#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007942.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_7007942
loop_
_publ_author_name
'Fontecha, Julia Barreira'
'Goetz, Sandrine'
'McKee, Vickie'
_publ_section_title
;
 Dinuclear complexes of a pseudocalixarene macrocycle: structural
 consequences of intramolecular hydrogen bonding.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              923
_journal_page_last               929
_journal_paper_doi               10.1039/b413639j
_journal_year                    2005
_chemical_formula_sum            'C64 H104 Cl2 N4 Ni2 O21'
_chemical_formula_weight         1453.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.9805(12)
_cell_length_b                   13.7050(6)
_cell_length_c                   18.8743(8)
_cell_measurement_reflns_used    21493
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.27
_cell_volume                     7237.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50518
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.872055
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6664
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0589P)²+27.7475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                5805
_reflns_number_total             6664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413639j.txt
_cod_data_source_block           Complex5a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7007942
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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 0.070237(19) 0.09613(4) 0.27355(3) 0.03032(19) Uani 1 1 d . . .
O1 O 0.01954(10) 0.1626(2) 0.21712(16) 0.0303(7) Uani 1 1 d . . .
C1 C -0.02132(15) 0.1210(3) 0.1945(2) 0.0309(10) Uani 1 1 d . . .
C2 C -0.04466(16) 0.1580(4) 0.1342(2) 0.0362(11) Uani 1 1 d . . .
C3 C -0.08563(17) 0.1114(4) 0.1104(3) 0.0432(12) Uani 1 1 d . . .
H3 H -0.1012 0.1367 0.0697 0.052 Uiso 1 1 calc R . .
C4 C -0.10498(17) 0.0298(4) 0.1430(3) 0.0482(14) Uani 1 1 d . . .
C5 C -0.15091(19) -0.0188(5) 0.1135(4) 0.0644(18) Uani 1 1 d . . .
C6 C -0.1481(3) -0.0291(9) 0.0354(5) 0.135(5) Uani 1 1 d . . .
H6A H -0.1202 -0.0687 0.0230 0.050 Uiso 1 1 calc R . .
H6B H -0.1451 0.0356 0.0137 0.050 Uiso 1 1 calc R . .
H6C H -0.1771 -0.0610 0.0179 0.050 Uiso 1 1 calc R . .
C7 C -0.19371(19) 0.0417(5) 0.1349(4) 0.0703(19) Uani 1 1 d . . .
H7A H -0.1954 0.0454 0.1867 0.050 Uiso 1 1 calc R . .
H7B H -0.2229 0.0113 0.1166 0.050 Uiso 1 1 calc R . .
H7C H -0.1906 0.1076 0.1153 0.050 Uiso 1 1 calc R . .
C8 C -0.1576(3) -0.1209(6) 0.1412(7) 0.149(5) Uani 1 1 d . . .
H8A H -0.1593 -0.1194 0.1930 0.050 Uiso 1 1 calc R . .
H8B H -0.1305 -0.1615 0.1264 0.050 Uiso 1 1 calc R . .
H8C H -0.1872 -0.1483 0.1221 0.050 Uiso 1 1 calc R . .
C9 C -0.08313(17) -0.0025(4) 0.2045(3) 0.0457(13) Uani 1 1 d . . .
H9 H -0.0968 -0.0557 0.2296 0.055 Uiso 1 1 calc R . .
C10 C -0.04115(15) 0.0416(3) 0.2309(3) 0.0352(11) Uani 1 1 d . . .
C11 C -0.0267(2) 0.2500 0.0982(3) 0.0382(16) Uani 1 2 d S . .
H11A H -0.0372 0.2500 0.0482 0.046 Uiso 1 2 calc SR . .
H11B H 0.0087 0.2500 0.0987 0.046 Uiso 1 2 calc SR . .
C12 C -0.02316(16) 0.0079(3) 0.2995(3) 0.0382(11) Uani 1 1 d . . .
H12 H -0.0432 -0.0352 0.3254 0.046 Uiso 1 1 calc R . .
N1 N 0.01673(13) 0.0304(3) 0.3284(2) 0.0361(9) Uani 1 1 d . B .
C13 C 0.02417(18) -0.0051(4) 0.4011(3) 0.0469(13) Uani 1 1 d . . .
H13A H -0.0032 -0.0467 0.4149 0.056 Uiso 1 1 calc R A 1
H13B H 0.0250 0.0513 0.4338 0.056 Uiso 1 1 calc R A 1
C14 C 0.0701(2) -0.0632(4) 0.4092(3) 0.0497(13) Uani 0.75 1 d P B 1
H14 H 0.0702 -0.0895 0.4586 0.060 Uiso 0.75 1 calc PR B 1
O2 O 0.07064(17) -0.1428(3) 0.3646(3) 0.0495(12) Uani 0.75 1 d P B 1
C14' C 0.0701(2) -0.0632(4) 0.4092(3) 0.0497(13) Uani 0.25 1 d P B 2
H14' H 0.0703 -0.1101 0.3686 0.060 Uiso 0.25 1 calc PR B 2
O2' O 0.0702(7) -0.1203(17) 0.4693(12) 0.092(7) Uani 0.25 1 d P B 2
C15 C 0.11540(18) -0.0035(4) 0.4011(3) 0.0436(12) Uani 1 1 d . . .
H15A H 0.1136 0.0539 0.4329 0.052 Uiso 1 1 calc R B 1
H15B H 0.1430 -0.0435 0.4162 0.052 Uiso 1 1 calc R B 1
N2 N 0.12351(13) 0.0304(3) 0.3283(2) 0.0352(9) Uani 1 1 d . B .
C16 C 0.16294(16) 0.0068(3) 0.2985(3) 0.0385(11) Uani 1 1 d . . .
H16 H 0.1826 -0.0378 0.3238 0.046 Uiso 1 1 calc R B .
C17 C 0.18125(15) 0.0401(3) 0.2307(2) 0.0352(10) Uani 1 1 d . B .
C18 C 0.22247(17) -0.0051(4) 0.2043(3) 0.0448(13) Uani 1 1 d . . .
H18 H 0.2350 -0.0598 0.2290 0.054 Uiso 1 1 calc R B .
C19 C 0.24567(16) 0.0262(4) 0.1440(3) 0.0435(12) Uani 1 1 d . B .
C20 C 0.2898(2) -0.0248(5) 0.1136(4) 0.0662(19) Uani 1 1 d . . .
C21 C 0.3011(3) -0.1187(6) 0.1512(6) 0.160(6) Uani 1 1 d . B .
H21A H 0.2733 -0.1622 0.1488 0.050 Uiso 1 1 calc R . .
H21B H 0.3087 -0.1050 0.2009 0.050 Uiso 1 1 calc R . .
H21C H 0.3286 -0.1501 0.1284 0.050 Uiso 1 1 calc R . .
C22 C 0.3324(2) 0.0418(6) 0.1166(4) 0.081(2) Uani 1 1 d . B .
H22A H 0.3603 0.0084 0.0965 0.050 Uiso 1 1 calc R . .
H22B H 0.3390 0.0593 0.1660 0.050 Uiso 1 1 calc R . .
H22C H 0.3258 0.1010 0.0892 0.050 Uiso 1 1 calc R . .
C23 C 0.2805(2) -0.0510(6) 0.0367(5) 0.098(3) Uani 1 1 d . B .
H23A H 0.2531 -0.0952 0.0339 0.050 Uiso 1 1 calc R . .
H23B H 0.3088 -0.0831 0.0169 0.050 Uiso 1 1 calc R . .
H23C H 0.2737 0.0085 0.0098 0.050 Uiso 1 1 calc R . .
C24 C 0.22721(15) 0.1101(3) 0.1116(3) 0.0340(10) Uani 1 1 d . . .
H24 H 0.2434 0.1356 0.0714 0.041 Uiso 1 1 calc R B .
C25 C 0.18670(14) 0.1579(3) 0.1352(2) 0.0272(9) Uani 1 1 d . B .
C26 C 0.16216(14) 0.1202(3) 0.1940(2) 0.0287(9) Uani 1 1 d . . .
O3 O 0.12143(10) 0.1626(2) 0.21627(16) 0.0292(7) Uani 1 1 d . B .
C27 C 0.1696(2) 0.2500 0.0982(3) 0.0280(13) Uani 1 2 d S . .
H27A H 0.1815 0.2500 0.0488 0.034 Uiso 1 2 calc SR B .
H27B H 0.1343 0.2500 0.0966 0.034 Uiso 1 2 calc SR . .
O4 O 0.07067(16) 0.2500 0.3331(3) 0.0440(12) Uani 1 2 d S . .
Cl1 Cl -0.19827(7) 0.2500 0.57964(13) 0.0468(5) Uani 0.90 2 d SP . .
O11 O -0.22356(19) 0.1657(4) 0.5722(4) 0.123(2) Uani 1 1 d . . .
O12 O -0.1575(4) 0.2500 0.5319(8) 0.134(5) Uani 0.90 2 d SP . .
O13 O -0.1734(5) 0.2500 0.6420(6) 0.166(5) Uani 1 2 d S . .
Cl1' Cl -0.2121(8) 0.2500 0.6230(13) 0.043(4) Uiso 0.10 2 d SP . .
O12' O -0.233(6) 0.2500 0.663(9) 0.19(6) Uiso 0.10 2 d SP . .
Cl2 Cl 0.06891(6) 0.2500 0.57652(11) 0.0517(5) Uani 1 2 d S . .
O21 O 0.0805(3) 0.2500 0.6488(4) 0.121(4) Uani 1 2 d S . .
O22 O 0.0177(2) 0.2500 0.5679(4) 0.075(2) Uani 1 2 d S . .
O23 O 0.0871(2) 0.1666(5) 0.5445(4) 0.120(2) Uani 1 1 d . . .
O30 O 0.06870(12) -0.0174(2) 0.19884(19) 0.0426(8) Uani 1 1 d . . .
C31 C 0.07369(19) -0.0022(4) 0.1240(3) 0.0487(13) Uani 1 1 d . . .
H31A H 0.1063 -0.0218 0.1093 0.058 Uiso 1 1 calc R . .
H31B H 0.0699 0.0681 0.1136 0.058 Uiso 1 1 calc R . .
C32 C 0.0378(2) -0.0589(5) 0.0814(4) 0.0677(19) Uani 1 1 d . . .
H32A H 0.0419 -0.1288 0.0904 0.102 Uiso 1 1 calc R . .
H32B H 0.0426 -0.0456 0.0309 0.102 Uiso 1 1 calc R . .
H32C H 0.0054 -0.0391 0.0952 0.102 Uiso 1 1 calc R . .
O40 O -0.0056(2) 0.2500 0.4209(4) 0.070(2) Uani 1 2 d SD . .
C41 C -0.0573(7) 0.2190(12) 0.4114(10) 0.191(16) Uani 0.50 1 d PD . .
H41A H -0.0609 0.1470 0.4133 0.050 Uiso 0.50 1 d P . .
H41B H -0.0780 0.2500 0.4499 0.050 Uiso 1 2 d S . .
C42 C -0.0761(6) 0.2500 0.3490(10) 0.171(9) Uani 1 2 d SD . .
H42A H -0.1094 0.2288 0.3456 0.050 Uiso 0.50 1 calc PR . .
H42B H -0.0577 0.2221 0.3096 0.050 Uiso 0.50 1 calc PR . .
H42C H -0.0746 0.3214 0.3467 0.050 Uiso 0.50 1 calc PR . .
C52 C -0.0357(4) -0.2500 0.1820(8) 0.111(5) Uani 1 2 d SD . .
H52A H -0.0639 -0.2815 0.2027 0.050 Uiso 0.50 1 calc PR . .
H52B H -0.0257 -0.2859 0.1396 0.050 Uiso 0.50 1 calc PR . .
H52C H -0.0435 -0.1826 0.1691 0.050 Uiso 0.50 1 calc PR . .
C51 C 0.0022(4) -0.2500 0.2325(6) 0.080(3) Uani 1 2 d SD . .
H51A H 0.0099 -0.3183 0.2453 0.050 Uiso 0.50 1 calc PR . .
H51B H -0.0087 -0.2164 0.2760 0.050 Uiso 0.50 1 calc PR . .
O50 O 0.0449(4) -0.2029(7) 0.2068(8) 0.116(5) Uani 0.50 1 d PD . .
O60 O 0.14889(18) 0.2500 0.4185(3) 0.0553(14) Uani 1 2 d S . .
C61 C 0.1969(3) 0.2500 0.4082(6) 0.110(5) Uani 1 2 d S . .
H61A H 0.2097 0.3079 0.4332 0.050 Uiso 0.50 1 calc PR . .
H61B H 0.2097 0.1921 0.4332 0.050 Uiso 0.50 1 calc PR . .
C62 C 0.2164(3) 0.2500 0.3437(5) 0.075(3) Uani 1 2 d S . .
H62A H 0.2473 0.2836 0.3453 0.050 Uiso 0.50 1 calc PR . .
H62B H 0.1951 0.2838 0.3106 0.050 Uiso 0.50 1 calc PR . .
H62C H 0.2211 0.1826 0.3279 0.050 Uiso 0.50 1 calc PR . .
C72 C 0.1555(5) -0.2500 0.1196(8) 0.125(6) Uani 1 2 d S . .
H72A H 0.1800 -0.2065 0.1001 0.050 Uiso 0.50 1 calc PR . .
H72B H 0.1238 -0.2271 0.1050 0.050 Uiso 0.50 1 calc PR . .
H72C H 0.1606 -0.3164 0.1018 0.050 Uiso 0.50 1 calc PR . .
C71 C 0.1585(4) -0.2500 0.1947(7) 0.086(3) Uani 1 2 d S . .
H71A H 0.1543 -0.1822 0.2116 0.050 Uiso 0.50 1 calc PR . .
H71B H 0.1910 -0.2713 0.2084 0.050 Uiso 0.50 1 calc PR . .
O70 O 0.1236(3) -0.3123(6) 0.2313(5) 0.073(3) Uani 0.50 1 d P . .
H1O H 0.0240 0.2500 0.2066 0.050 Uiso 1 2 d S . .
H3O H 0.1210 0.2500 0.2048 0.050 Uiso 1 2 d S . .
H4OA H 0.0938 0.2500 0.3619 0.050 Uiso 1 2 d S . .
H4OB H 0.0464 0.2500 0.3607 0.050 Uiso 1 2 d S . .
H30 H 0.0609 -0.0772 0.2012 0.050 Uiso 1 1 d . . .
H40 H 0.0028 0.2500 0.4617 0.050 Uiso 1 2 d S . .
H50 H 0.0698 -0.2374 0.2147 0.050 Uiso 0.50 1 d P . .
H70 H 0.1400 -0.2944 0.2673 0.050 Uiso 0.50 1 d P . .
H60 H 0.1380 0.2500 0.4686 0.050 Uiso 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 '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
O1 Ni1 O3 90.72(12) . . ?
O1 Ni1 N2 177.90(14) . . ?
O3 Ni1 N2 87.21(13) . . ?
O1 Ni1 N1 87.16(14) . . ?
O3 Ni1 N1 177.79(14) . . ?
N2 Ni1 N1 94.90(15) . . ?
O1 Ni1 O30 88.02(13) . . ?
O3 Ni1 O30 89.37(12) . . ?
N2 Ni1 O30 91.58(15) . . ?
N1 Ni1 O30 89.92(15) . . ?
O1 Ni1 O4 81.47(13) . . ?
O3 Ni1 O4 81.37(13) . . ?
N2 Ni1 O4 98.58(15) . . ?
N1 Ni1 O4 98.93(15) . . ?
O30 Ni1 O4 165.86(14) . . ?
C1 O1 Ni1 125.4(3) . . ?
O1 C1 C10 120.6(4) . . ?
O1 C1 C2 119.9(4) . . ?
C10 C1 C2 119.5(4) . . ?
C3 C2 C1 118.7(5) . . ?
C3 C2 C11 120.8(5) . . ?
C1 C2 C11 120.5(4) . . ?
C2 C3 C4 123.4(5) . . ?
C9 C4 C3 117.2(5) . . ?
C9 C4 C5 122.0(6) . . ?
C3 C4 C5 120.6(5) . . ?
C6 C5 C8 105.3(8) . . ?
C6 C5 C7 111.1(7) . . ?
C8 C5 C7 108.6(7) . . ?
C6 C5 C4 110.8(5) . . ?
C8 C5 C4 112.1(6) . . ?
C7 C5 C4 109.0(5) . . ?
C4 C9 C10 121.8(5) . . ?
C1 C10 C9 119.2(5) . . ?
C1 C10 C12 122.8(4) . . ?
C9 C10 C12 117.6(4) . . ?
C2 C11 C2 112.3(5) . 7_565 ?
N1 C12 C10 126.9(4) . . ?
C12 N1 C13 116.2(4) . . ?
C12 N1 Ni1 122.2(3) . . ?
C13 N1 Ni1 121.2(3) . . ?
N1 C13 C14 112.7(4) . . ?
O2 C14 C15 110.8(5) . . ?
O2 C14 C13 111.3(5) . . ?
C15 C14 C13 114.5(4) . . ?
N2 C15 C14 113.2(4) . . ?
C16 N2 C15 117.7(4) . . ?
C16 N2 Ni1 121.6(3) . . ?
C15 N2 Ni1 120.3(3) . . ?
N2 C16 C17 127.7(4) . . ?
C18 C17 C26 118.9(4) . . ?
C18 C17 C16 117.7(4) . . ?
C26 C17 C16 123.1(4) . . ?
C19 C18 C17 123.0(4) . . ?
C18 C19 C24 116.2(4) . . ?
C18 C19 C20 123.2(5) . . ?
C24 C19 C20 120.6(5) . . ?
C22 C20 C21 109.6(7) . . ?
C22 C20 C23 108.4(6) . . ?
C21 C20 C23 106.6(7) . . ?
C22 C20 C19 110.4(5) . . ?
C21 C20 C19 112.5(5) . . ?
C23 C20 C19 109.2(5) . . ?
C25 C24 C19 123.4(4) . . ?
C24 C25 C26 118.8(4) . . ?
C24 C25 C27 120.2(4) . . ?
C26 C25 C27 121.0(4) . . ?
O3 C26 C25 120.2(4) . . ?
O3 C26 C17 120.3(4) . . ?
C25 C26 C17 119.5(4) . . ?
C26 O3 Ni1 125.1(3) . . ?
C25 C27 C25 112.4(5) 7_565 . ?
Ni1 O4 Ni1 123.9(2) . 7_565 ?
Cl1' Cl1 O11 82.6(7) . . ?
Cl1' Cl1 O11 82.6(7) . 7_565 ?
O11 Cl1 O11 116.0(5) . 7_565 ?
Cl1' Cl1 O13 55.9(14) . . ?
O11 Cl1 O13 110.7(5) . . ?
O11 Cl1 O13 110.7(5) 7_565 . ?
Cl1' Cl1 O12 153.6(14) . . ?
O11 Cl1 O12 110.1(4) . . ?
O11 Cl1 O12 110.1(4) 7_565 . ?
O13 Cl1 O12 97.7(9) . . ?
Cl1' Cl1 O12' 6(5) . . ?
O11 Cl1 O12' 79(2) . . ?
O11 Cl1 O12' 79(2) 7_565 . ?
O13 Cl1 O12' 62(5) . . ?
O12 Cl1 O12' 160(5) . . ?
Cl1 O11 Cl1' 35.8(8) . . ?
Cl1' O13 Cl1 41.1(12) . . ?
Cl1' O13 O12' 32(5) . . ?
Cl1 O13 O12' 73(5) . . ?
Cl1 Cl1' O12' 168(10) . . ?
Cl1 Cl1' O13 83.0(18) . . ?
O12' Cl1' O13 109(10) . . ?
Cl1 Cl1' O11 61.6(10) . . ?
O12' Cl1' O11 112(6) . . ?
O13 Cl1' O11 113.3(13) . . ?
Cl1 Cl1' O11 61.6(10) . 7_565 ?
O12' Cl1' O11 112(6) . 7_565 ?
O13 Cl1' O11 113.3(13) . 7_565 ?
O11 Cl1' O11 97.6(14) . 7_565 ?
Cl1' O12' O13 39(7) . . ?
Cl1' O12' Cl1 6(5) . . ?
O13 O12' Cl1 45(4) . . ?
O23 Cl2 O23 110.7(7) . 7_565 ?
O23 Cl2 O21 109.8(3) . . ?
O23 Cl2 O21 109.8(3) 7_565 . ?
O23 Cl2 O22 108.3(3) . . ?
O23 Cl2 O22 108.3(3) 7_565 . ?
O21 Cl2 O22 109.9(4) . . ?
C31 O30 Ni1 123.5(3) . . ?
O30 C31 C32 112.7(5) . . ?
C42 C41 O40 112.5(14) . . ?
C52 C51 O50 113.1(10) . . ?
C62 C61 O60 122.4(9) . . ?
C72 C71 O70 115.5(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.994(3) . ?
Ni1 O3 2.012(3) . ?
Ni1 N2 2.025(4) . ?
Ni1 N1 2.031(4) . ?
Ni1 O30 2.101(3) . ?
Ni1 O4 2.390(2) . ?
O1 C1 1.347(5) . ?
C1 C10 1.402(6) . ?
C1 C2 1.406(7) . ?
C2 C3 1.387(6) . ?
C2 C11 1.518(6) . ?
C3 C4 1.387(8) . ?
C4 C9 1.383(8) . ?
C4 C5 1.551(7) . ?
C5 C6 1.482(10) . ?
C5 C8 1.506(12) . ?
C5 C7 1.511(8) . ?
C9 C10 1.412(7) . ?
C10 C12 1.465(7) . ?
C11 C2 1.518(6) 7_565 ?
C12 N1 1.280(6) . ?
N1 C13 1.472(6) . ?
C13 C14 1.519(7) . ?
C14 O2 1.379(8) . ?
C14 C15 1.517(7) . ?
C15 N2 1.468(6) . ?
N2 C16 1.279(6) . ?
C16 C17 1.452(7) . ?
C17 C18 1.401(6) . ?
C17 C26 1.405(6) . ?
C18 C19 1.379(7) . ?
C19 C24 1.402(7) . ?
C19 C20 1.530(7) . ?
C20 C22 1.502(9) . ?
C20 C21 1.503(9) . ?
C20 C23 1.517(11) . ?
C24 C25 1.382(6) . ?
C25 C26 1.404(6) . ?
C25 C27 1.520(5) . ?
C26 O3 1.346(5) . ?
C27 C25 1.520(5) 7_565 ?
O4 Ni1 2.390(2) 7_565 ?
Cl1 Cl1' 0.90(2) . ?
Cl1 O11 1.362(5) . ?
Cl1 O11 1.362(5) 7_565 ?
Cl1 O13 1.366(9) . ?
Cl1 O12 1.454(10) . ?
Cl1 O12' 1.86(17) . ?
O11 Cl1' 1.535(16) . ?
O13 Cl1' 1.14(2) . ?
O13 O12' 1.72(16) . ?
Cl1' O12' 0.96(16) . ?
Cl1' O11 1.535(16) 7_565 ?
Cl2 O23 1.389(6) . ?
Cl2 O23 1.389(6) 7_565 ?
Cl2 O21 1.402(7) . ?
Cl2 O22 1.443(6) . ?
O30 C31 1.435(6) . ?
C31 C32 1.503(8) . ?
O40 C41 1.52(2) . ?
C41 C42 1.358(18) . ?
C52 C51 1.426(15) . ?
C51 O50 1.440(12) . ?
O60 C61 1.358(11) . ?
C61 C62 1.332(13) . ?
C72 C71 1.419(17) . ?
C71 O70 1.469(13) . ?
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
O40 H40 O22 0.81 2.05 2.850(9) 174.8 .
O4 H4OA O60 0.85 1.87 2.718(7) 174.7 .
O4 H4OB O40 0.86 1.85 2.702(8) 179.6 .
O30 H30 O50 0.85 1.78 2.632(10) 179.6 .
O50 H50 O70 0.86 1.85 2.705(14) 179.8 .
O60 H60 O23 0.99 2.32 3.155(9) 140.9 .
O60 H60 O23 0.99 2.32 3.155(9) 140.9 7_565
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
O3 Ni1 O1 C1 139.3(3) . . . . ?
N2 Ni1 O1 C1 129(4) . . . . ?
N1 Ni1 O1 C1 -40.0(3) . . . . ?
O30 Ni1 O1 C1 50.0(3) . . . . ?
O4 Ni1 O1 C1 -139.5(3) . . . . ?
Ni1 O1 C1 C10 25.9(5) . . . . ?
Ni1 O1 C1 C2 -154.6(3) . . . . ?
O1 C1 C2 C3 177.4(4) . . . . ?
C10 C1 C2 C3 -3.1(6) . . . . ?
O1 C1 C2 C11 -5.5(6) . . . . ?
C10 C1 C2 C11 173.9(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
C11 C2 C3 C4 -177.0(5) . . . . ?
C2 C3 C4 C9 3.4(7) . . . . ?
C2 C3 C4 C5 -179.9(5) . . . . ?
C9 C4 C5 C6 -138.2(7) . . . . ?
C3 C4 C5 C6 45.3(8) . . . . ?
C9 C4 C5 C8 -21.0(9) . . . . ?
C3 C4 C5 C8 162.6(7) . . . . ?
C9 C4 C5 C7 99.3(7) . . . . ?
C3 C4 C5 C7 -77.2(7) . . . . ?
C3 C4 C9 C10 -3.9(7) . . . . ?
C5 C4 C9 C10 179.6(5) . . . . ?
O1 C1 C10 C9 -177.9(4) . . . . ?
C2 C1 C10 C9 2.7(6) . . . . ?
O1 C1 C10 C12 8.7(7) . . . . ?
C2 C1 C10 C12 -170.7(4) . . . . ?
C4 C9 C10 C1 0.9(7) . . . . ?
C4 C9 C10 C12 174.7(4) . . . . ?
C3 C2 C11 C2 94.3(6) . . . 7_565 ?
C1 C2 C11 C2 -82.7(6) . . . 7_565 ?
C1 C10 C12 N1 -15.0(7) . . . . ?
C9 C10 C12 N1 171.5(5) . . . . ?
C10 C12 N1 C13 173.8(4) . . . . ?
C10 C12 N1 Ni1 -13.8(7) . . . . ?
O1 Ni1 N1 C12 32.7(4) . . . . ?
O3 Ni1 N1 C12 16(4) . . . . ?
N2 Ni1 N1 C12 -146.9(4) . . . . ?
O30 Ni1 N1 C12 -55.3(4) . . . . ?
O4 Ni1 N1 C12 113.6(4) . . . . ?
O1 Ni1 N1 C13 -155.2(4) . . . . ?
O3 Ni1 N1 C13 -172(4) . . . . ?
N2 Ni1 N1 C13 25.2(4) . . . . ?
O30 Ni1 N1 C13 116.7(4) . . . . ?
O4 Ni1 N1 C13 -74.3(4) . . . . ?
C12 N1 C13 C14 125.7(5) . . . . ?
Ni1 N1 C13 C14 -46.8(6) . . . . ?
N1 C13 C14 O2 -58.6(6) . . . . ?
N1 C13 C14 C15 68.0(6) . . . . ?
O2 C14 C15 N2 57.3(6) . . . . ?
C13 C14 C15 N2 -69.6(6) . . . . ?
C14 C15 N2 C16 -123.2(5) . . . . ?
C14 C15 N2 Ni1 48.8(5) . . . . ?
O1 Ni1 N2 C16 -23(4) . . . . ?
O3 Ni1 N2 C16 -33.5(4) . . . . ?
N1 Ni1 N2 C16 145.9(4) . . . . ?
O30 Ni1 N2 C16 55.8(4) . . . . ?
O4 Ni1 N2 C16 -114.3(4) . . . . ?
O1 Ni1 N2 C15 165(4) . . . . ?
O3 Ni1 N2 C15 154.8(4) . . . . ?
N1 Ni1 N2 C15 -25.9(4) . . . . ?
O30 Ni1 N2 C15 -115.9(4) . . . . ?
O4 Ni1 N2 C15 73.9(4) . . . . ?
C15 N2 C16 C17 -172.6(5) . . . . ?
Ni1 N2 C16 C17 15.4(7) . . . . ?
N2 C16 C17 C18 -171.8(5) . . . . ?
N2 C16 C17 C26 13.8(8) . . . . ?
C26 C17 C18 C19 0.8(8) . . . . ?
C16 C17 C18 C19 -173.8(5) . . . . ?
C17 C18 C19 C24 3.2(8) . . . . ?
C17 C18 C19 C20 -178.1(6) . . . . ?
C18 C19 C20 C22 -115.7(7) . . . . ?
C24 C19 C20 C22 62.9(8) . . . . ?
C18 C19 C20 C21 7.1(10) . . . . ?
C24 C19 C20 C21 -174.3(7) . . . . ?
C18 C19 C20 C23 125.2(6) . . . . ?
C24 C19 C20 C23 -56.2(7) . . . . ?
C18 C19 C24 C25 -3.2(7) . . . . ?
C20 C19 C24 C25 178.0(5) . . . . ?
C19 C24 C25 C26 -0.9(7) . . . . ?
C19 C24 C25 C27 178.5(4) . . . . ?
C24 C25 C26 O3 -177.1(4) . . . . ?
C27 C25 C26 O3 3.5(6) . . . . ?
C24 C25 C26 C17 5.0(6) . . . . ?
C27 C25 C26 C17 -174.4(4) . . . . ?
C18 C17 C26 O3 177.1(4) . . . . ?
C16 C17 C26 O3 -8.6(7) . . . . ?
C18 C17 C26 C25 -5.0(7) . . . . ?
C16 C17 C26 C25 169.3(4) . . . . ?
C25 C26 O3 Ni1 156.9(3) . . . . ?
C17 C26 O3 Ni1 -25.2(5) . . . . ?
O1 Ni1 O3 C26 -139.8(3) . . . . ?
N2 Ni1 O3 C26 39.8(3) . . . . ?
N1 Ni1 O3 C26 -123(4) . . . . ?
O30 Ni1 O3 C26 -51.8(3) . . . . ?
O4 Ni1 O3 C26 138.9(3) . . . . ?
C24 C25 C27 C25 -96.6(5) . . . 7_565 ?
C26 C25 C27 C25 82.8(6) . . . 7_565 ?
O1 Ni1 O4 Ni1 -45.5(2) . . . 7_565 ?
O3 Ni1 O4 Ni1 46.5(2) . . . 7_565 ?
N2 Ni1 O4 Ni1 132.4(2) . . . 7_565 ?
N1 Ni1 O4 Ni1 -131.3(2) . . . 7_565 ?
O30 Ni1 O4 Ni1 -3.1(7) . . . 7_565 ?
O11 Cl1 O11 Cl1' -78.0(12) 7_565 . . . ?
O13 Cl1 O11 Cl1' 49.2(12) . . . . ?
O12 Cl1 O11 Cl1' 156.1(13) . . . . ?
O12' Cl1 O11 Cl1' -5(5) . . . . ?
O11 Cl1 O13 Cl1' -65.1(4) . . . . ?
O11 Cl1 O13 Cl1' 65.1(4) 7_565 . . . ?
O12 Cl1 O13 Cl1' 180.000(5) . . . . ?
O12' Cl1 O13 Cl1' 0.000(6) . . . . ?
Cl1' Cl1 O13 O12' 0.000(17) . . . . ?
O11 Cl1 O13 O12' -65.1(4) . . . . ?
O11 Cl1 O13 O12' 65.1(4) 7_565 . . . ?
O12 Cl1 O13 O12' 180.000(15) . . . . ?
O11 Cl1 Cl1' O12' -58.8(4) . . . . ?
O11 Cl1 Cl1' O12' 58.8(3) 7_565 . . . ?
O13 Cl1 Cl1' O12' 180.00(13) . . . . ?
O12 Cl1 Cl1' O12' 180.00(13) . . . . ?
O11 Cl1 Cl1' O13 121.2(3) . . . . ?
O11 Cl1 Cl1' O13 -121.2(3) 7_565 . . . ?
O12 Cl1 Cl1' O13 0.000(6) . . . . ?
O12' Cl1 Cl1' O13 180.00(3) . . . . ?
O11 Cl1 Cl1' O11 117.6(6) 7_565 . . . ?
O13 Cl1 Cl1' O11 -121.2(3) . . . . ?
O12 Cl1 Cl1' O11 -121.2(3) . . . . ?
O12' Cl1 Cl1' O11 58.8(3) . . . . ?
O11 Cl1 Cl1' O11 -117.6(6) . . . 7_565 ?
O13 Cl1 Cl1' O11 121.2(3) . . . 7_565 ?
O12 Cl1 Cl1' O11 121.2(3) . . . 7_565 ?
O12' Cl1 Cl1' O11 -58.8(3) . . . 7_565 ?
O12' O13 Cl1' Cl1 180.000(5) . . . . ?
Cl1 O13 Cl1' O12' 180.00(3) . . . . ?
Cl1 O13 Cl1' O11 55.0(13) . . . . ?
O12' O13 Cl1' O11 -125.0(13) . . . . ?
Cl1 O13 Cl1' O11 -55.0(13) . . . 7_565 ?
O12' O13 Cl1' O11 125.0(13) . . . 7_565 ?
Cl1 O11 Cl1' O12' 169(9) . . . . ?
Cl1 O11 Cl1' O13 -67.5(18) . . . . ?
Cl1 O11 Cl1' O11 51.9(9) . . . 7_565 ?
Cl1 Cl1' O12' O13 180.00(16) . . . . ?
O11 Cl1' O12' O13 126(3) . . . . ?
O11 Cl1' O12' O13 -126(3) 7_565 . . . ?
O13 Cl1' O12' Cl1 180.0(3) . . . . ?
O11 Cl1' O12' Cl1 -54(4) . . . . ?
O11 Cl1' O12' Cl1 54(4) 7_565 . . . ?
Cl1 O13 O12' Cl1' 0.00(2) . . . . ?
Cl1' O13 O12' Cl1 0.00(4) . . . . ?
O11 Cl1 O12' Cl1' 120.4(9) . . . . ?
O11 Cl1 O12' Cl1' -120.4(9) 7_565 . . . ?
O13 Cl1 O12' Cl1' 0.00(13) . . . . ?
O12 Cl1 O12' Cl1' 0.00(9) . . . . ?
Cl1' Cl1 O12' O13 0.00(14) . . . . ?
O11 Cl1 O12' O13 120.4(8) . . . . ?
O11 Cl1 O12' O13 -120.4(8) 7_565 . . . ?
O12 Cl1 O12' O13 0.00(2) . . . . ?
O1 Ni1 O30 C31 52.8(4) . . . . ?
O3 Ni1 O30 C31 -37.9(4) . . . . ?
N2 Ni1 O30 C31 -125.1(4) . . . . ?
N1 Ni1 O30 C31 140.0(4) . . . . ?
O4 Ni1 O30 C31 10.9(8) . . . . ?
Ni1 O30 C31 C32 -134.8(4) . . . . ?
