#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/95/7009547.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_7009547
loop_
_publ_author_name
'He Cheng'
'Duan Chun-ying'
'Fang Chen-jie'
'Meng Qing-jin'
_publ_section_title
;
 Self-assembled dinuclear molecular box [Ag2L2]2+ and triple helicates
 [Co2L3]4+,
 [Ni2L3]4+{L = bis[4-(2-pyridylmethyleneamino)phenyl]
 ether}
;
_journal_issue                   14
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2419
_journal_page_last               2424
_journal_paper_doi               10.1039/b001820l
_journal_year                    2000
_chemical_formula_sum            'C74.5 H59 B4 F16 N13 Ni2 O3.5'
_chemical_formula_weight         1657.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.71(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.723(8)
_cell_length_b                   18.472(6)
_cell_length_c                   20.184(9)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.89
_cell_measurement_theta_min      4.50
_cell_volume                     7815(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_sigmaI/netI    0.1597
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7408
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        5.09
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.576
_exptl_crystal_colour            'orange                 '
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate                 '
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1892
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0603P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                2816
_reflns_number_total             6952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001820l.txt
_cod_data_source_block           Ni1
_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_cell_volume        7815(5)
_cod_original_sg_symbol_H-M      'Cc   '
_cod_original_formula_sum        'C74.50 H59 B4 F16 N13 Ni2 O3.50'
_cod_database_code               7009547
loop_
_symmetry_equiv_pos_as_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'
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 0.07680(6) 1.19105(7) 0.26320(7) 0.0736(4) Uani 1 1 d . . .
Ni2 Ni 0.45851(6) 0.82377(8) 0.65148(7) 0.0784(5) Uani 1 1 d . . .
N1 N -0.0110(4) 1.2056(4) 0.2730(4) 0.071(3) Uani 1 1 d . . .
N2 N 0.1043(4) 1.2009(4) 0.3754(4) 0.063(2) Uani 1 1 d . . .
N3 N 0.4873(3) 0.9318(4) 0.6309(4) 0.062(2) Uani 1 1 d . . .
N4 N 0.5519(4) 0.8035(6) 0.6516(5) 0.090(3) Uani 1 1 d . . .
N5 N 0.0349(4) 1.1811(5) 0.1489(4) 0.085(3) Uani 1 1 d . . .
N6 N 0.0569(4) 1.0760(4) 0.2463(4) 0.077(3) Uani 1 1 d . . .
N7 N 0.3704(4) 0.8552(4) 0.6633(4) 0.062(3) Uani 1 1 d . . .
N8 N 0.4914(4) 0.8474(5) 0.7631(4) 0.068(3) Uani 1 1 d . . .
N9 N 0.1075(4) 1.3002(5) 0.2622(4) 0.069(3) Uani 1 1 d . . .
N10 N 0.1697(4) 1.1788(5) 0.2616(4) 0.061(2) Uani 1 1 d . . .
N11 N 0.4048(4) 0.7851(4) 0.5439(4) 0.069(3) Uani 1 1 d . . .
N12 N 0.4408(4) 0.7123(5) 0.6686(4) 0.073(3) Uani 1 1 d . . .
C1 C -0.0708(6) 1.2032(7) 0.2194(6) 0.098(4) Uani 1 1 d . . .
H1A H -0.0750 1.1992 0.1719 0.118 Uiso 1 1 calc R . .
C2 C -0.1242(6) 1.2066(7) 0.2346(7) 0.100(4) Uani 1 1 d . . .
H2A H -0.1638 1.2039 0.1967 0.120 Uiso 1 1 calc R . .
C3 C -0.1228(6) 1.2134(6) 0.2986(7) 0.105(4) Uani 1 1 d . . .
H3A H -0.1599 1.2176 0.3075 0.126 Uiso 1 1 calc R . .
C4 C -0.0601(6) 1.2141(6) 0.3562(6) 0.094(4) Uani 1 1 d . . .
H4A H -0.0550 1.2154 0.4041 0.113 Uiso 1 1 calc R . .
C5 C -0.0094(5) 1.2127(6) 0.3367(6) 0.073(3) Uani 1 1 d . . .
C6 C 0.0580(5) 1.2116(5) 0.3946(5) 0.070(3) Uani 1 1 d . . .
H6A H 0.0650 1.2186 0.4427 0.084 Uiso 1 1 calc R . .
C7 C 0.1657(5) 1.1987(5) 0.4333(4) 0.070(3) Uani 1 1 d . . .
C8 C 0.2118(6) 1.2524(6) 0.4403(6) 0.100(5) Uani 1 1 d . . .
H8A H 0.2021 1.2909 0.4082 0.120 Uiso 1 1 calc R . .
C9 C 0.2715(7) 1.2477(6) 0.4947(6) 0.116(6) Uani 1 1 d . . .
H9A H 0.2994 1.2867 0.5033 0.139 Uiso 1 1 calc R . .
C10 C 0.2895(5) 1.1899(6) 0.5342(5) 0.080(4) Uani 1 1 d . . .
C11 C 0.2449(6) 1.1348(7) 0.5296(8) 0.132(6) Uani 1 1 d . . .
H11A H 0.2563 1.0959 0.5613 0.159 Uiso 1 1 calc R . .
C12 C 0.1835(6) 1.1399(6) 0.4763(7) 0.122(6) Uani 1 1 d . . .
H12A H 0.1546 1.1024 0.4704 0.147 Uiso 1 1 calc R . .
C13 C 0.3827(5) 1.1260(6) 0.5984(6) 0.083(4) Uani 1 1 d . . .
C14 C 0.3989(5) 1.0894(5) 0.6599(6) 0.078(4) Uani 1 1 d . . .
H14A H 0.3871 1.1070 0.6962 0.094 Uiso 1 1 calc R . .
C15 C 0.4342(5) 1.0239(6) 0.6705(5) 0.071(3) Uani 1 1 d . . .
H15A H 0.4460 0.9993 0.7139 0.085 Uiso 1 1 calc R . .
C16 C 0.4503(5) 0.9977(5) 0.6177(5) 0.060(3) Uani 1 1 d . . .
C17 C 0.4334(6) 1.0360(6) 0.5547(6) 0.091(4) Uani 1 1 d . . .
H17A H 0.4465 1.0193 0.5190 0.109 Uiso 1 1 calc R . .
C18 C 0.3981(6) 1.0978(7) 0.5429(6) 0.101(5) Uani 1 1 d . . .
H18A H 0.3845 1.1210 0.4986 0.121 Uiso 1 1 calc R . .
C19 C 0.5391(5) 0.9331(6) 0.6227(5) 0.079(4) Uani 1 1 d . . .
H19A H 0.5525 0.9760 0.6088 0.094 Uiso 1 1 calc R . .
C20 C 0.5800(6) 0.8667(7) 0.6347(6) 0.092(4) Uani 1 1 d . . .
C21 C 0.6360(6) 0.8627(11) 0.6286(8) 0.143(7) Uani 1 1 d . . .
H21A H 0.6547 0.9039 0.6185 0.172 Uiso 1 1 calc R . .
C22 C 0.6675(6) 0.7933(11) 0.6378(9) 0.164(8) Uani 1 1 d . . .
H22A H 0.7056 0.7874 0.6312 0.197 Uiso 1 1 calc R . .
C23 C 0.6382(8) 0.7363(10) 0.6568(8) 0.155(7) Uani 1 1 d . . .
H23A H 0.6590 0.6919 0.6674 0.186 Uiso 1 1 calc R . .
C24 C 0.5834(5) 0.7423(8) 0.6603(6) 0.102(5) Uani 1 1 d . . .
H24A H 0.5648 0.7007 0.6696 0.123 Uiso 1 1 calc R . .
C25 C 0.0265(5) 1.2352(7) 0.1026(5) 0.094(4) Uani 1 1 d . . .
H25A H 0.0359 1.2821 0.1203 0.113 Uiso 1 1 calc R . .
C26 C 0.0047(8) 1.2247(9) 0.0298(7) 0.146(7) Uani 1 1 d . . .
H26A H 0.0006 1.2625 -0.0022 0.175 Uiso 1 1 calc R . .
C27 C -0.0113(9) 1.1517(11) 0.0065(8) 0.191(10) Uani 1 1 d . . .
H27A H -0.0268 1.1408 -0.0423 0.230 Uiso 1 1 calc R . .
C28 C -0.0043(8) 1.0986(7) 0.0543(6) 0.141(7) Uani 1 1 d . . .
H28A H -0.0162 1.0515 0.0386 0.169 Uiso 1 1 calc R . .
C29 C 0.0198(7) 1.1136(6) 0.1247(6) 0.106(5) Uani 1 1 d . . .
C30 C 0.0335(5) 1.0610(6) 0.1775(5) 0.079(4) Uani 1 1 d . . .
H30A H 0.0257 1.0128 0.1635 0.095 Uiso 1 1 calc R . .
C31 C 0.0719(4) 1.0152(6) 0.2960(5) 0.064(3) Uani 1 1 d . . .
C32 C 0.0573(5) 1.0218(5) 0.3561(5) 0.073(4) Uani 1 1 d . . .
H32A H 0.0372 1.0632 0.3632 0.088 Uiso 1 1 calc R . .
C33 C 0.0733(5) 0.9653(6) 0.4062(5) 0.072(3) Uani 1 1 d . . .
H33A H 0.0612 0.9673 0.4453 0.087 Uiso 1 1 calc R . .
C34 C 0.1079(5) 0.9051(6) 0.3972(5) 0.067(3) Uani 1 1 d . . .
C35 C 0.1206(5) 0.8987(6) 0.3387(6) 0.077(4) Uani 1 1 d . . .
H35A H 0.1403 0.8570 0.3314 0.092 Uiso 1 1 calc R . .
C36 C 0.1044(4) 0.9558(6) 0.2863(5) 0.063(3) Uani 1 1 d . . .
H36A H 0.1156 0.9528 0.2467 0.076 Uiso 1 1 calc R . .
C37 C 0.1869(5) 0.8548(6) 0.5040(5) 0.079(4) Uani 1 1 d . . .
C38 C 0.2055(5) 0.7988(5) 0.5495(5) 0.071(3) Uani 1 1 d . . .
H38A H 0.1772 0.7608 0.5448 0.085 Uiso 1 1 calc R . .
C39 C 0.2647(5) 0.7962(6) 0.6021(5) 0.076(4) Uani 1 1 d . . .
H39A H 0.2772 0.7566 0.6329 0.091 Uiso 1 1 calc R . .
C40 C 0.3079(4) 0.8554(6) 0.6098(5) 0.066(3) Uani 1 1 d . . .
C41 C 0.2880(5) 0.9115(6) 0.5618(5) 0.078(4) Uani 1 1 d . . .
H41A H 0.3158 0.9496 0.5652 0.093 Uiso 1 1 calc R . .
C42 C 0.2280(5) 0.9127(6) 0.5088(6) 0.079(4) Uani 1 1 d . . .
H42A H 0.2148 0.9511 0.4767 0.095 Uiso 1 1 calc R . .
C43 C 0.3782(5) 0.8631(6) 0.7262(6) 0.074(3) Uani 1 1 d . . .
H43A H 0.3425 0.8682 0.7377 0.089 Uiso 1 1 calc R . .
C44 C 0.4439(5) 0.8650(5) 0.7864(5) 0.066(3) Uani 1 1 d . . .
C45 C 0.4542(6) 0.8811(7) 0.8553(6) 0.098(4) Uani 1 1 d . . .
H45A H 0.4205 0.8929 0.8686 0.118 Uiso 1 1 calc R . .
C46 C 0.5147(6) 0.8797(8) 0.9041(7) 0.113(5) Uani 1 1 d . . .
H46A H 0.5227 0.8903 0.9519 0.135 Uiso 1 1 calc R . .
C47 C 0.5649(7) 0.8629(8) 0.8849(6) 0.111(5) Uani 1 1 d . . .
H47A H 0.6068 0.8620 0.9183 0.133 Uiso 1 1 calc R . .
C48 C 0.5498(5) 0.8473(7) 0.8135(7) 0.100(5) Uani 1 1 d . . .
H48A H 0.5833 0.8359 0.7995 0.120 Uiso 1 1 calc R . .
C49 C 0.0752(6) 1.3632(6) 0.2691(6) 0.088(4) Uani 1 1 d . . .
H49A H 0.0357 1.3591 0.2726 0.105 Uiso 1 1 calc R . .
C50 C 0.1012(7) 1.4304(6) 0.2708(6) 0.107(6) Uani 1 1 d . . .
H50A H 0.0805 1.4713 0.2778 0.128 Uiso 1 1 calc R . .
C51 C 0.1592(7) 1.4375(7) 0.2620(7) 0.117(6) Uani 1 1 d . . .
H51A H 0.1755 1.4831 0.2595 0.141 Uiso 1 1 calc R . .
C52 C 0.1920(6) 1.3759(6) 0.2571(9) 0.129(6) Uani 1 1 d . . .
H52A H 0.2314 1.3781 0.2532 0.155 Uiso 1 1 calc R . .
C53 C 0.1617(5) 1.3094(6) 0.2585(6) 0.082(4) Uani 1 1 d . . .
C54 C 0.1956(5) 1.2409(6) 0.2531(6) 0.080(4) Uani 1 1 d . . .
H54A H 0.2328 1.2420 0.2442 0.096 Uiso 1 1 calc R . .
C55 C 0.2065(5) 1.1159(5) 0.2656(5) 0.058(3) Uani 1 1 d . . .
C56 C 0.2449(5) 1.0892(6) 0.3306(6) 0.084(4) Uani 1 1 d . . .
H56A H 0.2465 1.1127 0.3720 0.101 Uiso 1 1 calc R . .
C57 C 0.2816(6) 1.0284(6) 0.3371(5) 0.086(4) Uani 1 1 d . . .
H57A H 0.3093 1.0129 0.3822 0.103 Uiso 1 1 calc R . .
C58 C 0.2773(4) 0.9913(6) 0.2781(5) 0.061(3) Uani 1 1 d . . .
C59 C 0.2370(5) 1.0140(7) 0.2127(6) 0.083(4) Uani 1 1 d . . .
H59A H 0.2325 0.9870 0.1721 0.099 Uiso 1 1 calc R . .
C60 C 0.2016(5) 1.0781(6) 0.2054(5) 0.078(4) Uani 1 1 d . . .
H60A H 0.1751 1.0946 0.1602 0.093 Uiso 1 1 calc R . .
C61 C 0.3360(6) 0.8941(6) 0.3473(6) 0.082(4) Uani 1 1 d . . .
C62 C 0.2943(6) 0.8503(7) 0.3658(6) 0.096(4) Uani 1 1 d . . .
H62A H 0.2520 0.8444 0.3346 0.115 Uiso 1 1 calc R . .
C63 C 0.3173(5) 0.8173(6) 0.4298(6) 0.076(3) Uani 1 1 d . . .
H63A H 0.2896 0.7902 0.4439 0.091 Uiso 1 1 calc R . .
C64 C 0.3802(5) 0.8222(6) 0.4752(6) 0.070(3) Uani 1 1 d . . .
C65 C 0.4206(6) 0.8633(6) 0.4552(6) 0.089(4) Uani 1 1 d . . .
H65A H 0.4634 0.8669 0.4856 0.107 Uiso 1 1 calc R . .
C66 C 0.3991(6) 0.8993(7) 0.3909(6) 0.092(4) Uani 1 1 d . . .
H66A H 0.4268 0.9267 0.3772 0.110 Uiso 1 1 calc R . .
C67 C 0.3860(5) 0.7194(6) 0.5425(5) 0.075(3) Uani 1 1 d . . .
H67A H 0.3612 0.6976 0.4991 0.090 Uiso 1 1 calc R . .
O1 O 0.3491(4) 1.1890(4) 0.5885(4) 0.094(3) Uani 1 1 d . . .
O2 O 0.1257(3) 0.8517(4) 0.4484(4) 0.081(2) Uani 1 1 d . . .
O3 O 0.3124(4) 0.9308(4) 0.2791(4) 0.100(3) Uani 1 1 d . . .
C68 C 0.4042(5) 0.6791(6) 0.6100(6) 0.073(3) Uani 1 1 d . . .
C69 C 0.3828(6) 0.6074(7) 0.6096(7) 0.107(5) Uani 1 1 d . . .
H69A H 0.3562 0.5854 0.5672 0.129 Uiso 1 1 calc R . .
C70 C 0.4025(7) 0.5706(7) 0.6745(7) 0.126(6) Uani 1 1 d . . .
H70A H 0.3925 0.5221 0.6769 0.152 Uiso 1 1 calc R . .
C71 C 0.4375(6) 0.6096(7) 0.7350(7) 0.102(4) Uani 1 1 d . . .
H71A H 0.4471 0.5886 0.7799 0.122 Uiso 1 1 calc R . .
C72 C 0.4591(6) 0.6795(7) 0.7314(7) 0.100(4) Uani 1 1 d . . .
H72A H 0.4861 0.7028 0.7728 0.120 Uiso 1 1 calc R . .
B1 B 0.8589(3) 0.7866(4) 1.3352(4) 0.133(8) Uani 1 1 d D . .
F11 F 0.9233(3) 0.7876(5) 1.3566(4) 0.157(4) Uani 1 1 d D A .
F12 F 0.8284(5) 0.7928(7) 1.2628(4) 0.131(4) Uani 0.728(7) 1 d PDU A 1
F13 F 0.8516(6) 0.7261(6) 1.3696(8) 0.197(6) Uani 0.728(7) 1 d PDU A 1
F14 F 0.8224(8) 0.8155(14) 1.3679(10) 0.126(9) Uani 0.272(7) 1 d PDU A 1
F12' F 0.8526(7) 0.8554(5) 1.3549(7) 0.169(6) Uani 0.728(7) 1 d PDU A 2
F13' F 0.8398(17) 0.7495(11) 1.2724(8) 0.132(11) Uani 0.272(7) 1 d PDU A 2
F14' F 0.8246(9) 0.7602(19) 1.3717(12) 0.159(11) Uani 0.272(7) 1 d PDU A 2
B2 B 0.5645(3) -0.0649(4) 0.4301(4) 0.139(7) Uani 1 1 d D . .
F21 F 0.5488(4) -0.0368(5) 0.4837(4) 0.159(3) Uani 1 1 d D B .
F22 F 0.5734(13) -0.1310(7) 0.4615(11) 0.174(10) Uani 0.450(12) 1 d PDU B 1
F23 F 0.5186(8) -0.0493(14) 0.3645(6) 0.141(8) Uani 0.450(12) 1 d PDU B 1
F24 F 0.6175(6) -0.0244(11) 0.4421(13) 0.157(10) Uani 0.450(12) 1 d PDU B 1
F22' F 0.5607(11) -0.1381(5) 0.4241(11) 0.167(8) Uani 0.550(12) 1 d PDU B 2
F23' F 0.5360(12) -0.0412(14) 0.3610(7) 0.203(10) Uani 0.550(12) 1 d PDU B 2
F24' F 0.6283(4) -0.0614(13) 0.4461(12) 0.160(8) Uani 0.550(12) 1 d PDU B 2
B3 B 0.7234(3) 0.1524(4) 0.3655(4) 0.120(6) Uani 1 1 d D . .
F31 F 0.6915(7) 0.0972(6) 0.3222(8) 0.160(6) Uani 0.650(8) 1 d PDU C 1
F32 F 0.7008(10) 0.2156(6) 0.3298(10) 0.222(10) Uani 0.650(8) 1 d PDU C 1
F33 F 0.7289(7) 0.1429(11) 0.4347(5) 0.198(7) Uani 0.650(8) 1 d PDU C 1
F34 F 0.7857(4) 0.1505(9) 0.3741(8) 0.169(6) Uani 0.650(8) 1 d PDU C 1
F31' F 0.6821(6) 0.0956(7) 0.3503(11) 0.129(10) Uani 0.350(8) 1 d PDU C 2
F32' F 0.7684(8) 0.1442(13) 0.4326(6) 0.217(14) Uani 0.350(8) 1 d PDU C 2
F33' F 0.7514(6) 0.1543(14) 0.3170(7) 0.190(12) Uani 0.350(8) 1 d PDU C 2
F34' F 0.6898(7) 0.2146(6) 0.3604(12) 0.122(8) Uani 0.350(8) 1 d PDU C 2
B4 B 0.5223(3) 0.6016(4) 0.5349(4) 0.137(8) Uani 1 1 d D . .
F41 F 0.5131(5) 0.6735(4) 0.5235(5) 0.170(4) Uani 1 1 d D D .
F42 F 0.4637(5) 0.5705(11) 0.5121(12) 0.158(9) Uani 0.441(8) 1 d PDU D 1
F43 F 0.5621(11) 0.5837(13) 0.6021(7) 0.170(9) Uani 0.441(8) 1 d PDU D 1
F44 F 0.5566(7) 0.5888(14) 0.4945(8) 0.176(8) Uani 0.441(8) 1 d PDU D 1
F42' F 0.5167(8) 0.5882(9) 0.5980(6) 0.138(6) Uani 0.559(8) 1 d PDU D 2
F43' F 0.5832(5) 0.5775(12) 0.5557(10) 0.199(8) Uani 0.559(8) 1 d PDU D 2
F44' F 0.4953(11) 0.5620(9) 0.4749(7) 0.181(8) Uani 0.559(8) 1 d PDU D 2
N13 N 0.6123(9) 0.1139(12) 0.5834(9) 0.132(7) Uani 0.632(8) 1 d PU E 1
C73 C 0.6552(12) 0.0991(15) 0.5800(13) 0.127(7) Uani 0.632(8) 1 d PU E 1
C74 C 0.7088(12) 0.0784(14) 0.5777(14) 0.147(9) Uani 0.632(8) 1 d PU E 1
H74A H 0.7213 0.1040 0.5438 0.220 Uiso 0.632(8) 1 d PR E 1
H74B H 0.7403 0.0856 0.6253 0.220 Uiso 0.632(8) 1 d PR E 1
H74C H 0.7053 0.0277 0.5664 0.220 Uiso 0.632(8) 1 d PR E 1
N14 N 0.8574(15) -0.0811(11) 0.5737(15) 0.111(9) Uani 0.368(8) 1 d PU E 2
C75 C 0.8199(18) -0.0620(16) 0.520(2) 0.112(9) Uani 0.368(8) 1 d PU E 2
C76 C 0.7810(16) -0.0485(16) 0.4583(17) 0.103(10) Uani 0.368(8) 1 d PU E 2
H76A H 0.7577 -0.0047 0.4564 0.154 Uiso 0.368(8) 1 d PR E 2
H76B H 0.7520 -0.0888 0.4457 0.154 Uiso 0.368(8) 1 d PR E 2
H76C H 0.8018 -0.0454 0.4251 0.154 Uiso 0.368(8) 1 d PR E 2
O4 O 0.8821(13) -0.019(2) 0.8402(17) 0.148(8) Uani 0.230(9) 1 d PDU F 1
C77 C 0.853(2) -0.015(4) 0.893(2) 0.156(13) Uani 0.230(9) 1 d PDU F 1
O4' O 0.8201(14) -0.0220(19) 0.7827(16) 0.149(8) Uani 0.270(9) 1 d PDU F 2
C77' C 0.7681(19) -0.041(3) 0.718(2) 0.140(11) Uani 0.270(9) 1 d PDU F 2
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N1 Ni1 N2 77.7(3) . . ?
N1 Ni1 N10 175.6(3) . . ?
N2 Ni1 N10 98.1(3) . . ?
N1 Ni1 N9 101.9(3) . . ?
N2 Ni1 N9 88.1(3) . . ?
N10 Ni1 N9 76.8(3) . . ?
N1 Ni1 N5 94.0(3) . . ?
N2 Ni1 N5 171.6(4) . . ?
N10 Ni1 N5 90.3(3) . . ?
N9 Ni1 N5 94.7(3) . . ?
N1 Ni1 N6 89.6(3) . . ?
N2 Ni1 N6 102.2(3) . . ?
N10 Ni1 N6 92.3(3) . . ?
N9 Ni1 N6 166.1(4) . . ?
N5 Ni1 N6 76.5(3) . . ?
N8 Ni2 N12 92.1(3) . . ?
N8 Ni2 N4 95.3(3) . . ?
N12 Ni2 N4 94.5(4) . . ?
N8 Ni2 N11 164.4(3) . . ?
N12 Ni2 N11 77.1(3) . . ?
N4 Ni2 N11 96.8(3) . . ?
N8 Ni2 N7 78.0(3) . . ?
N12 Ni2 N7 90.0(3) . . ?
N4 Ni2 N7 172.0(3) . . ?
N11 Ni2 N7 90.7(3) . . ?
N8 Ni2 N3 90.3(3) . . ?
N12 Ni2 N3 172.3(3) . . ?
N4 Ni2 N3 78.1(4) . . ?
N11 Ni2 N3 101.8(3) . . ?
N7 Ni2 N3 97.6(3) . . ?
C5 N1 C1 115.5(10) . . ?
C5 N1 Ni1 116.7(7) . . ?
C1 N1 Ni1 127.6(8) . . ?
C6 N2 C7 114.6(8) . . ?
C6 N2 Ni1 113.8(6) . . ?
C7 N2 Ni1 131.6(7) . . ?
C19 N3 C16 118.0(9) . . ?
C19 N3 Ni2 114.1(7) . . ?
C16 N3 Ni2 127.5(6) . . ?
C24 N4 C20 117.5(10) . . ?
C24 N4 Ni2 129.6(9) . . ?
C20 N4 Ni2 112.8(8) . . ?
C25 N5 C29 119.8(9) . . ?
C25 N5 Ni1 125.2(8) . . ?
C29 N5 Ni1 114.9(7) . . ?
C30 N6 C31 117.3(9) . . ?
C30 N6 Ni1 110.4(7) . . ?
C31 N6 Ni1 131.9(6) . . ?
C43 N7 C40 119.5(9) . . ?
C43 N7 Ni2 112.0(7) . . ?
C40 N7 Ni2 127.6(6) . . ?
C48 N8 C44 115.2(9) . . ?
C48 N8 Ni2 130.6(8) . . ?
C44 N8 Ni2 114.3(6) . . ?
C53 N9 C49 116.5(10) . . ?
C53 N9 Ni1 117.0(8) . . ?
C49 N9 Ni1 126.4(7) . . ?
C54 N10 C55 115.7(8) . . ?
C54 N10 Ni1 113.6(7) . . ?
C55 N10 Ni1 130.7(6) . . ?
C67 N11 C64 115.0(8) . . ?
C67 N11 Ni2 112.9(7) . . ?
C64 N11 Ni2 131.6(6) . . ?
C68 N12 C72 120.6(10) . . ?
C68 N12 Ni2 113.4(7) . . ?
C72 N12 Ni2 125.8(8) . . ?
C2 C1 N1 121.2(11) . . ?
C3 C2 C1 123.5(12) . . ?
C2 C3 C4 116.1(12) . . ?
C5 C4 C3 116.8(11) . . ?
N1 C5 C4 126.6(10) . . ?
N1 C5 C6 113.5(10) . . ?
C4 C5 C6 119.6(10) . . ?
N2 C6 C5 118.3(9) . . ?
C12 C7 C8 118.3(10) . . ?
C12 C7 N2 120.2(10) . . ?
C8 C7 N2 120.9(8) . . ?
C9 C8 C7 120.0(10) . . ?
C10 C9 C8 121.4(12) . . ?
C9 C10 O1 118.7(10) . . ?
C9 C10 C11 120.2(11) . . ?
O1 C10 C11 120.2(10) . . ?
C12 C11 C10 118.6(12) . . ?
C7 C12 C11 120.7(12) . . ?
C14 C13 O1 120.3(11) . . ?
C14 C13 C18 119.6(12) . . ?
O1 C13 C18 120.0(10) . . ?
C13 C14 C15 120.5(11) . . ?
C16 C15 C14 119.9(10) . . ?
C15 C16 C17 118.9(10) . . ?
C15 C16 N3 118.4(9) . . ?
C17 C16 N3 122.6(10) . . ?
C18 C17 C16 121.8(12) . . ?
C17 C18 C13 119.1(11) . . ?
N3 C19 C20 121.2(11) . . ?
C21 C20 N4 120.5(13) . . ?
C21 C20 C19 125.9(14) . . ?
N4 C20 C19 113.5(11) . . ?
C20 C21 C22 118.9(16) . . ?
C23 C22 C21 116.4(14) . . ?
C24 C23 C22 122.4(17) . . ?
C23 C24 N4 124.0(15) . . ?
N5 C25 C26 122.7(12) . . ?
C25 C26 C27 115.3(13) . . ?
C28 C27 C26 120.6(14) . . ?
C29 C28 C27 119.9(13) . . ?
N5 C29 C28 121.6(10) . . ?
N5 C29 C30 115.0(10) . . ?
C28 C29 C30 123.3(11) . . ?
N6 C30 C29 123.1(10) . . ?
C36 C31 C32 121.3(10) . . ?
C36 C31 N6 120.8(10) . . ?
C32 C31 N6 117.7(9) . . ?
C31 C32 C33 119.0(11) . . ?
C32 C33 C34 119.7(11) . . ?
C35 C34 O2 120.3(10) . . ?
C35 C34 C33 120.5(10) . . ?
O2 C34 C33 119.1(10) . . ?
C34 C35 C36 120.6(11) . . ?
C31 C36 C35 118.6(10) . . ?
C38 C37 C42 121.2(9) . . ?
C38 C37 O2 117.9(10) . . ?
C42 C37 O2 120.8(9) . . ?
C37 C38 C39 121.3(10) . . ?
C38 C39 C40 119.2(9) . . ?
C41 C40 N7 120.1(10) . . ?
C41 C40 C39 118.3(9) . . ?
N7 C40 C39 121.5(9) . . ?
C40 C41 C42 121.3(10) . . ?
C41 C42 C37 118.6(9) . . ?
N7 C43 C44 122.4(10) . . ?
C45 C44 N8 123.9(10) . . ?
C45 C44 C43 123.6(11) . . ?
N8 C44 C43 112.4(9) . . ?
C46 C45 C44 118.1(13) . . ?
C45 C46 C47 121.4(13) . . ?
C46 C47 C48 116.4(12) . . ?
N8 C48 C47 125.0(13) . . ?
C50 C49 N9 120.9(13) . . ?
C49 C50 C51 119.9(13) . . ?
C52 C51 C50 119.3(13) . . ?
C51 C52 C53 115.8(13) . . ?
N9 C53 C52 127.3(12) . . ?
N9 C53 C54 115.1(11) . . ?
C52 C53 C54 117.6(11) . . ?
N10 C54 C53 116.8(10) . . ?
C56 C55 C60 118.3(10) . . ?
C56 C55 N10 119.9(9) . . ?
C60 C55 N10 121.7(9) . . ?
C55 C56 C57 122.0(11) . . ?
C58 C57 C56 119.9(10) . . ?
C57 C58 C59 119.9(10) . . ?
C57 C58 O3 124.0(8) . . ?
C59 C58 O3 116.1(9) . . ?
C58 C59 C60 120.5(10) . . ?
C55 C60 C59 119.4(10) . . ?
C66 C61 C62 121.3(11) . . ?
C66 C61 O3 119.6(11) . . ?
C62 C61 O3 119.0(10) . . ?
C63 C62 C61 117.9(11) . . ?
C62 C63 C64 122.2(12) . . ?
C65 C64 C63 119.0(11) . . ?
C65 C64 N11 119.3(9) . . ?
C63 C64 N11 121.7(10) . . ?
C64 C65 C66 121.0(12) . . ?
C61 C66 C65 118.6(13) . . ?
N11 C67 C68 119.2(9) . . ?
C13 O1 C10 116.8(8) . . ?
C34 O2 C37 119.0(8) . . ?
C58 O3 C61 113.5(8) . . ?
N12 C68 C69 122.9(10) . . ?
N12 C68 C67 117.1(10) . . ?
C69 C68 C67 120.0(10) . . ?
C70 C69 C68 118.1(12) . . ?
C71 C70 C69 116.5(13) . . ?
C70 C71 C72 122.2(12) . . ?
N12 C72 C71 119.3(11) . . ?
F14' B1 F14 44.4(17) . . ?
F14' B1 F13' 106(2) . . ?
F14 B1 F13' 128.2(19) . . ?
F14' B1 F11 127.5(11) . . ?
F14 B1 F11 128.8(10) . . ?
F13' B1 F11 102.9(17) . . ?
F14' B1 F12' 91.6(18) . . ?
F14 B1 F12' 48.1(12) . . ?
F13' B1 F12' 135.7(13) . . ?
F11 B1 F12' 96.8(9) . . ?
F14' B1 F12 116.9(12) . . ?
F14 B1 F12 109.6(11) . . ?
F13' B1 F12 36.1(11) . . ?
F11 B1 F12 112.5(8) . . ?
F12' B1 F12 99.7(9) . . ?
F14' B1 F13 38.3(14) . . ?
F14 B1 F13 81.6(14) . . ?
F13' B1 F13 90.2(14) . . ?
F11 B1 F13 100.3(9) . . ?
F12' B1 F13 124.8(11) . . ?
F12 B1 F13 120.4(10) . . ?
B1 F13 F14 49.0(7) . . ?
B1 F14 F13 49.3(8) . . ?
F22 B2 F24 116.8(15) . . ?
F22 B2 F22' 30.2(13) . . ?
F24 B2 F22' 125.9(15) . . ?
F22 B2 F24' 88.8(16) . . ?
F24 B2 F24' 30.7(13) . . ?
F22' B2 F24' 95.4(15) . . ?
F22 B2 F23 124.4(15) . . ?
F24 B2 F23 110.5(15) . . ?
F22' B2 F23 97.2(14) . . ?
F24' B2 F23 124.5(14) . . ?
F22 B2 F23' 133.9(15) . . ?
F24 B2 F23' 92.6(15) . . ?
F22' B2 F23' 103.9(15) . . ?
F24' B2 F23' 105.7(16) . . ?
F23 B2 F23' 19.1(17) . . ?
F22 B2 F21 90.6(12) . . ?
F24 B2 F21 97.7(13) . . ?
F22' B2 F21 114.9(12) . . ?
F24' B2 F21 112.0(12) . . ?
F23 B2 F21 110.6(10) . . ?
F23' B2 F21 121.4(14) . . ?
F32' B3 F31 124.7(13) . . ?
F32' B3 F33' 109.9(10) . . ?
F31 B3 F33' 80.7(13) . . ?
F32' B3 F34 61.4(11) . . ?
F31 B3 F34 109.5(11) . . ?
F33' B3 F34 48.5(9) . . ?
F32' B3 F31' 109.1(11) . . ?
F31 B3 F31' 29.0(13) . . ?
F33' B3 F31' 109.4(11) . . ?
F34 B3 F31' 127.0(11) . . ?
F32' B3 F34' 110.7(12) . . ?
F31 B3 F34' 116.3(10) . . ?
F33' B3 F34' 109.2(12) . . ?
F34 B3 F34' 123.9(11) . . ?
F31' B3 F34' 108.5(9) . . ?
F32' B3 F32 127.5(14) . . ?
F31 B3 F32 107.8(10) . . ?
F33' B3 F32 77.4(14) . . ?
F34 B3 F32 104.5(13) . . ?
F31' B3 F32 117.1(11) . . ?
F34' B3 F32 32.1(14) . . ?
F32' B3 F33 39.4(11) . . ?
F31 B3 F33 112.1(12) . . ?
F33' B3 F33 149.0(10) . . ?
F34 B3 F33 100.8(10) . . ?
F31' B3 F33 85.0(12) . . ?
F34' B3 F33 90.7(13) . . ?
F32 B3 F33 121.2(14) . . ?
F44' B4 F43 132.0(14) . . ?
F44' B4 F44 61.9(13) . . ?
F43 B4 F44 104.2(14) . . ?
F44' B4 F41 113.3(9) . . ?
F43 B4 F41 114.3(12) . . ?
F44 B4 F41 99.0(13) . . ?
F44' B4 F42' 125.0(14) . . ?
F43 B4 F42' 43.8(12) . . ?
F44 B4 F42' 145.6(13) . . ?
F41 B4 F42' 106.0(10) . . ?
F44' B4 F42 54.3(12) . . ?
F43 B4 F42 115.3(16) . . ?
F44 B4 F42 116.2(14) . . ?
F41 B4 F42 106.9(11) . . ?
F42' B4 F42 78.8(13) . . ?
F44' B4 F43' 98.9(14) . . ?
F43 B4 F43' 53.2(12) . . ?
F44 B4 F43' 51.0(10) . . ?
F41 B4 F43' 116.6(13) . . ?
F42' B4 F43' 96.0(12) . . ?
F42 B4 F43' 135.8(14) . . ?
N13 C73 C74 178(3) . . ?
N14 C75 C76 172(4) . . ?
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 2.096(9) . ?
Ni1 N2 2.111(7) . ?
Ni1 N10 2.135(8) . ?
Ni1 N9 2.136(8) . ?
Ni1 N5 2.137(8) . ?
Ni1 N6 2.173(8) . ?
Ni2 N8 2.127(8) . ?
Ni2 N12 2.151(9) . ?
Ni2 N4 2.153(9) . ?
Ni2 N11 2.161(8) . ?
Ni2 N7 2.184(9) . ?
Ni2 N3 2.189(8) . ?
N1 C5 1.280(13) . ?
N1 C1 1.372(13) . ?
N2 C6 1.269(13) . ?
N2 C7 1.433(11) . ?
N3 C19 1.252(13) . ?
N3 C16 1.444(12) . ?
N4 C24 1.314(14) . ?
N4 C20 1.435(16) . ?
N5 C25 1.332(14) . ?
N5 C29 1.334(14) . ?
N6 C30 1.309(11) . ?
N6 C31 1.456(12) . ?
N7 C43 1.221(12) . ?
N7 C40 1.415(11) . ?
N8 C48 1.325(12) . ?
N8 C44 1.372(13) . ?
N9 C53 1.275(14) . ?
N9 C49 1.411(13) . ?
N10 C54 1.331(13) . ?
N10 C55 1.416(12) . ?
N11 C67 1.283(13) . ?
N11 C64 1.451(13) . ?
N12 C68 1.308(12) . ?
N12 C72 1.318(13) . ?
C1 C2 1.364(17) . ?
C2 C3 1.286(16) . ?
C3 C4 1.450(16) . ?
C4 C5 1.354(16) . ?
C5 C6 1.526(14) . ?
C7 C12 1.353(14) . ?
C7 C8 1.410(15) . ?
C8 C9 1.378(15) . ?
C9 C10 1.300(14) . ?
C10 O1 1.374(11) . ?
C10 C11 1.415(16) . ?
C11 C12 1.398(16) . ?
C13 C14 1.335(14) . ?
C13 O1 1.364(13) . ?
C13 C18 1.396(17) . ?
C14 C15 1.421(14) . ?
C15 C16 1.344(14) . ?
C16 C17 1.376(14) . ?
C17 C18 1.363(16) . ?
C19 C20 1.501(16) . ?
C20 C21 1.327(18) . ?
C21 C22 1.45(2) . ?
C22 C23 1.38(2) . ?
C23 C24 1.279(18) . ?
C25 C26 1.371(16) . ?
C26 C27 1.43(2) . ?
C27 C28 1.34(2) . ?
C28 C29 1.339(15) . ?
C29 C30 1.387(14) . ?
C31 C36 1.377(14) . ?
C31 C32 1.381(14) . ?
C32 C33 1.401(13) . ?
C33 C34 1.413(15) . ?
C34 C35 1.327(14) . ?
C34 O2 1.370(11) . ?
C35 C36 1.437(14) . ?
C37 C38 1.338(13) . ?
C37 C42 1.398(15) . ?
C37 O2 1.412(11) . ?
C38 C39 1.356(12) . ?
C39 C40 1.437(14) . ?
C40 C41 1.371(14) . ?
C41 C42 1.370(13) . ?
C43 C44 1.518(13) . ?
C44 C45 1.351(14) . ?
C45 C46 1.348(15) . ?
C46 C47 1.374(19) . ?
C47 C48 1.377(16) . ?
C49 C50 1.370(15) . ?
C50 C51 1.402(19) . ?
C51 C52 1.384(19) . ?
C52 C53 1.412(16) . ?
C53 C54 1.507(16) . ?
C55 C56 1.359(13) . ?
C55 C60 1.368(14) . ?
C56 C57 1.374(14) . ?
C57 C58 1.344(13) . ?
C58 C59 1.350(12) . ?
C58 O3 1.369(11) . ?
C59 C60 1.406(14) . ?
C61 C66 1.364(15) . ?
C61 C62 1.402(17) . ?
C61 O3 1.440(12) . ?
C62 C63 1.338(15) . ?
C63 C64 1.371(14) . ?
C64 C65 1.369(16) . ?
C65 C66 1.368(14) . ?
C67 C68 1.465(15) . ?
C68 C69 1.409(16) . ?
C69 C70 1.386(17) . ?
C70 C71 1.377(16) . ?
C71 C72 1.393(17) . ?
B1 F14' 1.354(11) . ?
B1 F14 1.354(10) . ?
B1 F13' 1.356(10) . ?
B1 F11 1.356(8) . ?
B1 F12' 1.357(9) . ?
B1 F12 1.359(8) . ?
B1 F13 1.360(9) . ?
F13 F14 1.77(3) . ?
B2 F22 1.355(10) . ?
B2 F24 1.358(10) . ?
B2 F22' 1.358(9) . ?
B2 F24' 1.359(9) . ?
B2 F23 1.362(9) . ?
B2 F23' 1.362(10) . ?
B2 F21 1.366(8) . ?
B3 F32' 1.354(9) . ?
B3 F31 1.356(9) . ?
B3 F33' 1.357(9) . ?
B3 F34 1.360(9) . ?
B3 F31' 1.360(9) . ?
B3 F34' 1.362(9) . ?
B3 F32 1.364(9) . ?
B3 F33 1.366(9) . ?
B4 F44' 1.344(9) . ?
B4 F43 1.348(10) . ?
B4 F44 1.348(10) . ?
B4 F41 1.350(8) . ?
B4 F42' 1.351(9) . ?
B4 F42 1.357(9) . ?
B4 F43' 1.357(9) . ?
N13 C73 1.04(3) . ?
C73 C74 1.30(3) . ?
N14 C75 1.14(4) . ?
C75 C76 1.25(4) . ?
O4 C77 1.44(2) . ?
O4' C77' 1.43(2) . ?
