#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:32:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179484 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/81/4338185.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_4338185
loop_
_publ_author_name
'Reger, Daniel L.'
'Pascui, Andrea E.'
'Pellechia, Perry J.'
'Smith, Mark D.'
'Jezierska, Julia'
'Ozarowski, Andrew'
_publ_section_title
;
 Hydroxide-Bridged Cubane Complexes of Nickel(II) and Cadmium(II):
 Magnetic, EPR, and Unusual Dynamic Properties.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4325
_journal_page_last               4339
_journal_paper_doi               10.1021/ic403013d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
; 
C46.42 H58.84 N18 Ni4 O8, 2(C3 H7 N O), 
1.58(C H4 O), 0.42(C4 H10 O), 4(Cl O4) 
;
_chemical_formula_sum            'C55.67 H83.34 Cl4 N20 Ni4 O28'
_chemical_formula_weight         1857.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.8900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7442(12)
_cell_length_b                   17.5713(10)
_cell_length_c                   22.1788(12)
_cell_measurement_reflns_used    8997
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.219
_cell_measurement_theta_min      2.177
_cell_volume                     7623.4(7)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_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  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39396
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             3846
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         6744
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0497
_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)+(0.0758P)²+11.5598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                5154
_reflns_number_total             6744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403013d_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338184--4338186.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4338185
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'
'-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 0.54858(3) 0.62815(3) 0.21308(2) 0.01970(15) Uani 1 1 d . . .
Ni2 Ni 0.56587(3) 0.50166(3) 0.31781(2) 0.02032(15) Uani 1 1 d . . .
C1 C 0.6863(2) 0.7449(2) 0.2882(2) 0.0292(10) Uani 1 1 d . A .
H1 H 0.7244 0.7821 0.2981 0.035 Uiso 1 1 calc R . .
C2 C 0.7118(2) 0.5402(2) 0.4576(2) 0.0265(10) Uani 1 1 d . A .
H2 H 0.7546 0.5385 0.5005 0.032 Uiso 1 1 calc R . .
C3 C 0.6883(2) 0.7207(2) 0.3549(2) 0.0266(10) Uani 1 1 d . . .
C4 C 0.7067(2) 0.6473(2) 0.3791(2) 0.0246(9) Uani 1 1 d . . .
H4 H 0.7244 0.6136 0.3571 0.029 Uiso 1 1 calc R . .
C5 C 0.6993(2) 0.6227(2) 0.4350(2) 0.0254(9) Uani 1 1 d . . .
C6 C 0.6787(2) 0.6744(3) 0.4706(2) 0.0310(10) Uani 1 1 d . . .
H6 H 0.6740 0.6584 0.5093 0.037 Uiso 1 1 calc R . .
C7 C 0.6652(2) 0.7490(3) 0.4488(2) 0.0342(11) Uani 1 1 d . . .
H7 H 0.6532 0.7848 0.4741 0.041 Uiso 1 1 calc R . .
C8 C 0.6687(2) 0.7726(3) 0.3909(2) 0.0311(10) Uani 1 1 d . . .
H8 H 0.6579 0.8236 0.3758 0.037 Uiso 1 1 calc R . .
C11 C 0.6139(3) 0.8593(3) 0.2327(2) 0.0370(12) Uani 1 1 d . A .
H11 H 0.6488 0.8968 0.2474 0.044 Uiso 1 1 calc R . .
C12 C 0.5466(3) 0.8717(3) 0.1950(2) 0.0402(12) Uani 1 1 d . A .
H12 H 0.5246 0.9189 0.1780 0.048 Uiso 1 1 calc R . .
C13 C 0.5165(2) 0.8005(2) 0.1867(2) 0.0316(10) Uani 1 1 d . . .
H13 H 0.4689 0.7914 0.1615 0.038 Uiso 1 1 calc R A .
C21 C 0.7540(2) 0.6664(3) 0.2441(2) 0.0389(12) Uani 1 1 d . A .
H21 H 0.7933 0.6980 0.2571 0.047 Uiso 1 1 calc R . .
C22 C 0.7446(2) 0.5979(3) 0.2135(2) 0.0435(13) Uani 1 1 d . A .
H22 H 0.7759 0.5717 0.2016 0.052 Uiso 1 1 calc R . .
C23 C 0.6803(2) 0.5738(3) 0.2031(2) 0.0312(10) Uani 1 1 d . . .
H23 H 0.6596 0.5276 0.1814 0.037 Uiso 1 1 calc R A .
C31 C 0.7799(2) 0.4554(3) 0.4179(2) 0.0393(12) Uani 1 1 d . A .
H31 H 0.8219 0.4540 0.4574 0.047 Uiso 1 1 calc R . .
C32 C 0.7665(2) 0.4204(3) 0.3589(2) 0.0434(13) Uani 1 1 d . A .
H32 H 0.7969 0.3900 0.3487 0.052 Uiso 1 1 calc R . .
C33 C 0.6993(2) 0.4383(3) 0.3165(2) 0.0331(11) Uani 1 1 d . . .
H33 H 0.6759 0.4211 0.2715 0.040 Uiso 1 1 calc R A .
C41 C 0.6596(2) 0.4892(2) 0.5309(2) 0.0310(11) Uani 1 1 d . A .
H41 H 0.6989 0.4906 0.5729 0.037 Uiso 1 1 calc R . .
C42 C 0.5956(2) 0.4661(3) 0.5202(2) 0.0300(10) Uani 1 1 d . A .
H42 H 0.5813 0.4484 0.5525 0.036 Uiso 1 1 calc R . .
C43 C 0.5561(2) 0.4741(2) 0.4518(2) 0.0270(10) Uani 1 1 d . . .
H43 H 0.5089 0.4619 0.4296 0.032 Uiso 1 1 calc R A .
N11 N 0.56208(17) 0.74639(19) 0.21833(16) 0.0248(8) Uani 1 1 d . A .
N12 N 0.62274(18) 0.7834(2) 0.24569(17) 0.0273(8) Uani 1 1 d . . .
N21 N 0.65109(17) 0.62434(19) 0.22780(16) 0.0250(8) Uani 1 1 d . A .
N22 N 0.69768(18) 0.6818(2) 0.25262(17) 0.0286(8) Uani 1 1 d . . .
N31 N 0.67147(17) 0.4827(2) 0.34683(17) 0.0271(8) Uani 1 1 d . A .
N32 N 0.72243(17) 0.4925(2) 0.41024(17) 0.0275(8) Uani 1 1 d . . .
N41 N 0.59217(17) 0.50081(19) 0.42084(17) 0.0258(8) Uani 1 1 d . A .
N42 N 0.65678(17) 0.50967(19) 0.47104(17) 0.0259(8) Uani 1 1 d . . .
O1 O 0.55318(14) 0.61829(15) 0.30734(13) 0.0207(6) Uani 1 1 d D . .
H1A H 0.584(2) 0.645(2) 0.335(2) 0.049(16) Uiso 1 1 d D . .
O2 O 0.53817(14) 0.51200(15) 0.21625(13) 0.0204(6) Uani 1 1 d D . .
H2A H 0.561(2) 0.480(2) 0.208(3) 0.052(17) Uiso 1 1 d D . .
O3A O 0.52718(18) 0.63513(18) 0.11059(15) 0.0361(8) Uani 0.791(5) 1 d PD A 5
H3A H 0.555(2) 0.667(3) 0.107(3) 0.054 Uiso 0.791(5) 1 d PD A 5
H3B H 0.4894(17) 0.639(4) 0.075(2) 0.054 Uiso 0.791(5) 1 d PD A 5
O3B O 0.52718(18) 0.63513(18) 0.11059(15) 0.0361(8) Uani 0.209(5) 1 d PD A 6
C34 C 0.4756(10) 0.6626(13) 0.0474(7) 0.036(6) Uiso 0.209(5) 1 d PD A 6
H34A H 0.4641 0.7154 0.0525 0.054 Uiso 0.209(5) 1 calc PR A 6
H34B H 0.4346 0.6309 0.0333 0.054 Uiso 0.209(5) 1 calc PR A 6
H34C H 0.4930 0.6602 0.0135 0.054 Uiso 0.209(5) 1 calc PR A 6
Cl1A Cl 0.62150(17) 0.34586(15) 0.12268(18) 0.0339(6) Uani 0.719(7) 1 d P B 1
O11A O 0.5980(3) 0.4113(3) 0.1447(3) 0.0346(16) Uiso 0.719(7) 1 d P B 1
O12A O 0.6883(3) 0.3606(3) 0.1299(3) 0.0562(17) Uiso 0.719(7) 1 d P B 1
O13A O 0.5764(3) 0.3384(3) 0.0523(3) 0.0537(17) Uiso 0.719(7) 1 d P B 1
O14A O 0.6203(3) 0.2769(3) 0.1564(3) 0.0623(18) Uiso 0.719(7) 1 d P B 1
Cl1B Cl 0.6396(4) 0.3455(5) 0.1473(4) 0.0339(6) Uani 0.281(7) 1 d P B 2
O11B O 0.5921(7) 0.3941(9) 0.1547(7) 0.032(4) Uiso 0.281(7) 1 d P B 2
O12B O 0.7021(8) 0.3825(9) 0.1591(8) 0.055(4) Uiso 0.281(7) 1 d P B 2
O13B O 0.6275(12) 0.3100(14) 0.0857(12) 0.110(8) Uiso 0.281(7) 1 d P B 2
O14B O 0.6460(8) 0.2972(8) 0.1978(8) 0.060(4) Uiso 0.281(7) 1 d P B 2
Cl2 Cl 0.86599(6) 0.50859(6) 0.12594(6) 0.0375(3) Uani 1 1 d . . .
O21 O 0.9223(3) 0.5331(3) 0.1826(3) 0.135(3) Uani 1 1 d . . .
O22 O 0.8330(2) 0.5713(2) 0.08240(18) 0.0592(11) Uani 1 1 d . . .
O23 O 0.8180(2) 0.4703(2) 0.1425(2) 0.0673(12) Uani 1 1 d . . .
O24 O 0.8850(3) 0.4548(3) 0.0889(3) 0.0942(17) Uani 1 1 d . . .
C51 C 0.5270(3) 0.0771(3) 0.4767(3) 0.0607(16) Uani 1 1 d D . .
H51 H 0.5480 0.0456 0.4562 0.073 Uiso 1 1 calc R . .
C52 C 0.4250(3) 0.1324(4) 0.4734(4) 0.0693(18) Uani 1 1 d D . .
H52A H 0.4578 0.1497 0.5179 0.104 Uiso 1 1 calc R . .
H52B H 0.3908 0.0995 0.4778 0.104 Uiso 1 1 calc R . .
H52C H 0.4023 0.1765 0.4456 0.104 Uiso 1 1 calc R . .
C53 C 0.4213(3) 0.0624(4) 0.3747(3) 0.075(2) Uani 1 1 d D . .
H53A H 0.4514 0.0335 0.3608 0.112 Uiso 1 1 calc R . .
H53B H 0.4016 0.1054 0.3442 0.112 Uiso 1 1 calc R . .
H53C H 0.3844 0.0292 0.3734 0.112 Uiso 1 1 calc R . .
N5 N 0.4604(2) 0.0906(3) 0.4427(2) 0.0474(11) Uani 1 1 d D . .
O5 O 0.5638(2) 0.1027(3) 0.5333(2) 0.0757(13) Uani 1 1 d D . .
C44A C 0.5511(6) 0.3364(5) 0.3449(5) 0.0420(19) Uiso 0.50 1 d PD A 3
H44A H 0.5231 0.3519 0.3657 0.050 Uiso 0.50 1 calc PR A 3
C45A C 0.6288(7) 0.2445(9) 0.3380(9) 0.095(5) Uiso 0.50 1 d PD A 3
H45A H 0.6717 0.2575 0.3768 0.143 Uiso 0.50 1 calc PR A 3
H45B H 0.6258 0.2725 0.2986 0.143 Uiso 0.50 1 calc PR A 3
H45C H 0.6277 0.1897 0.3294 0.143 Uiso 0.50 1 calc PR A 3
C46A C 0.5469(6) 0.2080(6) 0.3839(6) 0.052(3) Uiso 0.50 1 d PD A 3
H46A H 0.5037 0.2252 0.3832 0.077 Uiso 0.50 1 calc PR A 3
H46B H 0.5809 0.2007 0.4304 0.077 Uiso 0.50 1 calc PR A 3
H46C H 0.5394 0.1597 0.3595 0.077 Uiso 0.50 1 calc PR A 3
N4A N 0.5715(4) 0.2650(4) 0.3518(4) 0.036(2) Uiso 0.50 1 d PD A 3
O4A O 0.56605(16) 0.38398(16) 0.31318(15) 0.0339(7) Uani 0.50 1 d PD A 3
C44B C 0.5377(6) 0.3313(5) 0.3255(5) 0.0420(19) Uiso 0.50 1 d PD A 4
H44B H 0.5037 0.3434 0.3400 0.050 Uiso 0.50 1 calc PR A 4
C45B C 0.6005(5) 0.2335(6) 0.3006(6) 0.048(3) Uiso 0.50 1 d PD A 4
H45D H 0.6333 0.2746 0.3075 0.072 Uiso 0.50 1 calc PR A 4
H45E H 0.5786 0.2194 0.2531 0.072 Uiso 0.50 1 calc PR A 4
H45F H 0.6244 0.1892 0.3274 0.072 Uiso 0.50 1 calc PR A 4
C46B C 0.5163(9) 0.1998(8) 0.3432(9) 0.106(6) Uiso 0.50 1 d PD A 4
H46D H 0.4747 0.1823 0.3051 0.159 Uiso 0.50 1 calc PR A 4
H46E H 0.5044 0.2212 0.3775 0.159 Uiso 0.50 1 calc PR A 4
H46F H 0.5476 0.1568 0.3621 0.159 Uiso 0.50 1 calc PR A 4
N4B N 0.5497(5) 0.2585(5) 0.3206(5) 0.048(2) Uiso 0.50 1 d PD A 4
O4B O 0.56605(16) 0.38398(16) 0.31318(15) 0.0339(7) Uani 0.50 1 d PD A 4
O1S O 0.5923(4) 0.7533(4) 0.0844(3) 0.0847(15) Uiso 0.791(5) 1 d PD A 7
C1S C 0.6417(5) 0.7322(6) 0.0646(5) 0.0847(15) Uiso 0.791(5) 1 d PD A 7
H1S1 H 0.6206 0.7244 0.0160 0.127 Uiso 0.791(5) 1 calc PR A 7
H1S2 H 0.6634 0.6849 0.0872 0.127 Uiso 0.791(5) 1 calc PR A 7
H1S3 H 0.6763 0.7724 0.0765 0.127 Uiso 0.791(5) 1 calc PR A 7
C2S C 0.6348(18) 0.733(2) 0.1069(16) 0.0847(15) Uiso 0.209(5) 1 d PD A -8
H2S1 H 0.5944 0.7008 0.0829 0.127 Uiso 0.209(5) 1 calc PR A -8
H2S2 H 0.6222 0.7864 0.0973 0.127 Uiso 0.209(5) 1 calc PR A -8
H2S3 H 0.6525 0.7236 0.1552 0.127 Uiso 0.209(5) 1 calc PR A -8
C3S C 0.6924(15) 0.712(2) 0.0829(11) 0.0847(15) Uiso 0.209(5) 1 d PD A -8
H3S1 H 0.7331 0.7445 0.1058 0.102 Uiso 0.209(5) 1 calc PR A -8
H3S2 H 0.7066 0.6579 0.0935 0.102 Uiso 0.209(5) 1 calc PR A -8
C4S C 0.7067(14) 0.6972(16) -0.0220(14) 0.0847(15) Uiso 0.209(5) 1 d PD A -8
H4S1 H 0.6792 0.6908 -0.0709 0.102 Uiso 0.209(5) 1 calc PR A -8
H4S2 H 0.7273 0.6475 -0.0027 0.102 Uiso 0.209(5) 1 calc PR A -8
C5S C 0.7640(15) 0.758(2) -0.0081(19) 0.0847(15) Uiso 0.209(5) 1 d PD A -8
H5S1 H 0.7981 0.7538 0.0388 0.127 Uiso 0.209(5) 1 calc PR A -8
H5S2 H 0.7439 0.8086 -0.0167 0.127 Uiso 0.209(5) 1 calc PR A -8
H5S3 H 0.7861 0.7479 -0.0376 0.127 Uiso 0.209(5) 1 calc PR A -8
O2S O 0.6619(10) 0.7244(13) 0.0095(10) 0.0847(15) Uiso 0.209(5) 1 d PD A -8
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
O1 Ni1 O2 80.73(11) . .
O1 Ni1 O1 77.73(11) . 2_655
O2 Ni1 O1 78.51(11) . 2_655
O1 Ni1 N11 94.79(12) . .
O2 Ni1 N11 175.33(12) . .
O1 Ni1 N11 101.91(12) 2_655 .
O1 Ni1 N21 105.13(12) . .
O2 Ni1 N21 95.04(12) . .
O1 Ni1 N21 172.54(12) 2_655 .
N11 Ni1 N21 84.83(13) . .
O1 Ni1 O3A 170.98(12) . .
O2 Ni1 O3A 96.80(12) . .
O1 Ni1 O3A 93.29(12) 2_655 .
N11 Ni1 O3A 87.82(12) . .
N21 Ni1 O3A 83.68(14) . .
O2 Ni2 O1 78.45(11) 2_655 .
O2 Ni2 O2 80.89(12) 2_655 .
O1 Ni2 O2 80.19(11) . .
O2 Ni2 O4A 95.49(12) 2_655 .
O1 Ni2 O4A 170.94(11) . .
O2 Ni2 O4A 92.27(11) . .
O2 Ni2 N41 97.68(12) 2_655 .
O1 Ni2 N41 95.10(12) . .
O2 Ni2 N41 175.26(12) . .
O4A Ni2 N41 92.37(13) . .
O2 Ni2 N31 174.84(12) 2_655 .
O1 Ni2 N31 105.25(12) . .
O2 Ni2 N31 96.09(12) . .
O4A Ni2 N31 80.40(13) . .
N41 Ni2 N31 85.66(14) . .
N22 C1 N12 110.1(3) . .
N22 C1 C3 112.1(4) . .
N12 C1 C3 112.0(4) . .
N22 C1 H1 107.4 . .
N12 C1 H1 107.4 . .
C3 C1 H1 107.4 . .
N32 C2 N42 110.1(3) . .
N32 C2 C5 112.3(3) . .
N42 C2 C5 111.9(3) . .
N32 C2 H2 107.4 . .
N42 C2 H2 107.4 . .
C5 C2 H2 107.4 . .
C4 C3 C8 119.6(4) . .
C4 C3 C1 121.1(4) . .
C8 C3 C1 119.2(4) . .
C3 C4 C5 120.6(4) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C4 C5 C6 119.5(4) . .
C4 C5 C2 121.1(4) . .
C6 C5 C2 119.3(4) . .
C7 C6 C5 119.3(4) . .
C7 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C8 C7 C6 121.2(4) . .
C8 C7 H7 119.4 . .
C6 C7 H7 119.4 . .
C7 C8 C3 119.4(4) . .
C7 C8 H8 120.3 . .
C3 C8 H8 120.3 . .
C12 C11 N12 107.8(4) . .
C12 C11 H11 126.1 . .
N12 C11 H11 126.1 . .
C11 C12 C13 104.9(4) . .
C11 C12 H12 127.5 . .
C13 C12 H12 127.5 . .
N11 C13 C12 112.0(4) . .
N11 C13 H13 124.0 . .
C12 C13 H13 124.0 . .
N22 C21 C22 107.5(4) . .
N22 C21 H21 126.2 . .
C22 C21 H21 126.2 . .
C21 C22 C23 106.1(4) . .
C21 C22 H22 126.9 . .
C23 C22 H22 126.9 . .
N21 C23 C22 110.7(4) . .
N21 C23 H23 124.6 . .
C22 C23 H23 124.6 . .
N32 C31 C32 107.4(4) . .
N32 C31 H31 126.3 . .
C32 C31 H31 126.3 . .
C31 C32 C33 105.6(4) . .
C31 C32 H32 127.2 . .
C33 C32 H32 127.2 . .
N31 C33 C32 111.6(4) . .
N31 C33 H33 124.2 . .
C32 C33 H33 124.2 . .
N42 C41 C42 107.5(4) . .
N42 C41 H41 126.2 . .
C42 C41 H41 126.2 . .
C41 C42 C43 105.0(4) . .
C41 C42 H42 127.5 . .
C43 C42 H42 127.5 . .
N41 C43 C42 112.1(4) . .
N41 C43 H43 123.9 . .
C42 C43 H43 123.9 . .
C13 N11 N12 104.4(3) . .
C13 N11 Ni1 128.7(3) . .
N12 N11 Ni1 126.0(3) . .
N11 N12 C11 110.8(4) . .
N11 N12 C1 122.1(3) . .
C11 N12 C1 126.8(4) . .
C23 N21 N22 104.8(3) . .
C23 N21 Ni1 128.0(3) . .
N22 N21 Ni1 126.0(3) . .
C21 N22 N21 110.9(4) . .
C21 N22 C1 127.9(4) . .
N21 N22 C1 121.0(3) . .
C33 N31 N32 104.4(3) . .
C33 N31 Ni2 127.4(3) . .
N32 N31 Ni2 125.1(3) . .
C31 N32 N31 111.0(4) . .
C31 N32 C2 128.5(4) . .
N31 N32 C2 120.5(3) . .
C43 N41 N42 104.3(3) . .
C43 N41 Ni2 128.4(3) . .
N42 N41 Ni2 125.4(3) . .
C41 N42 N41 111.1(4) . .
C41 N42 C2 127.6(4) . .
N41 N42 C2 121.2(3) . .
Ni1 O1 Ni1 101.44(11) . 2_655
Ni1 O1 Ni2 98.20(11) . .
Ni1 O1 Ni2 100.69(12) 2_655 .
Ni1 O1 H1A 111(4) . .
Ni1 O1 H1A 125(4) 2_655 .
Ni2 O1 H1A 117(4) . .
Ni2 O2 Ni1 101.23(12) 2_655 .
Ni2 O2 Ni2 98.21(12) 2_655 .
Ni1 O2 Ni2 98.06(11) . .
Ni2 O2 H2A 122(4) 2_655 .
Ni1 O2 H2A 125(4) . .
Ni2 O2 H2A 105(4) . .
Ni1 O3A H3A 108(4) . .
Ni1 O3A H3B 132(5) . .
H3A O3A H3B 107(3) . .
O12A Cl1A O11A 108.5(4) . .
O12A Cl1A O14A 110.4(4) . .
O11A Cl1A O14A 114.3(4) . .
O12A Cl1A O13A 108.6(4) . .
O11A Cl1A O13A 105.5(4) . .
O14A Cl1A O13A 109.3(4) . .
O14B Cl1B O11B 95.6(10) . .
O14B Cl1B O13B 115.3(13) . .
O11B Cl1B O13B 122.9(12) . .
O14B Cl1B O12B 112.8(10) . .
O11B Cl1B O12B 113.1(10) . .
O13B Cl1B O12B 98.1(12) . .
O21 Cl2 O23 111.8(4) . .
O21 Cl2 O24 111.4(4) . .
O23 Cl2 O24 105.4(3) . .
O21 Cl2 O22 110.9(3) . .
O23 Cl2 O22 109.3(2) . .
O24 Cl2 O22 107.9(3) . .
O5 C51 N5 124.7(6) . .
O5 C51 H51 117.6 . .
N5 C51 H51 117.6 . .
N5 C52 H52A 109.5 . .
N5 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
N5 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
N5 C53 H53A 109.5 . .
N5 C53 H53B 109.5 . .
H53A C53 H53B 109.5 . .
N5 C53 H53C 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
C51 N5 C52 120.0(5) . .
C51 N5 C53 121.7(5) . .
C52 N5 C53 118.3(5) . .
O4A C44A N4A 123.8(9) . .
O4A C44A H44A 118.1 . .
N4A C44A H44A 118.1 . .
N4A C45A H45A 109.5 . .
N4A C45A H45B 109.5 . .
H45A C45A H45B 109.5 . .
N4A C45A H45C 109.5 . .
H45A C45A H45C 109.5 . .
H45B C45A H45C 109.5 . .
N4A C46A H46A 109.5 . .
N4A C46A H46B 109.5 . .
H46A C46A H46B 109.5 . .
N4A C46A H46C 109.5 . .
H46A C46A H46C 109.5 . .
H46B C46A H46C 109.5 . .
C44A N4A C45A 119.2(9) . .
C44A N4A C46A 122.3(8) . .
C45A N4A C46A 117.6(9) . .
C44A O4A Ni2 130.3(5) . .
N4B C44B H44B 117.1 . .
N4B C45B H45D 109.5 . .
N4B C45B H45E 109.5 . .
H45D C45B H45E 109.5 . .
N4B C45B H45F 109.5 . .
H45D C45B H45F 109.5 . .
H45E C45B H45F 109.5 . .
N4B C46B H46D 109.5 . .
N4B C46B H46E 109.5 . .
H46D C46B H46E 109.5 . .
N4B C46B H46F 109.5 . .
H46D C46B H46F 109.5 . .
H46E C46B H46F 109.5 . .
C44B N4B C45B 122.2(9) . .
C44B N4B C46B 120.5(9) . .
C45B N4B C46B 117.0(9) . .
C3S C2S H2S1 109.5 . .
C3S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
C3S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
O2S C3S C2S 106.8(16) . .
O2S C3S H3S1 110.4 . .
C2S C3S H3S1 110.4 . .
O2S C3S H3S2 110.4 . .
C2S C3S H3S2 110.4 . .
H3S1 C3S H3S2 108.6 . .
O2S C4S C5S 108.5(16) . .
O2S C4S H4S1 110.0 . .
C5S C4S H4S1 110.0 . .
O2S C4S H4S2 110.0 . .
C5S C4S H4S2 110.0 . .
H4S1 C4S H4S2 108.4 . .
C4S C5S H5S1 109.5 . .
C4S C5S H5S2 109.5 . .
H5S1 C5S H5S2 109.5 . .
C4S C5S H5S3 109.5 . .
H5S1 C5S H5S3 109.5 . .
H5S2 C5S H5S3 109.5 . .
C3S O2S C4S 113.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.056(3) .
Ni1 O2 2.058(3) .
Ni1 O1 2.063(3) 2_655
Ni1 N11 2.095(3) .
Ni1 N21 2.108(3) .
Ni1 O3A 2.115(3) .
Ni2 O2 2.056(3) 2_655
Ni2 O1 2.067(3) .
Ni2 O2 2.070(3) .
Ni2 O4A 2.071(3) .
Ni2 N41 2.099(3) .
Ni2 N31 2.123(4) .
C1 N22 1.444(6) .
C1 N12 1.456(5) .
C1 C3 1.523(6) .
C1 H1 1.0000 .
C2 N32 1.438(5) .
C2 N42 1.457(5) .
C2 C5 1.519(6) .
C2 H2 1.0000 .
C3 C4 1.386(6) .
C3 C8 1.396(6) .
C4 C5 1.388(6) .
C4 H4 0.9500 .
C5 C6 1.398(6) .
C6 C7 1.385(6) .
C6 H6 0.9500 .
C7 C8 1.382(6) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C11 C12 1.348(7) .
C11 N12 1.360(5) .
C11 H11 0.9500 .
C12 C13 1.387(6) .
C12 H12 0.9500 .
C13 N11 1.331(5) .
C13 H13 0.9500 .
C21 N22 1.347(6) .
C21 C22 1.353(7) .
C21 H21 0.9500 .
C22 C23 1.382(7) .
C22 H22 0.9500 .
C23 N21 1.340(5) .
C23 H23 0.9500 .
C31 N32 1.353(6) .
C31 C32 1.358(7) .
C31 H31 0.9500 .
C32 C33 1.386(6) .
C32 H32 0.9500 .
C33 N31 1.334(6) .
C33 H33 0.9500 .
C41 N42 1.351(5) .
C41 C42 1.367(6) .
C41 H41 0.9500 .
C42 C43 1.385(6) .
C42 H42 0.9500 .
C43 N41 1.333(5) .
C43 H43 0.9500 .
N11 N12 1.354(5) .
N21 N22 1.364(5) .
N31 N32 1.369(5) .
N41 N42 1.368(4) .
O1 Ni1 2.063(3) 2_655
O1 H1A 0.83(2) .
O2 Ni2 2.056(3) 2_655
O2 H2A 0.83(2) .
O3A H3A 0.850(10) .
O3A H3B 0.859(10) .
C34 H3B 0.69(4) .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
Cl1A O12A 1.414(7) .
Cl1A O11A 1.428(6) .
Cl1A O14A 1.430(7) .
Cl1A O13A 1.442(6) .
Cl1B O14B 1.364(16) .
Cl1B O11B 1.405(16) .
Cl1B O13B 1.42(2) .
Cl1B O12B 1.424(17) .
Cl2 O21 1.386(4) .
Cl2 O23 1.418(4) .
Cl2 O24 1.427(5) .
Cl2 O22 1.434(4) .
C51 O5 1.242(7) .
C51 N5 1.330(6) .
C51 H51 0.9500 .
C52 N5 1.433(6) .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C53 N5 1.457(7) .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
C44A O4A 1.225(8) .
C44A N4A 1.318(9) .
C44A H44A 0.9500 .
C45A N4A 1.452(10) .
C45A H45A 0.9800 .
C45A H45B 0.9800 .
C45A H45C 0.9800 .
C46A N4A 1.458(9) .
C46A H46A 0.9800 .
C46A H46B 0.9800 .
C46A H46C 0.9800 .
C44B N4B 1.320(9) .
C44B H44B 0.9500 .
C45B N4B 1.427(10) .
C45B H45D 0.9800 .
C45B H45E 0.9800 .
C45B H45F 0.9800 .
C46B N4B 1.470(11) .
C46B H46D 0.9800 .
C46B H46E 0.9800 .
C46B H46F 0.9800 .
O1S C1S 1.376(10) .
C1S H1S1 0.9800 .
C1S H1S2 0.9800 .
C1S H1S3 0.9800 .
C2S C3S 1.604(19) .
C2S H2S1 0.9800 .
C2S H2S2 0.9800 .
C2S H2S3 0.9800 .
C3S O2S 1.482(18) .
C3S H3S1 0.9900 .
C3S H3S2 0.9900 .
C4S O2S 1.503(17) .
C4S C5S 1.560(19) .
C4S H4S1 0.9900 .
C4S H4S2 0.9900 .
C5S H5S1 0.9800 .
C5S H5S2 0.9800 .
C5S H5S3 0.9800 .
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
O2 H2A O11A 0.83(2) 2.24(3) 3.024(6) 157(5)
O2 H2A O11B 0.83(2) 2.19(3) 2.988(14) 161(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N22 C1 C3 C4 6.6(5) . .
N12 C1 C3 C4 131.0(4) . .
N22 C1 C3 C8 -171.0(4) . .
N12 C1 C3 C8 -46.6(5) . .
C8 C3 C4 C5 6.4(6) . .
C1 C3 C4 C5 -171.1(4) . .
C3 C4 C5 C6 -5.5(6) . .
C3 C4 C5 C2 173.3(4) . .
N32 C2 C5 C4 -7.6(5) . .
N42 C2 C5 C4 -132.0(4) . .
N32 C2 C5 C6 171.1(4) . .
N42 C2 C5 C6 46.8(5) . .
C4 C5 C6 C7 0.8(6) . .
C2 C5 C6 C7 -178.0(4) . .
C5 C6 C7 C8 2.9(7) . .
C6 C7 C8 C3 -2.0(7) . .
C4 C3 C8 C7 -2.7(6) . .
C1 C3 C8 C7 174.9(4) . .
N12 C11 C12 C13 0.2(5) . .
C11 C12 C13 N11 1.0(6) . .
N22 C21 C22 C23 1.1(6) . .
C21 C22 C23 N21 -1.5(6) . .
N32 C31 C32 C33 -0.1(6) . .
C31 C32 C33 N31 0.4(6) . .
N42 C41 C42 C43 0.0(5) . .
C41 C42 C43 N41 -0.3(5) . .
C12 C13 N11 N12 -1.8(5) . .
C12 C13 N11 Ni1 -171.1(3) . .
O1 Ni1 N11 C13 -107.8(4) . .
O1 Ni1 N11 C13 -29.3(4) 2_655 .
N21 Ni1 N11 C13 147.4(4) . .
O3A Ni1 N11 C13 63.6(4) . .
O1 Ni1 N11 N12 85.0(3) . .
O1 Ni1 N11 N12 163.5(3) 2_655 .
N21 Ni1 N11 N12 -19.8(3) . .
O3A Ni1 N11 N12 -103.6(3) . .
C13 N11 N12 C11 1.9(5) . .
Ni1 N11 N12 C11 171.6(3) . .
C13 N11 N12 C1 176.6(4) . .
Ni1 N11 N12 C1 -13.7(5) . .
C12 C11 N12 N11 -1.3(5) . .
C12 C11 N12 C1 -175.7(4) . .
N22 C1 N12 N11 57.2(5) . .
C3 C1 N12 N11 -68.4(5) . .
N22 C1 N12 C11 -129.1(4) . .
C3 C1 N12 C11 105.4(5) . .
C22 C23 N21 N22 1.4(5) . .
C22 C23 N21 Ni1 168.9(3) . .
O1 Ni1 N21 C23 119.7(3) . .
O2 Ni1 N21 C23 38.0(4) . .
N11 Ni1 N21 C23 -146.7(4) . .
O3A Ni1 N21 C23 -58.3(4) . .
O1 Ni1 N21 N22 -75.2(3) . .
O2 Ni1 N21 N22 -157.0(3) . .
N11 Ni1 N21 N22 18.4(3) . .
O3A Ni1 N21 N22 106.7(3) . .
C22 C21 N22 N21 -0.3(5) . .
C22 C21 N22 C1 174.0(4) . .
C23 N21 N22 C21 -0.7(5) . .
Ni1 N21 N22 C21 -168.5(3) . .
C23 N21 N22 C1 -175.4(4) . .
Ni1 N21 N22 C1 16.8(5) . .
N12 C1 N22 C21 128.0(4) . .
C3 C1 N22 C21 -106.6(5) . .
N12 C1 N22 N21 -58.3(5) . .
C3 C1 N22 N21 67.1(5) . .
C32 C33 N31 N32 -0.5(5) . .
C32 C33 N31 Ni2 -161.2(3) . .
O1 Ni2 N31 C33 -124.2(4) . .
O2 Ni2 N31 C33 -42.7(4) . .
O4A Ni2 N31 C33 48.5(4) . .
N41 Ni2 N31 C33 141.7(4) . .
O1 Ni2 N31 N32 78.9(3) . .
O2 Ni2 N31 N32 160.4(3) . .
O4A Ni2 N31 N32 -108.3(3) . .
N41 Ni2 N31 N32 -15.2(3) . .
C32 C31 N32 N31 -0.2(6) . .
C32 C31 N32 C2 -177.3(4) . .
C33 N31 N32 C31 0.5(5) . .
Ni2 N31 N32 C31 161.7(3) . .
C33 N31 N32 C2 177.8(4) . .
Ni2 N31 N32 C2 -21.0(5) . .
N42 C2 N32 C31 -121.1(5) . .
C5 C2 N32 C31 113.6(5) . .
N42 C2 N32 N31 62.1(5) . .
C5 C2 N32 N31 -63.2(5) . .
C42 C43 N41 N42 0.4(5) . .
C42 C43 N41 Ni2 165.3(3) . .
O2 Ni2 N41 C43 31.4(4) 2_655 .
O1 Ni2 N41 C43 110.4(4) . .
O4A Ni2 N41 C43 -64.4(4) . .
N31 Ni2 N41 C43 -144.6(4) . .
O2 Ni2 N41 N42 -166.6(3) 2_655 .
O1 Ni2 N41 N42 -87.6(3) . .
O4A Ni2 N41 N42 97.5(3) . .
N31 Ni2 N41 N42 17.3(3) . .
C42 C41 N42 N41 0.2(5) . .
C42 C41 N42 C2 178.1(4) . .
C43 N41 N42 C41 -0.4(5) . .
Ni2 N41 N42 C41 -165.8(3) . .
C43 N41 N42 C2 -178.4(4) . .
Ni2 N41 N42 C2 16.1(5) . .
N32 C2 N42 C41 122.5(4) . .
C5 C2 N42 C41 -111.9(5) . .
N32 C2 N42 N41 -59.8(5) . .
C5 C2 N42 N41 65.8(5) . .
O2 Ni1 O1 Ni1 -89.95(12) . 2_655
O1 Ni1 O1 Ni1 -9.80(15) 2_655 2_655
N11 Ni1 O1 Ni1 91.37(13) . 2_655
N21 Ni1 O1 Ni1 177.29(12) . 2_655
O2 Ni1 O1 Ni2 12.78(11) . .
O1 Ni1 O1 Ni2 92.93(9) 2_655 .
N11 Ni1 O1 Ni2 -165.90(12) . .
N21 Ni1 O1 Ni2 -79.98(13) . .
O2 Ni2 O1 Ni1 -95.34(12) 2_655 .
O2 Ni2 O1 Ni1 -12.73(11) . .
N41 Ni2 O1 Ni1 167.85(12) . .
N31 Ni2 O1 Ni1 80.97(14) . .
O2 Ni2 O1 Ni1 8.03(11) 2_655 2_655
O2 Ni2 O1 Ni1 90.64(12) . 2_655
N41 Ni2 O1 Ni1 -88.79(13) . 2_655
N31 Ni2 O1 Ni1 -175.67(12) . 2_655
O1 Ni1 O2 Ni2 87.33(12) . 2_655
O1 Ni1 O2 Ni2 8.08(11) 2_655 2_655
N21 Ni1 O2 Ni2 -168.13(13) . 2_655
O3A Ni1 O2 Ni2 -83.91(14) . 2_655
O1 Ni1 O2 Ni2 -12.76(11) . .
O1 Ni1 O2 Ni2 -92.01(12) 2_655 .
N21 Ni1 O2 Ni2 91.79(13) . .
O3A Ni1 O2 Ni2 176.00(13) . .
O2 Ni2 O2 Ni2 -10.21(15) 2_655 2_655
O1 Ni2 O2 Ni2 -89.95(12) . 2_655
O4A Ni2 O2 Ni2 84.99(13) . 2_655
N31 Ni2 O2 Ni2 165.57(12) . 2_655
O2 Ni2 O2 Ni1 92.45(10) 2_655 .
O1 Ni2 O2 Ni1 12.71(11) . .
O4A Ni2 O2 Ni1 -172.35(12) . .
N31 Ni2 O2 Ni1 -91.77(13) . .
O5 C51 N5 C52 -5.2(9) . .
O5 C51 N5 C53 176.2(6) . .
O4A C44A N4A C45A 17.6(18) . .
O4A C44A N4A C46A -173.3(10) . .
N4A C44A O4A Ni2 -159.5(7) . .
O2 Ni2 O4A C44A -65.4(7) 2_655 .
O2 Ni2 O4A C44A -146.4(7) . .
N41 Ni2 O4A C44A 32.6(8) . .
N31 Ni2 O4A C44A 117.8(7) . .
