) 0.2920(14) 0.074(11) Uiso 1 1 d D . .
H111 H 0.5402(9) 0.1970(10) 0.2175(16) 0.075(10) Uiso 1 1 d D . .
H1W7 H 0.9204(11) 0.2127(10) 1.5798(17) 0.066(10) Uiso 1 1 d D . .
H110 H 0.6731(9) 0.1656(9) 0.3279(15) 0.055(9) Uiso 1 1 d D . .
H2W6 H 1.0094(10) 0.0915(9) 1.6969(15) 0.051(9) Uiso 1 1 d D . .
H210 H 0.6671(10) 0.1061(9) 0.3410(14) 0.045(8) Uiso 1 1 d D . .
H1W6 H 1.0272(8) 0.1434(12) 1.7317(14) 0.058(9) Uiso 1 1 d D . .
H2W7 H 0.9528(15) 0.1709(18) 1.6120(15) 0.15(2) Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 N1 178.60(6) . . ?
N2 Ni1 O5 78.64(5) . . ?
N1 Ni1 O5 101.34(5) . . ?
N2 Ni1 O4 103.39(5) . . ?
N1 Ni1 O4 78.01(5) . . ?
O5 Ni1 O4 93.46(5) . . ?
N2 Ni1 O2 100.82(5) . . ?
N1 Ni1 O2 77.78(5) . . ?
O5 Ni1 O2 90.17(5) . . ?
O4 Ni1 O2 155.77(4) . . ?
N2 Ni1 O7 77.80(5) . . ?
N1 Ni1 O7 102.21(5) . . ?
O5 Ni1 O7 156.45(4) . . ?
O4 Ni1 O7 91.78(5) . . ?
O2 Ni1 O7 94.40(5) . . ?
N4 Ni2 N3 176.37(6) . . ?
N4 Ni2 O13 78.98(5) . . ?
N3 Ni2 O13 98.51(5) . . ?
N4 Ni2 O10 98.73(5) . . ?
N3 Ni2 O10 78.57(5) . . ?
O13 Ni2 O10 89.84(5) . . ?
N4 Ni2 O12 104.68(5) . . ?
N3 Ni2 O12 78.06(5) . . ?
O13 Ni2 O12 94.93(5) . . ?
O10 Ni2 O12 156.59(4) . . ?
N4 Ni2 O15 77.56(5) . . ?
N3 Ni2 O15 104.98(5) . . ?
O13 Ni2 O15 156.50(4) . . ?
O10 Ni2 O15 94.89(5) . . ?
O12 Ni2 O15 89.82(5) . . ?
N5 Ni3 N6 177.22(6) . . ?
N5 Ni3 O20 79.13(5) . . ?
N6 Ni3 O20 99.04(5) . . ?
N5 Ni3 O23 99.81(5) . . ?
N6 Ni3 O23 78.03(5) . . ?
O20 Ni3 O23 89.71(5) . . ?
N5 Ni3 O21 103.91(5) . . ?
N6 Ni3 O21 78.20(5) . . ?
O20 Ni3 O21 92.64(5) . . ?
O23 Ni3 O21 156.19(4) . . ?
N5 Ni3 O17 77.60(5) . . ?
N6 Ni3 O17 104.23(5) . . ?
O20 Ni3 O17 156.73(4) . . ?
O23 Ni3 O17 94.63(5) . . ?
O21 Ni3 O17 92.52(5) . . ?
C1 O2 Ni1 114.51(10) . . ?
C7 O4 Ni1 114.62(10) . . ?
C14 O5 Ni1 114.33(10) . . ?
C8 O7 Ni1 114.35(10) . . ?
C15 O10 Ni2 114.20(10) . . ?
C21 O12 Ni2 114.69(10) . . ?
C22 O13 Ni2 114.31(10) . . ?
C28 O15 Ni2 113.76(10) . . ?
C29 O17 Ni3 114.25(10) . . ?
C35 O20 Ni3 114.17(10) . . ?
C42 O21 Ni3 114.30(10) . . ?
C36 O23 Ni3 114.45(10) . . ?
C6 N1 C2 121.41(14) . . ?
C6 N1 Ni1 118.93(11) . . ?
C2 N1 Ni1 119.63(11) . . ?
C9 N2 C13 121.59(14) . . ?
C9 N2 Ni1 119.62(11) . . ?
C13 N2 Ni1 118.71(11) . . ?
C20 N3 C16 121.85(14) . . ?
C20 N3 Ni2 119.33(11) . . ?
C16 N3 Ni2 118.66(11) . . ?
C27 N4 C23 121.61(14) . . ?
C27 N4 Ni2 120.02(11) . . ?
C23 N4 Ni2 118.24(11) . . ?
C34 N5 C30 121.55(14) . . ?
C34 N5 Ni3 118.35(11) . . ?
C30 N5 Ni3 119.96(11) . . ?
C41 N6 C37 121.63(14) . . ?
C41 N6 Ni3 118.83(11) . . ?
C37 N6 Ni3 119.43(11) . . ?
C52 N7 C54 122.08(15) . . ?
C47 N8 C43 121.88(15) . . ?
C64 N9 C66 122.10(15) . . ?
C59 N10 C55 121.70(15) . . ?
C67 N11 C71 122.35(15) . . ?
C78 N12 C76 121.74(15) . . ?
O1 C1 O2 126.79(15) . . ?
O1 C1 C2 118.01(14) . . ?
O2 C1 C2 115.20(14) . . ?
N1 C2 C3 121.08(15) . . ?
N1 C2 C1 112.87(14) . . ?
C3 C2 C1 126.04(15) . . ?
C2 C3 C4 118.43(15) . . ?
C5 C4 C3 119.57(15) . . ?
C6 C5 C4 118.75(16) . . ?
N1 C6 C5 120.74(15) . . ?
N1 C6 C7 113.17(14) . . ?
C5 C6 C7 126.06(15) . . ?
O3 C7 O4 127.42(15) . . ?
O3 C7 C6 117.33(14) . . ?
O4 C7 C6 115.24(14) . . ?
O8 C8 O7 127.01(15) . . ?
O8 C8 C9 117.20(14) . . ?
O7 C8 C9 115.78(14) . . ?
N2 C9 C10 120.66(15) . . ?
N2 C9 C8 112.41(14) . . ?
C10 C9 C8 126.92(15) . . ?
C11 C10 C9 118.57(15) . . ?
C10 C11 C12 120.03(15) . . ?
C13 C12 C11 118.16(15) . . ?
N2 C13 C12 120.96(15) . . ?
N2 C13 C14 112.65(14) . . ?
C12 C13 C14 126.39(15) . . ?
O6 C14 O5 127.07(16) . . ?
O6 C14 C13 117.38(14) . . ?
O5 C14 C13 115.54(14) . . ?
O9 C15 O10 126.07(16) . . ?
O9 C15 C16 118.51(15) . . ?
O10 C15 C16 115.42(14) . . ?
N3 C16 C17 120.68(15) . . ?
N3 C16 C15 112.71(14) . . ?
C17 C16 C15 126.61(15) . . ?
C16 C17 C18 118.39(15) . . ?
C19 C18 C17 119.79(16) . . ?
C20 C19 C18 118.62(16) . . ?
N3 C20 C19 120.64(15) . . ?
N3 C20 C21 112.74(14) . . ?
C19 C20 C21 126.56(15) . . ?
O11 C21 O12 126.88(15) . . ?
O11 C21 C20 117.93(14) . . ?
O12 C21 C20 115.17(14) . . ?
O14 C22 O13 126.09(16) . . ?
O14 C22 C23 118.36(14) . . ?
O13 C22 C23 115.53(14) . . ?
N4 C23 C24 120.90(15) . . ?
N4 C23 C22 112.75(14) . . ?
C24 C23 C22 126.32(15) . . ?
C23 C24 C25 118.46(15) . . ?
C26 C25 C24 119.77(15) . . ?
C25 C26 C27 118.72(15) . . ?
N4 C27 C26 120.51(15) . . ?
N4 C27 C28 113.01(14) . . ?
C26 C27 C28 126.47(14) . . ?
O16 C28 O15 126.55(15) . . ?
O16 C28 C27 117.89(14) . . ?
O15 C28 C27 115.55(14) . . ?
O18 C29 O17 126.69(15) . . ?
O18 C29 C30 117.19(14) . . ?
O17 C29 C30 116.12(14) . . ?
N5 C30 C31 120.52(15) . . ?
N5 C30 C29 111.92(14) . . ?
C31 C30 C29 127.55(15) . . ?
C30 C31 C32 118.42(15) . . ?
C31 C32 C33 120.07(15) . . ?
C34 C33 C32 118.05(15) . . ?
N5 C34 C33 121.37(15) . . ?
N5 C34 C35 112.34(14) . . ?
C33 C34 C35 126.30(15) . . ?
O19 C35 O20 126.58(15) . . ?
O19 C35 C34 117.82(14) . . ?
O20 C35 C34 115.59(14) . . ?
O24 C36 O23 126.69(15) . . ?
O24 C36 C37 118.27(14) . . ?
O23 C36 C37 115.04(14) . . ?
N6 C37 C38 121.30(15) . . ?
N6 C37 C36 113.00(14) . . ?
C38 C37 C36 125.68(15) . . ?
C37 C38 C39 118.02(15) . . ?
C40 C39 C38 119.91(16) . . ?
C41 C40 C39 118.79(15) . . ?
N6 C41 C40 120.33(15) . . ?
N6 C41 C42 113.54(14) . . ?
C40 C41 C42 126.07(15) . . ?
O22 C42 O21 127.42(15) . . ?
O22 C42 C41 117.43(14) . . ?
O21 C42 C41 115.13(14) . . ?
N8 C43 C44 119.72(15) . . ?
C43 C44 C45 120.40(16) . . ?
C44 C45 C46 118.09(16) . . ?
C44 C45 C48 118.36(15) . . ?
C46 C45 C48 123.54(15) . . ?
C47 C46 C45 119.27(16) . . ?
N8 C47 C46 120.63(16) . . ?
C49 C48 C45 124.93(16) . . ?
C48 C49 C50 124.06(16) . . ?
C51 C50 C53 118.04(15) . . ?
C51 C50 C49 122.62(15) . . ?
C53 C50 C49 119.34(16) . . ?
C52 C51 C50 119.91(16) . . ?
N7 C52 C51 120.02(16) . . ?
C54 C53 C50 119.53(16) . . ?
N7 C54 C53 120.38(16) . . ?
N10 C55 C56 119.69(15) . . ?
C55 C56 C57 120.52(16) . . ?
C56 C57 C58 117.98(16) . . ?
C56 C57 C60 118.17(15) . . ?
C58 C57 C60 123.84(15) . . ?
C59 C58 C57 119.28(16) . . ?
N10 C59 C58 120.81(16) . . ?
C61 C60 C57 125.38(16) . . ?
C60 C61 C62 123.84(16) . . ?
C63 C62 C65 117.95(15) . . ?
C63 C62 C61 119.01(15) . . ?
C65 C62 C61 123.04(15) . . ?
C64 C63 C62 119.75(16) . . ?
N9 C64 C63 120.12(16) . . ?
C66 C65 C62 119.64(16) . . ?
N9 C66 C65 120.43(16) . . ?
N11 C67 C68 120.26(16) . . ?
C67 C68 C69 119.33(16) . . ?
C70 C69 C68 118.26(15) . . ?
C70 C69 C72 117.92(15) . . ?
C68 C69 C72 123.81(15) . . ?
C71 C70 C69 120.11(16) . . ?
N11 C71 C70 119.69(15) . . ?
C73 C72 C69 125.13(16) . . ?
C72 C73 C74 123.71(16) . . ?
C77 C74 C75 118.11(16) . . ?
C77 C74 C73 122.85(15) . . ?
C75 C74 C73 119.03(15) . . ?
C76 C75 C74 119.63(16) . . ?
N12 C76 C75 120.35(16) . . ?
C78 C77 C74 119.81(16) . . ?
N12 C78 C77 120.33(16) . . ?
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 1.9620(14) . ?
Ni1 N1 1.9650(14) . ?
Ni1 O5 2.1193(12) . ?
Ni1 O4 2.1347(12) . ?
Ni1 O2 2.1406(12) . ?
Ni1 O7 2.1453(12) . ?
Ni2 N4 1.9600(14) . ?
Ni2 N3 1.9623(14) . ?
Ni2 O13 2.1074(12) . ?
Ni2 O10 2.1189(12) . ?
Ni2 O12 2.1264(12) . ?
Ni2 O15 2.1718(12) . ?
Ni3 N5 1.9609(14) . ?
Ni3 N6 1.9611(14) . ?
Ni3 O20 2.0981(12) . ?
Ni3 O23 2.1384(12) . ?
Ni3 O21 2.1412(12) . ?
Ni3 O17 2.1478(12) . ?
O1 C1 1.2380(19) . ?
O2 C1 1.2786(19) . ?
O3 C7 1.244(2) . ?
O4 C7 1.2669(19) . ?
O5 C14 1.2716(19) . ?
O6 C14 1.246(2) . ?
O7 C8 1.2594(19) . ?
O8 C8 1.2487(19) . ?
O9 C15 1.238(2) . ?
O10 C15 1.2737(19) . ?
O11 C21 1.241(2) . ?
O12 C21 1.2713(19) . ?
O13 C22 1.2689(19) . ?
O14 C22 1.247(2) . ?
O15 C28 1.2701(19) . ?
O16 C28 1.2465(19) . ?
O17 C29 1.2565(19) . ?
O18 C29 1.2542(19) . ?
O19 C35 1.2396(19) . ?
O20 C35 1.2755(19) . ?
O21 C42 1.2699(19) . ?
O22 C42 1.243(2) . ?
O23 C36 1.2796(19) . ?
O24 C36 1.2368(19) . ?
N1 C6 1.335(2) . ?
N1 C2 1.336(2) . ?
N2 C9 1.335(2) . ?
N2 C13 1.338(2) . ?
N3 C20 1.332(2) . ?
N3 C16 1.337(2) . ?
N4 C27 1.334(2) . ?
N4 C23 1.338(2) . ?
N5 C34 1.336(2) . ?
N5 C30 1.336(2) . ?
N6 C41 1.334(2) . ?
N6 C37 1.337(2) . ?
N7 C52 1.340(2) . ?
N7 C54 1.342(2) . ?
N8 C47 1.345(2) . ?
N8 C43 1.350(2) . ?
N9 C64 1.338(2) . ?
N9 C66 1.342(2) . ?
N10 C59 1.345(2) . ?
N10 C55 1.346(2) . ?
N11 C67 1.342(2) . ?
N11 C71 1.349(2) . ?
N12 C78 1.343(2) . ?
N12 C76 1.342(2) . ?
C1 C2 1.517(2) . ?
C2 C3 1.382(2) . ?
C3 C4 1.395(2) . ?
C4 C5 1.391(2) . ?
C5 C6 1.385(2) . ?
C6 C7 1.517(2) . ?
C8 C9 1.524(2) . ?
C9 C10 1.387(2) . ?
C10 C11 1.387(2) . ?
C11 C12 1.396(2) . ?
C12 C13 1.384(2) . ?
C13 C14 1.523(2) . ?
C15 C16 1.522(2) . ?
C16 C17 1.385(2) . ?
C17 C18 1.396(2) . ?
C18 C19 1.389(2) . ?
C19 C20 1.387(2) . ?
C20 C21 1.521(2) . ?
C22 C23 1.523(2) . ?
C23 C24 1.383(2) . ?
C24 C25 1.394(2) . ?
C25 C26 1.387(2) . ?
C26 C27 1.390(2) . ?
C27 C28 1.522(2) . ?
C29 C30 1.523(2) . ?
C30 C31 1.388(2) . ?
C31 C32 1.391(2) . ?
C32 C33 1.395(2) . ?
C33 C34 1.377(2) . ?
C34 C35 1.523(2) . ?
C36 C37 1.520(2) . ?
C37 C38 1.382(2) . ?
C38 C39 1.395(2) . ?
C39 C40 1.390(2) . ?
C40 C41 1.389(2) . ?
C41 C42 1.518(2) . ?
C43 C44 1.372(2) . ?
C44 C45 1.397(2) . ?
C45 C46 1.412(2) . ?
C45 C48 1.462(2) . ?
C46 C47 1.371(2) . ?
C48 C49 1.340(2) . ?
C49 C50 1.468(2) . ?
C50 C51 1.402(2) . ?
C50 C53 1.404(2) . ?
C51 C52 1.376(2) . ?
C53 C54 1.375(2) . ?
C55 C56 1.371(2) . ?
C56 C57 1.394(2) . ?
C57 C58 1.408(2) . ?
C57 C60 1.465(2) . ?
C58 C59 1.367(2) . ?
C60 C61 1.339(2) . ?
C61 C62 1.464(2) . ?
C62 C63 1.404(2) . ?
C62 C65 1.407(2) . ?
C63 C64 1.378(2) . ?
C65 C66 1.370(2) . ?
C67 C68 1.373(2) . ?
C68 C69 1.411(2) . ?
C69 C70 1.400(2) . ?
C69 C72 1.462(2) . ?
C70 C71 1.370(2) . ?
C72 C73 1.338(2) . ?
C73 C74 1.467(2) . ?
C74 C77 1.401(2) . ?
C74 C75 1.401(2) . ?
C75 C76 1.374(2) . ?
C77 C78 1.370(2) . ?
