#------------------------------------------------------------------------------
#$Date: 2016-10-08 00:15:26 +0200 (Sat 08 de Oct de 2016) $
#$Revision: 187110 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/00/7040088.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_7040088
loop_
_publ_author_name
'Arora, Himanshu'
'Cano, Joan'
'Lloret, Francesc'
'Mukherjee, Rabindranath'
_publ_section_title
;
 A carboxylate-bridged Ni cluster with a distorted cubane topology:
 structure, magnetism and density functional studies.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14174
_journal_page_last               14183
_journal_paper_doi               10.1039/c6dt01833e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C96 H154 Cl4 N14 Ni8 O56'
_chemical_formula_sum            'C96 H154 Cl4 N14 Ni8 O56'
_chemical_formula_weight         3011.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2016-07-31 deposited with the CCDC.
2016-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.096(5)
_cell_angle_beta                 106.057(5)
_cell_angle_gamma                103.057(5)
_cell_formula_units_Z            1
_cell_length_a                   13.536(5)
_cell_length_b                   15.627(5)
_cell_length_c                   15.848(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.308
_cell_measurement_theta_min      2.189
_cell_volume                     3002.8(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19942
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.733
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         14286
_refine_ls_number_restraints     820
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1361P)²+7.9932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8925
_reflns_number_total             14286
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01833e2.cif
_cod_data_source_block           17sepam
_cod_depositor_comments          'Adding full bibliography for 7040088.cif.'
_cod_database_code               7040088
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.538
_shelx_estimated_absorpt_t_max   0.871
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
NI1 Ni 0.27441(7) 0.63047(6) 0.39787(6) 0.0225(2) Uani 1 1 d . .
NI2 Ni 0.28624(7) 0.55065(6) 0.61349(6) 0.0219(2) Uani 1 1 d . .
NI3 Ni 0.04130(7) 0.27823(6) 0.29371(6) 0.0218(2) Uani 1 1 d . .
NI4 Ni 0.11680(7) 0.88983(6) 0.52674(6) 0.0244(2) Uani 1 1 d . .
CL1 Cl 0.33554(18) 0.94852(15) 0.24778(15) 0.0446(5) Uani 1 1 d . .
CL2 Cl 0.26334(18) 0.37411(17) -0.02064(16) 0.0507(6) Uani 1 1 d . .
O1 O 0.2475(4) 0.7457(3) 0.4612(3) 0.0230(9) Uani 1 1 d . .
O2 O 0.2455(4) 0.8903(3) 0.4845(4) 0.0278(10) Uani 1 1 d . .
O3 O 0.3443(4) 0.6150(3) 0.5239(3) 0.0227(9) Uani 1 1 d . .
O4 O 0.4398(4) 0.5445(3) 0.6028(3) 0.0260(10) Uani 1 1 d . .
O5 O 0.1494(4) 0.5864(3) 0.5866(3) 0.0262(10) Uani 1 1 d . .
O6 O 0.0442(4) 0.6568(3) 0.6352(3) 0.0260(10) Uani 1 1 d . .
O7 O 0.2145(4) 0.4391(3) 0.5042(3) 0.0246(10) Uani 1 1 d . .
O8 O 0.1456(4) 0.2927(3) 0.4241(3) 0.0215(9) Uani 1 1 d . .
O9 O 0.1313(4) 0.4035(3) 0.2949(3) 0.0245(10) Uani 1 1 d . .
O10 O 0.2920(4) 0.5060(3) 0.3395(3) 0.0261(10) Uani 1 1 d . .
O11 O -0.0382(4) 0.1557(3) 0.3125(3) 0.0254(10) Uani 1 1 d . .
O12 O -0.0090(4) 0.9058(3) 0.5735(3) 0.0275(10) Uani 1 1 d . .
O13 O 0.1250(3) 0.5615(3) 0.4038(3) 0.0225(9) Uani 1 1 d . .
H13A H 0.128255 0.571490 0.458884 0.034 Uiso 1 1 d R U
H13B H 0.110155 0.503420 0.380904 0.034 Uiso 1 1 d R U
O14 O 0.0717(4) 0.7500(3) 0.5058(3) 0.0274(10) Uani 1 1 d . .
H14A H 0.081926 0.738575 0.558478 0.041 Uiso 1 1 d R U
H14B H 0.110716 0.726424 0.478068 0.041 Uiso 1 1 d R U
O15 O 0.2194(4) 0.9064(4) 0.6584(3) 0.0307(11) Uani 1 1 d . .
H15A H 0.270078 0.955214 0.675613 0.046 Uiso 1 1 d R U
H15B H 0.184738 0.890624 0.692692 0.046 Uiso 1 1 d R U
O16 O 0.1586(4) 1.0310(3) 0.5453(3) 0.0288(11) Uani 1 1 d . .
H16 H 0.114204 1.049741 0.510042 0.043 Uiso 1 1 d R U
O17 O 0.0141(4) 0.8723(3) 0.3989(3) 0.0277(10) Uani 1 1 d . .
O18 O 0.2726(6) 0.8582(6) 0.2357(6) 0.084(3) Uani 1 1 d . .
O19 O 0.3218(11) 1.0120(8) 0.3144(7) 0.118(4) Uani 1 1 d . .
O20 O 0.3090(10) 0.9721(6) 0.1669(6) 0.116(4) Uani 1 1 d . .
O21 O 0.4441(7) 0.9525(7) 0.2798(9) 0.110(4) Uani 1 1 d . .
O22 O 0.3632(7) 0.4414(8) 0.0113(8) 0.130(5) Uani 1 1 d . .
O23 O 0.2662(6) 0.2936(6) 0.0063(5) 0.074(2) Uani 1 1 d . .
O24 O 0.1884(8) 0.4086(7) 0.0157(6) 0.093(3) Uani 1 1 d . .
O25 O 0.2173(6) 0.3518(5) -0.1180(5) 0.0571(17) Uani 1 1 d . .
C5S C 0.1750(13) 1.0206(10) -0.0249(9) 0.105(5) Uani 1 1 d D .
H3SA H 0.187725 0.972112 -0.064872 0.158 Uiso 1 1 calc R U
H3SB H 0.241970 1.068070 0.009387 0.158 Uiso 1 1 calc R U
H3SC H 0.125641 1.045443 -0.060862 0.158 Uiso 1 1 calc R U
N1 N 0.1989(5) 0.6367(4) 0.2684(4) 0.0269(12) Uani 1 1 d . .
N2 N 0.4297(4) 0.7048(4) 0.4054(4) 0.0232(11) Uani 1 1 d . .
N3 N 0.3752(5) 0.6724(4) 0.7152(4) 0.0259(12) Uani 1 1 d . .
N4 N 0.2559(4) 0.4813(4) 0.7057(4) 0.0232(11) Uani 1 1 d . .
N5 N -0.0875(4) 0.2436(4) 0.1708(4) 0.0241(11) Uani 1 1 d . .
N6 N 0.1278(4) 0.2084(4) 0.2254(4) 0.0237(11) Uani 1 1 d . .
N7 N -0.0256(5) 0.8614(4) 0.2497(4) 0.0325(14) Uani 1 1 d . .
C1 C 0.0955(6) 0.6351(5) 0.2447(5) 0.0325(16) Uani 1 1 d . .
H1 H 0.065392 0.644541 0.290663 0.039 Uiso 1 1 calc R U
C2 C 0.0304(7) 0.6199(6) 0.1538(6) 0.0397(18) Uani 1 1 d . .
H2 H -0.041282 0.619228 0.139282 0.048 Uiso 1 1 calc R U
C3 C 0.0761(7) 0.6063(6) 0.0877(6) 0.0430(19) Uani 1 1 d . .
H3 H 0.034769 0.594292 0.026505 0.052 Uiso 1 1 calc R U
C4 C 0.1840(7) 0.6102(6) 0.1108(5) 0.0394(18) Uani 1 1 d . .
H4 H 0.215371 0.601529 0.065686 0.047 Uiso 1 1 calc R U
C5 C 0.2441(6) 0.6271(5) 0.2019(5) 0.0282(14) Uani 1 1 d . .
C6 C 0.3641(6) 0.6365(6) 0.2329(6) 0.0383(17) Uani 1 1 d . .
H6A H 0.374663 0.581633 0.248379 0.046 Uiso 1 1 calc R U
H6B H 0.390649 0.641958 0.182745 0.046 Uiso 1 1 calc R U
C7 C 0.4286(6) 0.7199(5) 0.3157(5) 0.0328(15) Uani 1 1 d . .
H7A H 0.502377 0.738633 0.316646 0.039 Uiso 1 1 calc R U
H7B H 0.399010 0.769981 0.308366 0.039 Uiso 1 1 calc R U
C8 C 0.4688(5) 0.7938(5) 0.4784(5) 0.0266(14) Uani 1 1 d . .
H8A H 0.541946 0.824543 0.483632 0.032 Uiso 1 1 calc R U
H8B H 0.471760 0.781061 0.536250 0.032 Uiso 1 1 calc R U
C9 C 0.4020(5) 0.8600(5) 0.4648(5) 0.0282(15) Uani 1 1 d . .
H9A H 0.441389 0.918760 0.510672 0.034 Uiso 1 1 calc R U
H9B H 0.394547 0.869478 0.405068 0.034 Uiso 1 1 calc R U
C10 C 0.2897(5) 0.8284(5) 0.4710(5) 0.0239(13) Uani 1 1 d . .
C11 C 0.5048(5) 0.6512(5) 0.4289(5) 0.0260(14) Uani 1 1 d . .
H11A H 0.573328 0.682897 0.425462 0.031 Uiso 1 1 calc R U
H11B H 0.477002 0.592327 0.382090 0.031 Uiso 1 1 calc R U
C12 C 0.5265(5) 0.6330(5) 0.5225(5) 0.0290(15) Uani 1 1 d . .
H12A H 0.570937 0.592219 0.525213 0.035 Uiso 1 1 calc R U
H12B H 0.568837 0.690721 0.569083 0.035 Uiso 1 1 calc R U
C13 C 0.4310(5) 0.5923(5) 0.5485(4) 0.0231(13) Uani 1 1 d . .
C14 C 0.3759(6) 0.7517(5) 0.6970(5) 0.0308(15) Uani 1 1 d . .
H14 H 0.320872 0.752510 0.646975 0.037 Uiso 1 1 calc R U
C15 C 0.4551(7) 0.8325(6) 0.7493(6) 0.0385(17) Uani 1 1 d . .
H15 H 0.453112 0.886938 0.734862 0.046 Uiso 1 1 calc R U
C16 C 0.5376(7) 0.8321(6) 0.8234(6) 0.0396(18) Uani 1 1 d . .
H16A H 0.593254 0.885498 0.858674 0.048 Uiso 1 1 calc R U
C17 C 0.5349(6) 0.7501(5) 0.8437(5) 0.0332(16) Uani 1 1 d . .
H17 H 0.587671 0.748050 0.894639 0.040 Uiso 1 1 calc R U
C18 C 0.4533(6) 0.6708(5) 0.7878(5) 0.0292(14) Uani 1 1 d . .
C19 C 0.4452(6) 0.5778(5) 0.8048(5) 0.0317(15) Uani 1 1 d . .
H19A H 0.496823 0.586088 0.864484 0.038 Uiso 1 1 calc R U
H19B H 0.464260 0.539751 0.758954 0.038 Uiso 1 1 calc R U
C20 C 0.3331(5) 0.5281(5) 0.8018(5) 0.0281(14) Uani 1 1 d . .
H20A H 0.338544 0.482721 0.834816 0.034 Uiso 1 1 calc R U
H20B H 0.304721 0.572003 0.832698 0.034 Uiso 1 1 calc R U
C21 C 0.2703(5) 0.3893(5) 0.6762(5) 0.0251(13) Uani 1 1 d . .
H21A H 0.263881 0.358881 0.722746 0.030 Uiso 1 1 calc R U
H21B H 0.343482 0.398759 0.675863 0.030 Uiso 1 1 calc R U
C22 C 0.1945(6) 0.3235(5) 0.5835(4) 0.0248(13) Uani 1 1 d . .
H22A H 0.216735 0.268400 0.574040 0.030 Uiso 1 1 calc R U
H22B H 0.122837 0.305814 0.587379 0.030 Uiso 1 1 calc R U
C23 C 0.1857(5) 0.3559(4) 0.4983(4) 0.0201(12) Uani 1 1 d . .
C24 C 0.1429(5) 0.4711(5) 0.7055(5) 0.0257(14) Uani 1 1 d . .
H24A H 0.132511 0.442870 0.752664 0.031 Uiso 1 1 calc R U
H24B H 0.093009 0.429914 0.646855 0.031 Uiso 1 1 calc R U
C25 C 0.1156(6) 0.5605(5) 0.7219(5) 0.0254(14) Uani 1 1 d . .
H25A H 0.172757 0.604782 0.775184 0.030 Uiso 1 1 calc R U
H25B H 0.049951 0.550207 0.736907 0.030 Uiso 1 1 calc R U
C26 C 0.1001(5) 0.6033(5) 0.6426(4) 0.0191(12) Uani 1 1 d . .
C27 C -0.1891(6) 0.2195(5) 0.1724(5) 0.0308(15) Uani 1 1 d . .
H27 H -0.199318 0.217105 0.227604 0.037 Uiso 1 1 calc R U
C28 C -0.2785(6) 0.1982(6) 0.0949(5) 0.0366(17) Uani 1 1 d . .
H28 H -0.347634 0.183301 0.098053 0.044 Uiso 1 1 calc R U
C29 C -0.2630(7) 0.1995(7) 0.0127(6) 0.045(2) Uani 1 1 d . .
H29 H -0.321715 0.185894 -0.040494 0.054 Uiso 1 1 calc R U
C30 C -0.1604(7) 0.2209(6) 0.0104(5) 0.0399(18) Uani 1 1 d . .
H30 H -0.149143 0.220656 -0.044978 0.048 Uiso 1 1 calc R U
C31 C -0.0723(6) 0.2432(5) 0.0906(5) 0.0273(14) Uani 1 1 d . .
C32 C 0.0414(6) 0.2673(5) 0.0924(5) 0.0282(14) Uani 1 1 d . .
H32A H 0.080249 0.328985 0.132627 0.034 Uiso 1 1 calc R U
H32B H 0.042250 0.266317 0.031202 0.034 Uiso 1 1 calc R U
C33 C 0.0986(6) 0.1996(5) 0.1261(5) 0.0275(14) Uani 1 1 d . .
H33A H 0.052084 0.137636 0.092433 0.033 Uiso 1 1 calc R U
H33B H 0.163894 0.207400 0.110645 0.033 Uiso 1 1 calc R U
C34 C 0.2424(5) 0.2592(5) 0.2725(5) 0.0237(13) Uani 1 1 d . .
H34A H 0.284456 0.223414 0.249654 0.028 Uiso 1 1 calc R U
H34B H 0.259433 0.264654 0.337356 0.028 Uiso 1 1 calc R U
C35 C 0.2786(6) 0.3562(5) 0.2619(5) 0.0269(14) Uani 1 1 d . .
H35A H 0.356405 0.380113 0.290045 0.032 Uiso 1 1 calc R U
H35B H 0.261266 0.350518 0.196979 0.032 Uiso 1 1 calc R U
C36 C 0.2299(5) 0.4266(5) 0.3028(4) 0.0200(12) Uani 1 1 d . .
C37 C 0.1102(6) 0.1134(4) 0.2357(5) 0.0242(13) Uani 1 1 d . .
H37A H 0.162278 0.088055 0.216488 0.029 Uiso 1 1 calc R U
H37B H 0.039083 0.075749 0.193722 0.029 Uiso 1 1 calc R U
C38 C 0.1187(6) 0.1043(5) 0.3309(5) 0.0267(14) Uani 1 1 d . .
H38A H 0.184953 0.148452 0.375005 0.032 Uiso 1 1 calc R U
H38B H 0.122830 0.043426 0.332223 0.032 Uiso 1 1 calc R U
C39 C 0.0234(5) 0.1198(4) 0.3598(5) 0.0231(13) Uani 1 1 d . .
C40 C 0.0376(6) 0.8608(5) 0.3283(5) 0.0317(15) Uani 1 1 d . .
H40 H 0.103730 0.851181 0.331266 0.038 Uiso 1 1 calc R U
C41 C 0.0047(8) 0.8455(7) 0.1671(6) 0.046(2) Uani 1 1 d . .
H41A H 0.074357 0.835924 0.181816 0.069 Uiso 1 1 calc R U
H41B H 0.007362 0.898005 0.144326 0.069 Uiso 1 1 calc R U
H41C H -0.047655 0.792251 0.120934 0.069 Uiso 1 1 calc R U
C42 C -0.1284(7) 0.8773(7) 0.2400(6) 0.050(2) Uani 1 1 d . .
H42A H -0.142509 0.880856 0.296560 0.075 Uiso 1 1 calc R U
H42B H -0.184095 0.827661 0.191796 0.075 Uiso 1 1 calc R U
H42C H -0.127185 0.933886 0.225108 0.075 Uiso 1 1 calc R U
C43 C 0.2651(7) 1.0830(6) 0.5536(7) 0.044(2) Uani 1 1 d . .
H43A H 0.271749 1.074172 0.493818 0.066 Uiso 1 1 calc R U
H43B H 0.317889 1.062623 0.591618 0.066 Uiso 1 1 calc R U
H43C H 0.276553 1.147021 0.580741 0.066 Uiso 1 1 calc R U
O3S O 0.1285(10) 0.9838(8) 0.0391(9) 0.135(4) Uani 1 1 d D .
H5S H 0.176743 0.980585 0.083813 0.203 Uiso 1 1 d R U
O1S O 0.4622(10) 1.1809(10) 0.9091(10) 0.148(5) Uani 1 1 d . .
O2S O 0.3493(9) 1.0773(8) 0.7816(7) 0.123(4) Uani 1 1 d . .
C3S C 0.4508(17) 1.2610(12) 0.8784(16) 0.152(8) Uani 1 1 d . .
H0AA H 0.379833 1.267764 0.871828 0.183 Uiso 1 1 calc R U
H0AB H 0.462929 1.256850 0.820304 0.183 Uiso 1 1 calc R U
C4S C 0.5381(17) 1.3401(13) 0.9550(12) 0.139(7) Uani 1 1 d . .
H4SA H 0.518525 1.348663 1.009324 0.208 Uiso 1 1 calc R U
H4SB H 0.545330 1.395267 0.936521 0.208 Uiso 1 1 calc R U
H4SC H 0.605374 1.326405 0.967636 0.208 Uiso 1 1 calc R U
C2S C 0.4064(12) 1.0953(12) 0.8573(11) 0.100(4) Uani 1 1 d . .
C1S C 0.431(2) 1.0292(18) 0.9100(19) 0.208(12) Uani 1 1 d . .
H1SA H 0.402319 1.036438 0.959318 0.312 Uiso 1 1 calc R U
H1SB H 0.507387 1.041101 0.934487 0.312 Uiso 1 1 calc R U
H1SC H 0.398097 0.967586 0.869898 0.312 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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 O3 89.21(19) . .
O1 NI1 N1 93.5(2) . .
O3 NI1 N1 176.2(2) . .
O1 NI1 O10 174.12(18) . .
O3 NI1 O10 87.91(19) . .
N1 NI1 O10 89.1(2) . .
O1 NI1 O13 84.79(18) . .
O3 NI1 O13 87.30(18) . .
N1 NI1 O13 90.3(2) . .
O10 NI1 O13 89.96(18) . .
O1 NI1 N2 92.3(2) . .
O3 NI1 N2 88.1(2) . .
N1 NI1 N2 94.4(2) . .
O10 NI1 N2 92.7(2) . .
O13 NI1 N2 174.6(2) . .
O7 NI2 O5 90.0(2) . .
O7 NI2 N3 171.2(2) . .
O5 NI2 N3 93.6(2) . .
O7 NI2 N4 94.3(2) . .
O5 NI2 N4 96.0(2) . .
N3 NI2 N4 93.3(2) . .
O7 NI2 O3 85.76(19) . .
O5 NI2 O3 94.64(18) . .
N3 NI2 O3 86.0(2) . .
N4 NI2 O3 169.33(19) . .
O7 NI2 O4 88.78(19) . .
O5 NI2 O4 156.12(19) . .
N3 NI2 O4 84.7(2) . .
N4 NI2 O4 107.84(19) . .
O3 NI2 O4 61.49(17) . .
O7 NI2 C13 87.9(2) . .
O5 NI2 C13 125.8(2) . .
N3 NI2 C13 83.5(2) . .
N4 NI2 C13 138.1(2) . .
O3 NI2 C13 31.20(18) . .
O4 NI2 C13 30.32(19) . .
O9 NI3 O8 90.48(18) . .
O9 NI3 N5 101.2(2) . .
O8 NI3 N5 167.3(2) . .
O9 NI3 O11 171.86(19) . .
O8 NI3 O11 81.60(18) . .
N5 NI3 O11 86.6(2) . .
O9 NI3 O6 90.12(19) . 2_566
O8 NI3 O6 84.93(18) . 2_566
N5 NI3 O6 90.1(2) . 2_566
O11 NI3 O6 87.36(19) . 2_566
O9 NI3 N6 91.9(2) . .
O8 NI3 N6 93.4(2) . .
N5 NI3 N6 91.1(2) . .
O11 NI3 N6 90.5(2) . .
O6 NI3 N6 177.4(2) 2_566 .
O2 NI4 O17 93.8(2) . .
O2 NI4 O14 93.52(19) . .
O17 NI4 O14 90.3(2) . .
O2 NI4 O12 173.4(2) . .
O17 NI4 O12 86.6(2) . .
O14 NI4 O12 93.11(19) . .
O2 NI4 O16 87.18(19) . .
O17 NI4 O16 88.3(2) . .
O14 NI4 O16 178.5(2) . .
O12 NI4 O16 86.20(19) . .
O2 NI4 O15 87.2(2) . .
O17 NI4 O15 178.8(2) . .
O14 NI4 O15 89.1(2) . .
O12 NI4 O15 92.46(19) . .
O16 NI4 O15 92.3(2) . .
O19 CL1 O20 108.5(7) . .
O19 CL1 O21 105.9(8) . .
O20 CL1 O21 112.0(7) . .
O19 CL1 O18 111.8(7) . .
O20 CL1 O18 110.9(5) . .
O21 CL1 O18 107.8(5) . .
O22 CL2 O23 114.1(6) . .
O22 CL2 O25 110.4(5) . .
O23 CL2 O25 110.4(5) . .
O22 CL2 O24 110.1(8) . .
O23 CL2 O24 105.5(5) . .
O25 CL2 O24 105.9(5) . .
C10 O1 NI1 131.4(4) . .
C10 O2 NI4 129.8(4) . .
C13 O3 NI1 125.6(4) . .
C13 O3 NI2 89.9(4) . .
NI1 O3 NI2 134.7(2) . .
C13 O4 NI2 89.4(4) . .
C26 O5 NI2 125.8(4) . .
C26 O6 NI3 139.9(4) . 2_566
C23 O7 NI2 131.3(4) . .
C23 O8 NI3 134.2(4) . .
C36 O9 NI3 126.5(4) . .
C36 O10 NI1 134.3(4) . .
C39 O11 NI3 114.7(4) . .
C39 O12 NI4 122.9(4) 2_566 .
C43 O16 NI4 121.7(4) . .
C40 O17 NI4 125.1(5) . .
C1 N1 C5 118.4(6) . .
C1 N1 NI1 118.7(5) . .
C5 N1 NI1 122.0(5) . .
C11 N2 C8 108.6(5) . .
C11 N2 C7 107.6(5) . .
C8 N2 C7 110.7(5) . .
C11 N2 NI1 109.0(4) . .
C8 N2 NI1 109.7(4) . .
C7 N2 NI1 111.1(4) . .
C14 N3 C18 119.2(6) . .
C14 N3 NI2 119.5(5) . .
C18 N3 NI2 118.6(5) . .
C21 N4 C24 110.2(5) . .
C21 N4 C20 107.4(5) . .
C24 N4 C20 109.0(5) . .
C21 N4 NI2 107.2(4) . .
C24 N4 NI2 110.2(4) . .
C20 N4 NI2 112.7(4) . .
C31 N5 C27 119.1(6) . .
C31 N5 NI3 122.2(5) . .
C27 N5 NI3 118.7(5) . .
C34 N6 C33 109.9(5) . .
C34 N6 C37 108.0(5) . .
C33 N6 C37 107.6(5) . .
C34 N6 NI3 106.5(4) . .
C33 N6 NI3 115.0(4) . .
C37 N6 NI3 109.7(4) . .
C40 N7 C42 121.6(7) . .
C40 N7 C41 121.4(7) . .
C42 N7 C41 116.9(7) . .
N1 C1 C2 123.1(7) . .
C3 C2 C1 117.4(8) . .
C2 C3 C4 120.5(8) . .
C5 C4 C3 119.1(7) . .
N1 C5 C4 121.3(7) . .
N1 C5 C6 116.7(6) . .
C4 C5 C6 122.0(7) . .
C7 C6 C5 111.9(6) . .
N2 C7 C6 114.6(6) . .
N2 C8 C9 116.2(6) . .
C10 C9 C8 115.0(6) . .
O1 C10 O2 124.7(6) . .
O1 C10 C9 119.8(6) . .
O2 C10 C9 115.5(6) . .
N2 C11 C12 117.5(6) . .
C13 C12 C11 118.2(6) . .
O4 C13 O3 119.1(6) . .
O4 C13 C12 120.1(6) . .
O3 C13 C12 120.2(6) . .
O4 C13 NI2 60.3(3) . .
O3 C13 NI2 58.9(3) . .
C12 C13 NI2 169.9(5) . .
N3 C14 C15 122.4(7) . .
C14 C15 C16 119.4(8) . .
C17 C16 C15 118.1(7) . .
C16 C17 C18 119.7(7) . .
N3 C18 C17 121.2(7) . .
N3 C18 C19 115.8(6) . .
C17 C18 C19 123.0(7) . .
C18 C19 C20 113.1(6) . .
N4 C20 C19 112.8(6) . .
N4 C21 C22 118.4(5) . .
C23 C22 C21 118.5(6) . .
O7 C23 O8 124.2(6) . .
O7 C23 C22 121.2(6) . .
O8 C23 C22 114.5(6) . .
N4 C24 C25 114.2(6) . .
C24 C25 C26 116.3(6) . .
O6 C26 O5 120.6(6) . .
O6 C26 C25 121.0(5) . .
O5 C26 C25 118.3(6) . .
N5 C27 C28 122.4(7) . .
C29 C28 C27 118.6(7) . .
C30 C29 C28 119.2(8) . .
C29 C30 C31 120.3(7) . .
N5 C31 C30 120.4(7) . .
N5 C31 C32 116.8(6) . .
C30 C31 C32 122.8(7) . .
C31 C32 C33 111.4(6) . .
N6 C33 C32 116.3(6) . .
N6 C34 C35 115.7(6) . .
C36 C35 C34 116.6(5) . .
O10 C36 O9 124.2(6) . .
O10 C36 C35 115.5(6) . .
O9 C36 C35 120.3(6) . .
N6 C37 C38 116.8(5) . .
C37 C38 C39 113.3(6) . .
O12 C39 O11 123.9(6) 2_566 .
O12 C39 C38 118.6(6) 2_566 .
O11 C39 C38 117.5(6) . .
O17 C40 N7 123.3(7) . .
C2S O1S C3S 122.7(17) . .
O1S C3S C4S 103(2) . .
O2S C2S O1S 123(2) . .
O2S C2S C1S 126.9(19) . .
O1S C2S C1S 109.9(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
NI1 O1 2.031(4) .
NI1 O3 2.049(5) .
NI1 N1 2.058(6) .
NI1 O10 2.067(5) .
NI1 O13 2.103(4) .
NI1 N2 2.117(5) .
NI2 O7 2.006(5) .
NI2 O5 2.014(5) .
NI2 N3 2.067(6) .
NI2 N4 2.067(5) .
NI2 O3 2.123(5) .
NI2 O4 2.154(4) .
NI2 C13 2.479(7) .
NI3 O9 2.053(5) .
NI3 O8 2.088(4) .
NI3 N5 2.092(5) .
NI3 O11 2.097(5) .
NI3 O6 2.100(4) 2_566
NI3 N6 2.126(5) .
NI4 O2 2.030(5) .
NI4 O17 2.036(5) .
NI4 O14 2.059(5) .
NI4 O12 2.079(5) .
NI4 O16 2.084(5) .
NI4 O15 2.087(5) .
CL1 O19 1.373(9) .
CL1 O20 1.383(8) .
CL1 O21 1.397(9) .
CL1 O18 1.418(7) .
CL2 O22 1.395(9) .
CL2 O23 1.417(7) .
CL2 O25 1.426(7) .
CL2 O24 1.446(9) .
O1 C10 1.247(8) .
O2 C10 1.259(8) .
O3 C13 1.284(7) .
O4 C13 1.252(8) .
O5 C26 1.269(7) .
O6 C26 1.251(7) .
O6 NI3 2.100(4) 2_566
O7 C23 1.246(8) .
O8 C23 1.253(7) .
O9 C36 1.264(8) .
O10 C36 1.241(8) .
O11 C39 1.271(8) .
O12 C39 1.254(8) 2_566
O16 C43 1.442(9) .
O17 C40 1.235(9) .
C5S O3S 1.480(14) .
N1 C1 1.338(9) .
N1 C5 1.356(9) .
N2 C11 1.477(8) .
N2 C8 1.485(9) .
N2 C7 1.486(9) .
N3 C14 1.328(9) .
N3 C18 1.340(9) .
N4 C21 1.489(9) .
N4 C24 1.501(8) .
N4 C20 1.500(9) .
N5 C31 1.342(9) .
N5 C27 1.350(9) .
N6 C34 1.466(8) .
N6 C33 1.480(8) .
N6 C37 1.500(8) .
N7 C40 1.304(10) .
N7 C42 1.441(10) .
N7 C41 1.468(10) .
C1 C2 1.403(11) .
C2 C3 1.361(12) .
C3 C4 1.387(12) .
C4 C5 1.382(10) .
C5 C6 1.524(10) .
C6 C7 1.522(11) .
C8 C9 1.531(9) .
C9 C10 1.526(9) .
C11 C12 1.530(10) .
C12 C13 1.509(9) .
C14 C15 1.374(11) .
C15 C16 1.382(12) .
C16 C17 1.380(11) .
C17 C18 1.386(10) .
C18 C19 1.518(10) .
C19 C20 1.522(10) .
C21 C22 1.525(10) .
C22 C23 1.522(9) .
C24 C25 1.514(9) .
C25 C26 1.530(9) .
C27 C28 1.381(10) .
C28 C29 1.378(11) .
C29 C30 1.367(12) .
C30 C31 1.396(10) .
C31 C32 1.490(10) .
C32 C33 1.543(10) .
C34 C35 1.543(9) .
C35 C36 1.527(9) .
C37 C38 1.519(9) .
C38 C39 1.534(9) .
C39 O12 1.254(8) 2_566
O1S C2S 1.332(19) .
O1S C3S 1.46(2) .
O2S C2S 1.168(17) .
C3S C4S 1.52(3) .
C2S C1S 1.49(3) .
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
O13 H13A O5 0.84 1.92 2.755(7) 172.7 .
O13 H13B O9 0.86 1.98 2.733(6) 146.8 .
O14 H14B O1 0.87 1.91 2.674(6) 145.8 .
O14 H14A O6 0.87 2.02 2.809(7) 150.7 .
O15 H15B O11_$1 0.85 1.92 2.629(7) 139.5 2_566
O15 H15A O2S 0.84 2.08 2.798(12) 143.0 .
O16 H16 O12_$2 0.85 2.01 2.863(7) 180.0 2_576
O3S H5S O20 0.84 1.96 2.779(17) 165.8 .
