#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:17:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179783 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007943.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_7007943
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 H90 N10 Ni2 O17'
_chemical_formula_weight         1388.88
_chemical_name_systematic
;
?
;
_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                90.00
_cell_angle_beta                 99.6140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3462(5)
_cell_length_b                   31.9837(13)
_cell_length_c                   16.4255(6)
_cell_measurement_reflns_used    8986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.91
_cell_measurement_theta_min      2.22
_cell_volume                     6912.9(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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50389
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.856645
_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       plate
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         12167
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1082P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.1922
_reflns_number_gt                8067
_reflns_number_total             12167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413639j.txt
_cod_data_source_block           Complex6a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               7007943
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 0.08891(4) 0.181465(17) 0.06288(3) 0.02883(16) Uani 1 1 d . . .
Ni2 Ni 0.41083(4) 0.202082(16) 0.00434(3) 0.02859(16) Uani 1 1 d . . .
O1 O 0.16137(19) 0.23782(8) 0.07299(17) 0.0293(6) Uani 1 1 d . . .
C1 C 0.1126(3) 0.27312(13) 0.0904(3) 0.0304(9) Uani 1 1 d . . .
C2 C 0.0094(3) 0.27904(14) 0.0558(3) 0.0334(10) Uani 1 1 d . B .
C3 C -0.0386(3) 0.31588(14) 0.0741(3) 0.0382(11) Uani 1 1 d . . .
H3 H -0.1078 0.3200 0.0504 0.046 Uiso 1 1 calc R . .
C4 C 0.0109(3) 0.34688(14) 0.1258(3) 0.0393(11) Uani 1 1 d . . .
C5 C -0.0471(4) 0.38508(15) 0.1499(3) 0.0460(12) Uani 1 1 d . . .
C6 C -0.1119(5) 0.3711(2) 0.2125(4) 0.083(2) Uani 1 1 d . . .
H6A H -0.1496 0.3951 0.2290 0.125 Uiso 1 1 calc R . .
H6B H -0.0681 0.3596 0.2611 0.125 Uiso 1 1 calc R . .
H6C H -0.1599 0.3496 0.1878 0.125 Uiso 1 1 calc R . .
C7 C -0.1101(6) 0.4047(2) 0.0758(4) 0.088(2) Uani 1 1 d . . .
H7A H -0.0661 0.4130 0.0365 0.132 Uiso 1 1 calc R . .
H7B H -0.1449 0.4294 0.0929 0.132 Uiso 1 1 calc R . .
H7C H -0.1605 0.3845 0.0496 0.132 Uiso 1 1 calc R . .
C8 C 0.0243(5) 0.4181(2) 0.1941(6) 0.104(3) Uani 1 1 d . . .
H8A H 0.0690 0.4284 0.1568 0.156 Uiso 1 1 calc R . .
H8B H 0.0654 0.4058 0.2432 0.156 Uiso 1 1 calc R . .
H8C H -0.0156 0.4414 0.2106 0.156 Uiso 1 1 calc R . .
C9 C 0.1120(3) 0.33947(14) 0.1587(3) 0.0353(10) Uani 1 1 d . . .
H9 H 0.1477 0.3597 0.1947 0.042 Uiso 1 1 calc R . .
C10 C 0.1635(3) 0.30350(13) 0.1411(3) 0.0300(10) Uani 1 1 d . . .
C11 C 0.2738(3) 0.29758(13) 0.1808(2) 0.0279(9) Uani 1 1 d . . .
H11A H 0.2862 0.2675 0.1922 0.034 Uiso 1 1 calc R . .
H11B H 0.2857 0.3125 0.2344 0.034 Uiso 1 1 calc R . .
C12 C 0.3495(3) 0.31328(13) 0.1283(3) 0.0307(10) Uani 1 1 d . C .
C13 C 0.3917(3) 0.35222(13) 0.1424(3) 0.0332(10) Uani 1 1 d . . .
H13 H 0.3729 0.3686 0.1857 0.040 Uiso 1 1 calc R . .
C14 C 0.4623(3) 0.36919(13) 0.0953(3) 0.0347(10) Uani 1 1 d . . .
C15 C 0.5138(3) 0.41116(14) 0.1159(3) 0.0407(11) Uani 1 1 d . . .
C16 C 0.4498(5) 0.44100(18) 0.1585(5) 0.087(2) Uani 1 1 d . . .
H16A H 0.4863 0.4675 0.1701 0.130 Uiso 1 1 calc R . .
H16B H 0.4373 0.4285 0.2103 0.130 Uiso 1 1 calc R . .
H16C H 0.3849 0.4461 0.1223 0.130 Uiso 1 1 calc R . .
C17 C 0.5372(6) 0.4323(2) 0.0377(4) 0.096(3) Uani 1 1 d . . .
H17A H 0.5700 0.4594 0.0521 0.144 Uiso 1 1 calc R . .
H17B H 0.4737 0.4367 -0.0010 0.144 Uiso 1 1 calc R . .
H17C H 0.5827 0.4145 0.0119 0.144 Uiso 1 1 calc R . .
C18 C 0.6141(4) 0.40323(19) 0.1732(5) 0.079(2) Uani 1 1 d . . .
H18A H 0.6487 0.4299 0.1874 0.119 Uiso 1 1 calc R . .
H18B H 0.6572 0.3852 0.1454 0.119 Uiso 1 1 calc R . .
H18C H 0.6008 0.3895 0.2237 0.119 Uiso 1 1 calc R . .
C19 C 0.4842(3) 0.34458(14) 0.0316(3) 0.0360(10) Uani 1 1 d . . .
H19 H 0.5294 0.3551 -0.0024 0.043 Uiso 1 1 calc R . .
C20 C 0.4424(3) 0.30450(13) 0.0148(3) 0.0288(9) Uani 1 1 d . C .
C21 C 0.3746(3) 0.28824(13) 0.0631(3) 0.0320(10) Uani 1 1 d . . .
O2 O 0.3334(2) 0.24994(9) 0.04808(18) 0.0318(7) Uani 1 1 d . C .
C22 C 0.4722(3) 0.28269(14) -0.0557(3) 0.0308(10) Uani 1 1 d . . .
H22 H 0.5062 0.2989 -0.0912 0.037 Uiso 1 1 calc R C .
N1 N 0.4571(2) 0.24411(11) -0.0746(2) 0.0312(8) Uani 1 1 d . C .
C23 C 0.4858(3) 0.23075(14) -0.1534(3) 0.0369(10) Uani 1 1 d . . .
H23A H 0.5228 0.2539 -0.1754 0.044 Uiso 1 1 calc R C .
H23B H 0.4232 0.2254 -0.1937 0.044 Uiso 1 1 calc R . .
C24 C 0.5521(4) 0.19158(16) -0.1465(3) 0.0455(12) Uani 1 1 d . C .
H24 H 0.5699 0.1865 -0.2025 0.055 Uiso 1 1 calc R . .
O3 O 0.6446(3) 0.19736(13) -0.0917(2) 0.0625(11) Uani 1 1 d . . .
C25 C 0.5004(4) 0.15221(16) -0.1227(3) 0.0482(13) Uani 1 1 d . . .
H25A H 0.4336 0.1492 -0.1588 0.058 Uiso 1 1 calc R C .
H25B H 0.5423 0.1276 -0.1315 0.058 Uiso 1 1 calc R . .
N2 N 0.4858(3) 0.15312(12) -0.0368(2) 0.0358(9) Uani 1 1 d . C .
C26 C 0.5280(3) 0.12380(14) 0.0101(3) 0.0376(11) Uani 1 1 d . . .
H26 H 0.5662 0.1037 -0.0144 0.045 Uiso 1 1 calc R C .
C27 C 0.5229(3) 0.11840(13) 0.0970(3) 0.0315(10) Uani 1 1 d . C .
C28 C 0.5989(3) 0.09411(14) 0.1441(3) 0.0377(11) Uani 1 1 d . . .
H28 H 0.6476 0.0808 0.1169 0.045 Uiso 1 1 calc R C .
C29 C 0.6059(3) 0.08877(14) 0.2281(3) 0.0370(11) Uani 1 1 d . C .
C30 C 0.6959(4) 0.06502(18) 0.2771(3) 0.0519(14) Uani 1 1 d . . .
C31 C 0.7929(4) 0.0907(3) 0.2731(4) 0.091(3) Uani 1 1 d . C .
H31A H 0.7864 0.1184 0.2970 0.137 Uiso 1 1 calc R . .
H31B H 0.8021 0.0936 0.2154 0.137 Uiso 1 1 calc R . .
H31C H 0.8519 0.0763 0.3044 0.137 Uiso 1 1 calc R . .
C32 C 0.6858(4) 0.0598(2) 0.3684(3) 0.0617(16) Uani 1 1 d . C .
H32A H 0.6803 0.0874 0.3932 0.093 Uiso 1 1 calc R . .
H32B H 0.7458 0.0453 0.3977 0.093 Uiso 1 1 calc R . .
H32C H 0.6248 0.0434 0.3724 0.093 Uiso 1 1 calc R . .
C33 C 0.7031(6) 0.0214(2) 0.2398(4) 0.094(3) Uani 1 1 d . C .
H33A H 0.6403 0.0059 0.2420 0.141 Uiso 1 1 calc R . .
H33B H 0.7609 0.0063 0.2712 0.141 Uiso 1 1 calc R . .
H33C H 0.7128 0.0241 0.1822 0.141 Uiso 1 1 calc R . .
C34 C 0.5296(3) 0.10771(14) 0.2646(3) 0.0351(10) Uani 1 1 d . . .
H34 H 0.5314 0.1042 0.3223 0.042 Uiso 1 1 calc R C .
C35 C 0.4512(3) 0.13146(12) 0.2202(3) 0.0289(9) Uani 1 1 d . C .
C36 C 0.4481(3) 0.13683(12) 0.1357(3) 0.0286(9) Uani 1 1 d . . .
O4 O 0.3740(2) 0.16027(9) 0.08968(17) 0.0306(7) Uani 1 1 d . C .
C37 C 0.3739(3) 0.15199(13) 0.2657(3) 0.0293(9) Uani 1 1 d . . .
H37A H 0.3559 0.1797 0.2404 0.035 Uiso 1 1 calc R C .
H37B H 0.4062 0.1568 0.3237 0.035 Uiso 1 1 calc R . .
C38 C 0.2766(3) 0.12713(12) 0.2653(2) 0.0272(9) Uani 1 1 d . C .
C39 C 0.2633(3) 0.10367(12) 0.3331(3) 0.0286(9) Uani 1 1 d . . .
H39 H 0.3159 0.1035 0.3799 0.034 Uiso 1 1 calc R C .
C40 C 0.1749(3) 0.07989(13) 0.3359(3) 0.0320(10) Uani 1 1 d . C .
C41 C 0.1658(3) 0.05507(15) 0.4151(3) 0.0383(11) Uani 1 1 d . . .
C42 C 0.1847(4) 0.08397(17) 0.4896(3) 0.0504(13) Uani 1 1 d . C .
H42A H 0.2521 0.0967 0.4936 0.076 Uiso 1 1 calc R . .
H42B H 0.1813 0.0679 0.5398 0.076 Uiso 1 1 calc R . .
H42C H 0.1328 0.1059 0.4834 0.076 Uiso 1 1 calc R . .
C43 C 0.2462(4) 0.02010(16) 0.4244(3) 0.0538(14) Uani 1 1 d . C .
H43A H 0.3140 0.0325 0.4286 0.081 Uiso 1 1 calc R . .
H43B H 0.2334 0.0016 0.3762 0.081 Uiso 1 1 calc R . .
H43C H 0.2422 0.0039 0.4745 0.081 Uiso 1 1 calc R . .
C44 C 0.0603(4) 0.03491(17) 0.4095(3) 0.0518(14) Uani 1 1 d . C .
H44A H 0.0478 0.0163 0.3615 0.078 Uiso 1 1 calc R . .
H44B H 0.0082 0.0568 0.4037 0.078 Uiso 1 1 calc R . .
H44C H 0.0575 0.0188 0.4598 0.078 Uiso 1 1 calc R . .
C45 C 0.1018(3) 0.08028(13) 0.2659(3) 0.0337(10) Uani 1 1 d . . .
H45 H 0.0427 0.0637 0.2652 0.040 Uiso 1 1 calc R C .
C46 C 0.1104(3) 0.10407(13) 0.1952(3) 0.0301(9) Uani 1 1 d . C .
C47 C 0.1987(3) 0.12844(13) 0.1959(3) 0.0280(9) Uani 1 1 d . . .
O5 O 0.2083(2) 0.15359(9) 0.13257(17) 0.0314(7) Uani 1 1 d . C .
C48 C 0.0305(3) 0.10099(14) 0.1235(3) 0.0356(10) Uani 1 1 d . . .
H48 H -0.0154 0.0782 0.1228 0.043 Uiso 1 1 calc R C .
N3 N 0.0153(2) 0.12543(11) 0.0617(2) 0.0309(8) Uani 1 1 d . B .
C49 C -0.0624(3) 0.11363(15) -0.0081(3) 0.0433(12) Uani 1 1 d . . .
H49A H -0.0991 0.0887 0.0073 0.052 Uiso 1 1 calc R A 1
H49B H -0.0288 0.1058 -0.0553 0.052 Uiso 1 1 calc R A 1
C50 C -0.1388(3) 0.14816(17) -0.0352(3) 0.0477(13) Uani 0.50 1 d P B 1
H50 H -0.1656 0.1574 0.0152 0.057 Uiso 0.50 1 calc PR B 1
O6 O -0.2192(5) 0.1324(2) -0.0886(5) 0.0546(19) Uani 0.50 1 d P B 1
C50' C -0.1388(3) 0.14816(17) -0.0352(3) 0.0477(13) Uani 0.50 1 d P B 2
H50' H -0.1845 0.1358 -0.0836 0.057 Uiso 0.50 1 calc PR B 2
O6' O -0.1987(5) 0.1545(2) 0.0184(4) 0.056(2) Uani 0.50 1 d P B 2
C51 C -0.0948(3) 0.18707(15) -0.0710(3) 0.0421(12) Uani 1 1 d . . .
H51A H -0.0566 0.1784 -0.1149 0.050 Uiso 1 1 calc R B 1
H51B H -0.1513 0.2054 -0.0964 0.050 Uiso 1 1 calc R B 1
N4 N -0.0277(3) 0.21052(12) -0.0082(2) 0.0334(8) Uani 1 1 d . B .
C52 C -0.0499(3) 0.24916(15) 0.0018(3) 0.0368(11) Uani 1 1 d . . .
H52 H -0.1116 0.2591 -0.0296 0.044 Uiso 1 1 calc R B .
N11 N 0.1985(3) 0.17805(16) -0.0918(3) 0.0569(12) Uani 1 1 d . . .
O11 O 0.1622(4) 0.16439(12) -0.0347(3) 0.0731(13) Uani 1 1 d . C .
O12 O 0.2857(2) 0.19124(11) -0.0908(2) 0.0479(9) Uani 1 1 d . C .
O13 O 0.1284(5) 0.1880(2) -0.1494(4) 0.139(2) Uani 1 1 d . C .
O61 O 0.0314(2) 0.19576(9) 0.17278(17) 0.0322(7) Uani 1 1 d D . .
C61 C 0.0931(3) 0.20612(13) 0.2348(3) 0.0314(10) Uani 1 1 d D . .
H61 H 0.1541 0.2193 0.2258 0.038 Uiso 1 1 calc R . .
N61 N 0.0811(3) 0.20041(11) 0.3114(2) 0.0331(8) Uani 1 1 d D . .
C62 C 0.1575(4) 0.21272(16) 0.3814(3) 0.0463(12) Uani 1 1 d D . .
H62A H 0.1336 0.2056 0.4329 0.069 Uiso 1 1 calc R . .
H62B H 0.1691 0.2429 0.3793 0.069 Uiso 1 1 calc R . .
H62C H 0.2211 0.1979 0.3789 0.069 Uiso 1 1 calc R . .
C63 C -0.0083(4) 0.17850(17) 0.3318(3) 0.0484(13) Uani 1 1 d D . .
H63A H -0.0038 0.1772 0.3919 0.073 Uiso 1 1 calc R . .
H63B H -0.0106 0.1501 0.3093 0.073 Uiso 1 1 calc R . .
H63C H -0.0700 0.1936 0.3076 0.073 Uiso 1 1 calc R . .
O71 O 0.5332(2) 0.21832(10) 0.09455(18) 0.0381(7) Uani 0.70 1 d PD C 1
C71 C 0.6215(5) 0.2137(3) 0.1079(5) 0.0419(18) Uani 0.70 1 d PD C 1
H71 H 0.6444 0.1906 0.0796 0.050 Uiso 0.70 1 calc PR C 1
N71 N 0.6938(3) 0.23385(12) 0.1536(2) 0.0400(9) Uani 0.70 1 d PD C 1
C72 C 0.7992(5) 0.2265(3) 0.1661(6) 0.065(2) Uani 0.70 1 d PD C 1
H72A H 0.8132 0.2014 0.1357 0.098 Uiso 0.70 1 calc PR C 1
H72B H 0.8242 0.2224 0.2251 0.098 Uiso 0.70 1 calc PR C 1
H72C H 0.8337 0.2505 0.1461 0.098 Uiso 0.70 1 calc PR C 1
C73 C 0.6645(6) 0.2770(3) 0.1804(6) 0.069(2) Uani 0.70 1 d PD C 1
H73A H 0.6916 0.2983 0.1472 0.104 Uiso 0.70 1 calc PR C 1
H73B H 0.6928 0.2812 0.2389 0.104 Uiso 0.70 1 calc PR C 1
H73C H 0.5903 0.2793 0.1727 0.104 Uiso 0.70 1 calc PR C 1
O71' O 0.5332(2) 0.21832(10) 0.09455(18) 0.0381(7) Uani 0.30 1 d PD C 2
C71' C 0.6122(8) 0.2383(4) 0.1022(9) 0.027(4) Uani 0.30 1 d PD C 2
H71' H 0.6126 0.2605 0.0639 0.033 Uiso 0.30 1 calc PR C 2
N71' N 0.6938(3) 0.23385(12) 0.1536(2) 0.0400(9) Uani 0.30 1 d PD C 2
C72' C 0.7107(14) 0.1940(6) 0.2040(14) 0.086(9) Uani 0.30 1 d PD C 2
H72D H 0.6504 0.1761 0.1914 0.130 Uiso 0.30 1 calc PR C 2
H72E H 0.7228 0.2009 0.2629 0.130 Uiso 0.30 1 calc PR C 2
H72F H 0.7698 0.1791 0.1901 0.130 Uiso 0.30 1 calc PR C 2
C73' C 0.7865(11) 0.2592(6) 0.1686(15) 0.067(7) Uani 0.30 1 d PD C 2
H73D H 0.8452 0.2417 0.1629 0.101 Uiso 0.30 1 calc PR C 2
H73E H 0.7954 0.2708 0.2246 0.101 Uiso 0.30 1 calc PR C 2
H73F H 0.7811 0.2821 0.1284 0.101 Uiso 0.30 1 calc PR C 2
N22 N 0.7119(4) 0.3018(3) -0.0751(5) 0.0808(19) Uani 1 1 d . . .
O21 O 0.7053(4) 0.2798(4) -0.0240(5) 0.210(5) Uani 1 1 d . . .
O22 O 0.7248(6) 0.2808(3) -0.1354(5) 0.173(4) Uani 1 1 d . . .
O23 O 0.7006(7) 0.3354(2) -0.0718(9) 0.229(6) Uani 1 1 d . . .
O81 O 0.5699(7) 0.4566(2) 0.3789(4) 0.148(3) Uani 1 1 d . . .
C81 C 0.6692(8) 0.4547(3) 0.3799(7) 0.128(4) Uani 1 1 d . . .
H81 H 0.7116 0.4328 0.4050 0.153 Uiso 1 1 calc R . .
N81 N 0.7028(4) 0.48758(15) 0.3409(3) 0.0707(15) Uani 1 1 d . . .
C82 C 0.6520(6) 0.5244(2) 0.3052(5) 0.085(2) Uani 1 1 d . . .
H82A H 0.5802 0.5233 0.3112 0.127 Uiso 1 1 calc R . .
H82B H 0.6574 0.5258 0.2465 0.127 Uiso 1 1 calc R . .
H82C H 0.6837 0.5492 0.3336 0.127 Uiso 1 1 calc R . .
C83 C 0.8130(6) 0.4844(3) 0.3363(5) 0.099(2) Uani 1 1 d . . .
H83A H 0.8504 0.5059 0.3715 0.148 Uiso 1 1 calc R . .
H83B H 0.8230 0.4886 0.2791 0.148 Uiso 1 1 calc R . .
H83C H 0.8381 0.4567 0.3553 0.148 Uiso 1 1 calc R . .
H2 H 0.2949 0.1550 0.1013 0.040 Uiso 1 1 d . . .
H1 H 0.2333 0.2413 0.0593 0.040 Uiso 1 1 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
O5 Ni1 N4 178.28(13) . . ?
O5 Ni1 O1 91.47(11) . . ?
N4 Ni1 O1 87.09(13) . . ?
O5 Ni1 N3 87.16(12) . . ?
N4 Ni1 N3 94.34(14) . . ?
O1 Ni1 N3 175.80(13) . . ?
O5 Ni1 O11 83.84(15) . . ?
N4 Ni1 O11 95.24(16) . . ?
O1 Ni1 O11 90.99(13) . . ?
N3 Ni1 O11 92.81(15) . . ?
O5 Ni1 O61 88.63(11) . . ?
N4 Ni1 O61 92.27(12) . . ?
O1 Ni1 O61 88.52(11) . . ?
N3 Ni1 O61 87.48(13) . . ?
O11 Ni1 O61 172.44(15) . . ?
N2 Ni2 N1 94.50(14) . . ?
N2 Ni2 O2 178.10(13) . . ?
N1 Ni2 O2 87.39(12) . . ?
N2 Ni2 O4 84.97(13) . . ?
N1 Ni2 O4 175.83(12) . . ?
O2 Ni2 O4 93.17(11) . . ?
N2 Ni2 O71 93.32(14) . . ?
N1 Ni2 O71 90.19(13) . . ?
O2 Ni2 O71 86.86(12) . . ?
O4 Ni2 O71 85.71(11) . . ?
N2 Ni2 O12 89.97(14) . . ?
N1 Ni2 O12 85.62(13) . . ?
O2 Ni2 O12 89.98(12) . . ?
O4 Ni2 O12 98.51(12) . . ?
O71 Ni2 O12 174.87(13) . . ?
C1 O1 Ni1 121.0(2) . . ?
O1 C1 C10 120.5(4) . . ?
O1 C1 C2 119.8(4) . . ?
C10 C1 C2 119.8(4) . . ?
C3 C2 C1 118.5(4) . . ?
C3 C2 C52 117.8(4) . . ?
C1 C2 C52 123.7(4) . . ?
C4 C3 C2 122.8(4) . . ?
C9 C4 C3 116.5(4) . . ?
C9 C4 C5 122.3(4) . . ?
C3 C4 C5 121.0(4) . . ?
C7 C5 C6 111.6(5) . . ?
C7 C5 C8 108.6(5) . . ?
C6 C5 C8 105.3(6) . . ?
C7 C5 C4 111.3(4) . . ?
C6 C5 C4 108.1(4) . . ?
C8 C5 C4 111.9(4) . . ?
C4 C9 C10 122.7(4) . . ?
C1 C10 C9 119.7(4) . . ?
C1 C10 C11 121.0(4) . . ?
C9 C10 C11 119.3(4) . . ?
C10 C11 C12 113.8(3) . . ?
C13 C12 C21 119.8(4) . . ?
C13 C12 C11 119.8(4) . . ?
C21 C12 C11 120.3(4) . . ?
C12 C13 C14 123.0(4) . . ?
C19 C14 C13 116.0(4) . . ?
C19 C14 C15 121.8(4) . . ?
C13 C14 C15 122.1(4) . . ?
C14 C15 C18 108.0(4) . . ?
C14 C15 C16 112.8(4) . . ?
C18 C15 C16 108.8(5) . . ?
C14 C15 C17 110.6(4) . . ?
C18 C15 C17 108.2(5) . . ?
C16 C15 C17 108.4(5) . . ?
C14 C19 C20 122.8(4) . . ?
C21 C20 C19 120.1(4) . . ?
C21 C20 C22 124.0(4) . . ?
C19 C20 C22 116.0(4) . . ?
O2 C21 C20 121.1(4) . . ?
O2 C21 C12 120.6(4) . . ?
C20 C21 C12 118.3(4) . . ?
C21 O2 Ni2 122.0(2) . . ?
N1 C22 C20 126.8(4) . . ?
C22 N1 C23 116.1(4) . . ?
C22 N1 Ni2 122.3(3) . . ?
C23 N1 Ni2 121.3(3) . . ?
N1 C23 C24 113.9(4) . . ?
O3 C24 C25 109.3(4) . . ?
O3 C24 C23 111.9(4) . . ?
C25 C24 C23 114.7(4) . . ?
N2 C25 C24 112.0(4) . . ?
C26 N2 C25 116.7(4) . . ?
C26 N2 Ni2 123.7(3) . . ?
C25 N2 Ni2 119.4(3) . . ?
N2 C26 C27 126.1(4) . . ?
C36 C27 C28 119.2(4) . . ?
C36 C27 C26 123.4(4) . . ?
C28 C27 C26 117.4(4) . . ?
C29 C28 C27 122.9(4) . . ?
C28 C29 C34 116.2(4) . . ?
C28 C29 C30 120.3(4) . . ?
C34 C29 C30 123.5(4) . . ?
C29 C30 C33 109.7(5) . . ?
C29 C30 C32 112.2(4) . . ?
C33 C30 C32 108.3(5) . . ?
C29 C30 C31 107.7(4) . . ?
C33 C30 C31 110.9(5) . . ?
C32 C30 C31 108.1(5) . . ?
C35 C34 C29 123.1(4) . . ?
C36 C35 C34 118.8(4) . . ?
C36 C35 C37 121.8(4) . . ?
C34 C35 C37 119.3(4) . . ?
O4 C36 C35 121.2(4) . . ?
O4 C36 C27 119.0(4) . . ?
C35 C36 C27 119.7(4) . . ?
C36 O4 Ni2 120.1(2) . . ?
C35 C37 C38 114.9(3) . . ?
C39 C38 C47 119.5(4) . . ?
C39 C38 C37 120.4(4) . . ?
C47 C38 C37 120.1(4) . . ?
C38 C39 C40 122.7(4) . . ?
C45 C40 C39 116.6(4) . . ?
C45 C40 C41 124.3(4) . . ?
C39 C40 C41 119.1(4) . . ?
C42 C41 C44 109.2(4) . . ?
C42 C41 C43 110.0(4) . . ?
C44 C41 C43 108.5(4) . . ?
C42 C41 C40 109.8(4) . . ?
C44 C41 C40 111.4(4) . . ?
C43 C41 C40 107.8(4) . . ?
C40 C45 C46 123.3(4) . . ?
C45 C46 C47 118.3(4) . . ?
C45 C46 C48 118.8(4) . . ?
C47 C46 C48 122.8(4) . . ?
O5 C47 C38 119.5(4) . . ?
O5 C47 C46 121.0(4) . . ?
C38 C47 C46 119.5(4) . . ?
C47 O5 Ni1 122.7(2) . . ?
N3 C48 C46 127.1(4) . . ?
C48 N3 C49 117.7(4) . . ?
C48 N3 Ni1 121.3(3) . . ?
C49 N3 Ni1 120.8(3) . . ?
N3 C49 C50 113.3(4) . . ?
O6 C50 C49 109.7(5) . . ?
O6 C50 C51 111.3(5) . . ?
C49 C50 C51 114.9(4) . . ?
N4 C51 C50 112.1(4) . . ?
C52 N4 C51 117.2(4) . . ?
C52 N4 Ni1 122.8(3) . . ?
C51 N4 Ni1 119.9(3) . . ?
N4 C52 C2 126.7(4) . . ?
O11 N11 O12 127.8(5) . . ?
O11 N11 O13 109.3(5) . . ?
O12 N11 O13 120.4(5) . . ?
N11 O11 Ni1 143.4(4) . . ?
N11 O12 Ni2 133.7(3) . . ?
C61 O61 Ni1 118.1(3) . . ?
O61 C61 N61 125.5(4) . . ?
C61 N61 C62 122.6(4) . . ?
C61 N61 C63 121.3(4) . . ?
C62 N61 C63 115.9(4) . . ?
C71 O71 Ni2 138.3(4) . . ?
O71 C71 N71 132.5(7) . . ?
C71 N71 C72 129.2(6) . . ?
C71 N71 C73 114.8(5) . . ?
C72 N71 C73 114.1(6) . . ?
O23 N22 O21 124.0(13) . . ?
O23 N22 O22 128.2(11) . . ?
O21 N22 O22 107.5(11) . . ?
O81 C81 N81 111.7(11) . . ?
C81 N81 C82 131.6(7) . . ?
C81 N81 C83 112.4(7) . . ?
C82 N81 C83 116.0(6) . . ?
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 O5 2.009(3) . ?
Ni1 N4 2.010(4) . ?
Ni1 O1 2.039(3) . ?
Ni1 N3 2.042(3) . ?
Ni1 O11 2.085(4) . ?
Ni1 O61 2.126(3) . ?
Ni2 N2 2.033(4) . ?
Ni2 N1 2.034(4) . ?
Ni2 O2 2.043(3) . ?
Ni2 O4 2.055(3) . ?
Ni2 O71 2.079(3) . ?
Ni2 O12 2.117(3) . ?
O1 C1 1.358(5) . ?
C1 C10 1.382(6) . ?
C1 C2 1.412(6) . ?
C2 C3 1.397(6) . ?
C2 C52 1.446(6) . ?
C3 C4 1.397(7) . ?
C4 C9 1.388(6) . ?
C4 C5 1.533(6) . ?
C5 C7 1.496(8) . ?
C5 C6 1.517(7) . ?
C5 C8 1.522(9) . ?
C9 C10 1.395(6) . ?
C10 C11 1.519(5) . ?
C11 C12 1.520(6) . ?
C12 C13 1.370(6) . ?
C12 C21 1.421(6) . ?
C13 C14 1.423(6) . ?
C14 C19 1.379(6) . ?
C14 C15 1.520(6) . ?
C15 C18 1.523(7) . ?
C15 C16 1.526(7) . ?
C15 C17 1.529(7) . ?
C19 C20 1.407(6) . ?
C20 C21 1.398(6) . ?
C20 C22 1.463(6) . ?
C21 O2 1.348(5) . ?
C22 N1 1.280(5) . ?
N1 C23 1.473(5) . ?
C23 C24 1.527(6) . ?
C24 O3 1.414(6) . ?
C24 C25 1.518(7) . ?
C25 N2 1.457(6) . ?
N2 C26 1.282(6) . ?
C26 C27 1.452(6) . ?
C27 C36 1.400(6) . ?
C27 C28 1.403(6) . ?
C28 C29 1.378(6) . ?
C29 C34 1.402(6) . ?
C29 C30 1.531(6) . ?
C30 C33 1.534(9) . ?
C30 C32 1.536(7) . ?
C30 C31 1.543(8) . ?
C34 C35 1.396(6) . ?
C35 C36 1.392(6) . ?
C35 C37 1.519(6) . ?
C36 O4 1.365(5) . ?
C37 C38 1.522(6) . ?
C38 C39 1.379(6) . ?
C38 C47 1.410(6) . ?
C39 C40 1.412(6) . ?
C40 C45 1.378(6) . ?
C40 C41 1.545(6) . ?
C41 C42 1.521(7) . ?
C41 C44 1.538(6) . ?
C41 C43 1.539(6) . ?
C45 C46 1.408(6) . ?
C46 C47 1.411(6) . ?
C46 C48 1.455(6) . ?
C47 O5 1.338(5) . ?
C48 N3 1.271(5) . ?
N3 C49 1.462(5) . ?
C49 C50 1.518(7) . ?
C50 O6 1.364(7) . ?
C50 C51 1.534(7) . ?
C51 N4 1.456(6) . ?
N4 C52 1.288(6) . ?
N11 O11 1.207(5) . ?
N11 O12 1.236(5) . ?
N11 O13 1.254(7) . ?
O61 C61 1.243(5) . ?
C61 N61 1.308(5) . ?
N61 C62 1.457(5) . ?
N61 C63 1.469(5) . ?
O71 C71 1.172(7) . ?
C71 N71 1.292(7) . ?
N71 C72 1.407(7) . ?
N71 C73 1.520(8) . ?
N22 O23 1.089(9) . ?
N22 O21 1.110(9) . ?
N22 O22 1.232(9) . ?
O81 C81 1.325(11) . ?
C81 N81 1.346(10) . ?
N81 C82 1.433(8) . ?
N81 C83 1.489(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
O1 H1 O2 1.03 1.41 2.430(4) 172.9 .
O4 H2 O5 1.12 1.34 2.440(4) 166.0 .
