#------------------------------------------------------------------------------
#$Date: 2016-08-07 10:22:46 +0200 (dom 07 de ago de 2016) $
#$Revision: 185227 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/51/7225191.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_7225191
loop_
_publ_author_name
'Beldon, Patrick J.'
'Henke, Sebastian'
'Monserrat, Bartomeu'
'Tominaka, Satoshi'
'Stock, Norbert'
'Cheetham, Anthony K.'
_publ_section_title
;
 Transition metal coordination complexes of chrysazin
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5121
_journal_paper_doi               10.1039/C5CE00792E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C76 H64 N4 Ni6 O28, 4(C3 H7 N O)'
_chemical_formula_sum            'C88 H92 N8 Ni6 O32'
_chemical_formula_weight         2125.95
_chemical_name_systematic
'tetra(acetato)-tetra(chrysazinato)-tetra(N,N-dimethylformamide)-hexa-nickel(II) bis(N,N-dimethylformamide) solvate'
_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   geom
_audit_creation_date             2015-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.504(3)
_cell_angle_beta                 97.873(4)
_cell_angle_gamma                95.172(4)
_cell_formula_units_Z            1
_cell_length_a                   9.7302(6)
_cell_length_b                   13.4388(5)
_cell_length_c                   17.0848(7)
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      70.9260
_cell_measurement_theta_min      4.6070
_cell_volume                     2190.67(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.8595
_diffrn_measured_fraction_theta_max 0.8311
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0645062000
_diffrn_orient_matrix_UB_12      0.0358257000
_diffrn_orient_matrix_UB_13      0.0866883000
_diffrn_orient_matrix_UB_21      0.0535171000
_diffrn_orient_matrix_UB_22      0.1016696000
_diffrn_orient_matrix_UB_23      -0.0253853000
_diffrn_orient_matrix_UB_31      -0.1371323000
_diffrn_orient_matrix_UB_32      0.0423122000
_diffrn_orient_matrix_UB_33      0.0151042000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12949
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.309
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.175
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.2686
_exptl_crystal_size_mid          0.1263
_exptl_crystal_size_min          0.0446
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1034P)²+3.2535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5763
_reflns_number_total             7058
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00792e2.cif
_cod_data_source_block           NiChrys-2
_cod_depositor_comments
'Adding full bibliography for 7225182--7225192.cif.'
_cod_original_cell_volume        2190.66(18)
_cod_database_code               7225191
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni6 C88 H92 O32 N8'
_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.
;
_reflns_odcompleteness_completeness 85.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-O16 = C42-O17
 1.25 with sigma of 0.01
3. Others
 Fixed Sof: O16(0.5) O17(0.5) H42A(0.5) H42(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C26(H26), C27(H27), C28(H28), C33(H33), C36(H36), C39(H39),
 C42(H42A), C42(H42)
4.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66510(7) -0.00616(4) 0.01944(4) 0.0285(2) Uani 1 1 d . . . . .
Ni2 Ni 0.54106(7) 0.13693(4) 0.12161(4) 0.0279(2) Uani 1 1 d . . . . .
Ni3 Ni 0.38721(7) 0.26560(5) 0.22572(4) 0.0319(2) Uani 1 1 d . . . . .
O1 O 0.7859(3) -0.1084(2) 0.04931(17) 0.0325(6) Uani 1 1 d . . . . .
O2 O 0.6339(3) 0.01324(18) 0.13521(15) 0.0288(6) Uani 1 1 d . . . . .
O3 O 0.5373(3) 0.1612(2) 0.23586(16) 0.0325(6) Uani 1 1 d . . . . .
O4 O 0.7285(6) -0.2037(3) 0.3791(3) 0.0904(17) Uani 1 1 d . . . . .
O5 O 0.5201(3) 0.10696(18) 0.00372(16) 0.0262(6) Uani 1 1 d . . . . .
O6 O 0.4450(3) 0.26047(19) 0.11238(16) 0.0300(6) Uani 1 1 d . . . . .
O7 O 0.2616(3) 0.3637(2) 0.18906(18) 0.0362(7) Uani 1 1 d . . . . .
O8 O 0.3695(4) 0.4889(2) -0.1272(2) 0.0542(9) Uani 1 1 d . . . . .
O9 O 0.8172(3) 0.1067(2) 0.03748(17) 0.0343(6) Uani 1 1 d . . . . .
O10 O 0.7340(3) 0.2133(2) 0.12536(18) 0.0349(6) Uani 1 1 d . . . . .
O11 O 0.3413(3) 0.05333(18) 0.09966(16) 0.0291(6) Uani 1 1 d . . . . .
O12 O 0.2415(3) 0.1468(2) 0.18699(18) 0.0361(7) Uani 1 1 d . . . . .
O13 O 0.5354(3) 0.3759(2) 0.27884(18) 0.0406(7) Uani 1 1 d . . . . .
O14 O 0.3011(3) 0.2714(2) 0.33059(18) 0.0408(7) Uani 1 1 d . . . . .
O15 O 0.9138(9) 0.4297(13) 0.5682(8) 0.290(9) Uani 1 1 d . . . . .
O16 O 0.8651(19) 0.2101(11) 0.5580(13) 0.194(8) Uani 0.5 1 d D . P A 1
O17 O 0.9796(15) 0.0728(13) 0.5314(10) 0.159(6) Uani 0.5 1 d D . P A 2
N1 N 0.7530(4) 0.4547(3) 0.2901(2) 0.0448(9) Uani 1 1 d . . . . .
N2 N 0.0950(5) 0.2697(3) 0.3803(2) 0.0520(10) Uani 1 1 d . . . . .
N3 N 0.6804(8) 0.4057(5) 0.5755(4) 0.098(2) Uani 1 1 d . . . . .
N4 N 0.8374(6) 0.0773(4) 0.6238(3) 0.0734(14) Uani 1 1 d . . . . .
C1 C 0.8114(4) -0.1435(3) 0.1169(3) 0.0335(9) Uani 1 1 d . . . . .
C2 C 0.9020(5) -0.2210(3) 0.1201(3) 0.0400(10) Uani 1 1 d . . . . .
H2 H 0.9401 -0.2408 0.0747 0.048 Uiso 1 1 calc R U . . .
C3 C 0.9357(5) -0.2678(3) 0.1868(3) 0.0451(11) Uani 1 1 d . . . . .
H3 H 0.9968 -0.3172 0.1864 0.054 Uiso 1 1 calc R U . . .
C4 C 0.8786(6) -0.2417(4) 0.2552(3) 0.0481(12) Uani 1 1 d . . . . .
H4 H 0.8990 -0.2749 0.3000 0.058 Uiso 1 1 calc R U . . .
C5 C 0.7919(5) -0.1667(3) 0.2563(3) 0.0418(10) Uani 1 1 d . . . . .
C6 C 0.7571(4) -0.1125(3) 0.1893(3) 0.0341(9) Uani 1 1 d . . . . .
C7 C 0.6740(4) -0.0295(3) 0.1969(3) 0.0318(9) Uani 1 1 d . . . . .
C8 C 0.6370(4) 0.0087(3) 0.2741(3) 0.0347(9) Uani 1 1 d . . . . .
C9 C 0.6669(6) -0.0485(4) 0.3399(3) 0.0472(12) Uani 1 1 d . . . . .
C10 C 0.7286(6) -0.1448(4) 0.3285(3) 0.0548(13) Uani 1 1 d . . . . .
C11 C 0.5736(4) 0.0998(3) 0.2892(3) 0.0338(9) Uani 1 1 d . . . . .
C12 C 0.5500(5) 0.1283(4) 0.3672(3) 0.0473(12) Uani 1 1 d . . . . .
H12 H 0.5095 0.1874 0.3773 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5839(7) 0.0730(4) 0.4286(3) 0.0605(15) Uani 1 1 d . . . . .
H13 H 0.5694 0.0958 0.4797 0.073 Uiso 1 1 calc R U . . .
C14 C 0.6400(7) -0.0176(4) 0.4148(3) 0.0626(16) Uani 1 1 d . . . . .
H14 H 0.6592 -0.0571 0.4560 0.075 Uiso 1 1 calc R U . . .
C15 C 0.5269(4) 0.1867(3) -0.0402(2) 0.0288(8) Uani 1 1 d . . . . .
C16 C 0.5938(4) 0.1760(3) -0.1075(2) 0.0345(9) Uani 1 1 d . . . . .
H16 H 0.6409 0.1197 -0.1163 0.041 Uiso 1 1 calc R U . . .
C17 C 0.5922(5) 0.2458(3) -0.1607(3) 0.0405(10) Uani 1 1 d . . . . .
H17 H 0.6393 0.2372 -0.2043 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5199(5) 0.3295(3) -0.1496(3) 0.0401(10) Uani 1 1 d . . . . .
H18 H 0.5139 0.3753 -0.1872 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4574(4) 0.3440(3) -0.0823(3) 0.0339(9) Uani 1 1 d . . . . .
C20 C 0.4644(4) 0.2766(3) -0.0230(2) 0.0311(9) Uani 1 1 d . . . . .
C21 C 0.4094(4) 0.3058(3) 0.0519(2) 0.0288(8) Uani 1 1 d . . . . .
C22 C 0.3232(4) 0.3865(3) 0.0579(3) 0.0318(9) Uani 1 1 d . . . . .
C23 C 0.3033(5) 0.4478(3) -0.0060(3) 0.0362(9) Uani 1 1 d . . . . .
C24 C 0.3773(5) 0.4325(3) -0.0752(3) 0.0385(10) Uani 1 1 d . . . . .
C25 C 0.2558(4) 0.4090(3) 0.1270(3) 0.0327(9) Uani 1 1 d . . . . .
C26 C 0.1696(5) 0.4907(3) 0.1241(3) 0.0405(10) Uani 1 1 d . . . . .
H26 H 0.1229 0.5059 0.1670 0.049 Uiso 1 1 calc R U . . .
C27 C 0.1530(5) 0.5465(3) 0.0619(3) 0.0453(11) Uani 1 1 d . . . . .
H27 H 0.0955 0.5982 0.0630 0.054 Uiso 1 1 calc R U . . .
C28 C 0.2220(5) 0.5265(3) -0.0036(3) 0.0438(11) Uani 1 1 d . . . . .
H28 H 0.2130 0.5662 -0.0453 0.053 Uiso 1 1 calc R U . . .
C29 C 0.8257(4) 0.1862(3) 0.0842(3) 0.0323(9) Uani 1 1 d . . . . .
C30 C 0.9594(4) 0.2551(3) 0.0911(3) 0.0403(10) Uani 1 1 d . . . . .
H30A H 0.9938 0.2758 0.1462 0.060 Uiso 1 1 calc R U . . .
H30B H 0.9417 0.3132 0.0642 0.060 Uiso 1 1 calc R U . . .
H30C H 1.0277 0.2201 0.0674 0.060 Uiso 1 1 calc R U . . .
C31 C 0.2370(4) 0.0736(3) 0.1355(2) 0.0316(9) Uani 1 1 d . . . . .
C32 C 0.1046(5) 0.0057(3) 0.1147(3) 0.0442(11) Uani 1 1 d . . . . .
H32A H 0.0499 0.0127 0.1572 0.066 Uiso 1 1 calc R U . . .
H32B H 0.1256 -0.0627 0.1066 0.066 Uiso 1 1 calc R U . . .
H32C H 0.0530 0.0232 0.0669 0.066 Uiso 1 1 calc R U . . .
C33 C 0.6515(5) 0.3863(3) 0.2572(3) 0.0382(10) Uani 1 1 d . . . . .
H33 H 0.6681 0.3425 0.2148 0.046 Uiso 1 1 calc R U . . .
C34 C 0.8808(6) 0.4678(4) 0.2555(4) 0.0612(15) Uani 1 1 d . . . . .
H34A H 0.8816 0.5274 0.2286 0.092 Uiso 1 1 calc R U . . .
H34B H 0.8857 0.4105 0.2182 0.092 Uiso 1 1 calc R U . . .
H34C H 0.9596 0.4743 0.2968 0.092 Uiso 1 1 calc R U . . .
C35 C 0.7305(7) 0.5310(5) 0.3515(4) 0.091(2) Uani 1 1 d . . . . .
H35A H 0.8166 0.5517 0.3862 0.136 Uiso 1 1 calc R U . . .
H35B H 0.6622 0.5040 0.3815 0.136 Uiso 1 1 calc R U . . .
H35C H 0.6978 0.5878 0.3274 0.136 Uiso 1 1 calc R U . . .
C36 C 0.1714(5) 0.2619(3) 0.3222(3) 0.0416(11) Uani 1 1 d . . . . .
H36 H 0.1242 0.2481 0.2706 0.050 Uiso 1 1 calc R U . . .
C37 C -0.0558(6) 0.2521(6) 0.3652(4) 0.0740(18) Uani 1 1 d . . . . .
H37A H -0.0864 0.1969 0.3924 0.111 Uiso 1 1 calc R U . . .
H37B H -0.0859 0.2364 0.3091 0.111 Uiso 1 1 calc R U . . .
H37C H -0.0950 0.3113 0.3839 0.111 Uiso 1 1 calc R U . . .
C38 C 0.1611(8) 0.2947(8) 0.4616(4) 0.111(3) Uani 1 1 d . . . . .
H38A H 0.1612 0.2349 0.4882 0.166 Uiso 1 1 calc R U . . .
H38B H 0.1107 0.3424 0.4882 0.166 Uiso 1 1 calc R U . . .
H38C H 0.2554 0.3232 0.4624 0.166 Uiso 1 1 calc R U . . .
C39 C 0.7967(16) 0.3985(13) 0.5394(8) 0.185(7) Uani 1 1 d . . . . .
H39 H 0.7838 0.3665 0.4878 0.222 Uiso 1 1 calc R U . . .
C40 C 0.5489(12) 0.3612(11) 0.5311(7) 0.195(7) Uani 1 1 d . . . . .
H40A H 0.5048 0.3149 0.5618 0.293 Uiso 1 1 calc R U . . .
H40B H 0.5647 0.3261 0.4820 0.293 Uiso 1 1 calc R U . . .
H40C H 0.4897 0.4131 0.5200 0.293 Uiso 1 1 calc R U . . .
C41 C 0.6883(12) 0.4517(8) 0.6547(5) 0.136(4) Uani 1 1 d . . . . .
H41A H 0.7481 0.4172 0.6899 0.203 Uiso 1 1 calc R U . . .
H41B H 0.5967 0.4480 0.6698 0.203 Uiso 1 1 calc R U . . .
H41C H 0.7254 0.5208 0.6577 0.203 Uiso 1 1 calc R U . . .
C42 C 0.8983(10) 0.1219(7) 0.5687(5) 0.099(3) Uani 1 1 d D . . . .
H42A H 0.8817 0.1867 0.5581 0.119 Uiso 0.5 1 calc R U P A 2
H42 H 0.9604 0.0909 0.5402 0.119 Uiso 0.5 1 calc R U P A 1
C43 C 0.7517(10) 0.1283(8) 0.6718(6) 0.131(4) Uani 1 1 d . . . . .
H43A H 0.7464 0.1954 0.6575 0.197 Uiso 1 1 calc R U . . .
H43B H 0.7910 0.1311 0.7267 0.197 Uiso 1 1 calc R U . . .
H43C H 0.6598 0.0929 0.6635 0.197 Uiso 1 1 calc R U . . .
C44 C 0.8708(12) -0.0222(6) 0.6371(6) 0.132(4) Uani 1 1 d . . . . .
H44A H 0.9192 -0.0483 0.5956 0.197 Uiso 1 1 calc R U . . .
H44B H 0.7863 -0.0651 0.6372 0.197 Uiso 1 1 calc R U . . .
H44C H 0.9291 -0.0199 0.6875 0.197 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 9 -3 0.0498 -0.0053 8.9967 -2.9690 0.0646 0.9898 0.3365
0 0 11 0.0445 -0.0009 0.0054 10.9964 0.9534 -0.2786 0.1664
0 -9 3 0.0766 0.0053 -8.9967 2.9690 -0.0646 -0.9898 -0.3365
6 0 -4 0.1114 5.9931 -0.0152 -4.0050 0.0389 0.4209 -0.8830
0 -1 -11 0.0068 0.0015 -1.0052 -10.9998 -0.9895 0.1771 -0.2089
1 4 8 0.0232 0.9957 4.0009 8.0097 0.9019 0.2567 0.1537
3 -7 4 0.1276 3.0003 -7.0032 3.9722 0.2870 -0.6523 -0.6478
-6 -1 -3 0.1090 -5.9919 -0.9881 -2.9960 -0.6816 -0.3451 0.7346
-1 -2 11 0.0434 -0.9985 -1.9920 10.9908 0.8170 -0.5350 0.2186
-1 1 11 0.0405 -1.0003 1.0074 11.0008 0.9252 -0.2304 0.3460
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 Ni2 129.01(9) . .
O1 Ni1 O2 87.40(11) . .
O1 Ni1 O5 94.64(11) . 2_655
O1 Ni1 O5 171.28(11) . .
O1 Ni1 O9 95.21(12) . .
O1 Ni1 O11 91.22(11) . 2_655
O2 Ni1 Ni2 42.52(7) . .
O2 Ni1 O5 84.08(10) . .
O2 Ni1 O5 87.94(11) . 2_655
O2 Ni1 O11 166.25(11) . 2_655
O5 Ni1 Ni2 92.68(7) 2_655 .
O5 Ni1 Ni2 42.99(7) . .
O5 Ni1 O5 83.23(10) 2_655 .
O9 Ni1 Ni2 80.47(8) . .
O9 Ni1 O2 91.71(11) . .
O9 Ni1 O5 170.12(11) . 2_655
O9 Ni1 O5 86.91(10) . .
O9 Ni1 O11 102.05(11) . 2_655
O11 Ni1 Ni2 139.59(8) 2_655 .
O11 Ni1 O5 96.61(10) 2_655 .
O11 Ni1 O5 78.52(10) 2_655 2_655
O2 Ni2 Ni1 44.07(8) . .
O2 Ni2 O5 90.54(11) . .
O2 Ni2 O6 177.56(11) . .
O2 Ni2 O10 88.28(11) . .
O2 Ni2 O11 91.39(11) . .
O3 Ni2 Ni1 134.94(8) . .
O3 Ni2 O2 91.32(11) . .
O3 Ni2 O5 173.03(11) . .
O3 Ni2 O6 86.41(11) . .
O3 Ni2 O10 95.11(12) . .
O3 Ni2 O11 93.23(11) . .
O5 Ni2 Ni1 48.07(7) . .
O5 Ni2 O10 91.66(11) . .
O5 Ni2 O11 80.01(10) . .
O6 Ni2 Ni1 138.29(8) . .
O6 Ni2 O5 91.61(11) . .
O6 Ni2 O10 92.82(11) . .
O6 Ni2 O11 87.84(11) . .
O10 Ni2 Ni1 80.24(8) . .
O10 Ni2 O11 171.66(11) . .
O11 Ni2 Ni1 93.75(7) . .
O6 Ni3 O3 79.85(11) . .
O7 Ni3 O3 165.30(12) . .
O7 Ni3 O6 85.46(11) . .
O7 Ni3 O12 93.00(12) . .
O7 Ni3 O13 91.93(13) . .
O7 Ni3 O14 88.32(12) . .
O12 Ni3 O3 87.47(11) . .
O12 Ni3 O6 89.46(11) . .
O12 Ni3 O14 85.68(12) . .
O13 Ni3 O3 89.32(12) . .
O13 Ni3 O6 97.08(12) . .
O13 Ni3 O12 172.10(13) . .
O13 Ni3 O14 88.30(13) . .
O14 Ni3 O3 106.36(12) . .
O14 Ni3 O6 171.90(12) . .
C1 O1 Ni1 129.0(3) . .
Ni2 O2 Ni1 93.41(11) . .
C7 O2 Ni1 134.0(2) . .
C7 O2 Ni2 132.0(2) . .
Ni2 O3 Ni3 94.88(12) . .
C11 O3 Ni2 126.1(2) . .
C11 O3 Ni3 133.6(3) . .
Ni1 O5 Ni1 96.77(10) 2_655 .
Ni2 O5 Ni1 101.37(11) . 2_655
Ni2 O5 Ni1 88.95(10) . .
C15 O5 Ni1 128.7(2) . .
C15 O5 Ni1 117.3(2) . 2_655
C15 O5 Ni2 117.6(2) . .
Ni2 O6 Ni3 94.89(11) . .
C21 O6 Ni2 130.3(2) . .
C21 O6 Ni3 133.4(2) . .
C25 O7 Ni3 129.8(3) . .
C29 O9 Ni1 127.4(3) . .
C29 O10 Ni2 124.8(3) . .
Ni1 O11 Ni2 99.08(11) 2_655 .
C31 O11 Ni1 126.9(3) . 2_655
C31 O11 Ni2 124.9(2) . .
C31 O12 Ni3 132.4(3) . .
C33 O13 Ni3 121.4(3) . .
C36 O14 Ni3 115.4(3) . .
C33 N1 C34 120.5(4) . .
C33 N1 C35 120.7(4) . .
C35 N1 C34 117.7(4) . .
C36 N2 C37 121.7(5) . .
C36 N2 C38 120.2(5) . .
C38 N2 C37 118.1(5) . .
C39 N3 C40 117.4(10) . .
C39 N3 C41 121.7(10) . .
C41 N3 C40 120.8(9) . .
C42 N4 C43 121.9(8) . .
C42 N4 C44 117.3(7) . .
C43 N4 C44 120.6(7) . .
O1 C1 C2 116.1(4) . .
O1 C1 C6 126.8(4) . .
C2 C1 C6 117.1(4) . .
C3 C2 C1 123.0(4) . .
C2 C3 C4 120.1(4) . .
C5 C4 C3 119.7(4) . .
C4 C5 C6 122.7(4) . .
C4 C5 C10 117.8(4) . .
C6 C5 C10 119.4(4) . .
C5 C6 C1 117.3(4) . .
C5 C6 C7 119.5(4) . .
C7 C6 C1 123.2(4) . .
O2 C7 C6 119.1(4) . .
O2 C7 C8 119.2(4) . .
C6 C7 C8 121.6(4) . .
C9 C8 C7 118.0(4) . .
C9 C8 C11 116.9(4) . .
C11 C8 C7 125.1(4) . .
C8 C9 C10 120.1(4) . .
C14 C9 C8 122.3(4) . .
C14 C9 C10 117.6(4) . .
O4 C10 C5 121.2(4) . .
O4 C10 C9 120.4(5) . .
C5 C10 C9 118.4(4) . .
O3 C11 C8 125.4(4) . .
O3 C11 C12 116.4(4) . .
C12 C11 C8 118.2(4) . .
C13 C12 C11 122.9(4) . .
C12 C13 C14 119.9(5) . .
C9 C14 C13 119.6(5) . .
O5 C15 C16 117.2(3) . .
O5 C15 C20 123.6(3) . .
C16 C15 C20 119.1(4) . .
C17 C16 C15 122.1(4) . .
C16 C17 C18 119.9(4) . .
C19 C18 C17 119.4(4) . .
C18 C19 C20 122.4(4) . .
C18 C19 C24 116.9(4) . .
C20 C19 C24 120.7(4) . .
C15 C20 C21 125.3(4) . .
C19 C20 C15 116.6(4) . .
C19 C20 C21 118.1(3) . .
O6 C21 C20 118.7(3) . .
O6 C21 C22 120.1(4) . .
C22 C21 C20 121.2(4) . .
C21 C22 C25 122.2(4) . .
C23 C22 C21 119.4(4) . .
C23 C22 C25 118.4(4) . .
C22 C23 C24 120.5(4) . .
C28 C23 C22 122.0(4) . .
C28 C23 C24 117.3(4) . .
O8 C24 C19 120.2(4) . .
O8 C24 C23 121.2(4) . .
C23 C24 C19 118.5(4) . .
O7 C25 C22 127.4(4) . .
O7 C25 C26 116.4(4) . .
C26 C25 C22 116.2(4) . .
C27 C26 C25 123.4(4) . .
C26 C27 C28 120.2(4) . .
C23 C28 C27 119.7(4) . .
O9 C29 O10 126.5(4) . .
O9 C29 C30 115.9(4) . .
O10 C29 C30 117.5(4) . .
O11 C31 C32 118.2(3) . .
O12 C31 O11 123.4(4) . .
O12 C31 C32 118.3(4) . .
O13 C33 N1 124.5(4) . .
O14 C36 N2 125.6(5) . .
O15 C39 N3 126.0(14) . .
O16 C42 N4 115.5(12) . .
O17 C42 N4 117.9(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 Ni2 2.9245(9) .
Ni1 O1 1.947(3) .
Ni1 O2 2.038(3) .
Ni1 O5 2.122(2) 2_655
Ni1 O5 2.176(3) .
Ni1 O9 1.991(3) .
Ni1 O11 2.063(3) 2_655
Ni2 O2 1.980(3) .
Ni2 O3 1.954(3) .
Ni2 O5 1.994(3) .
Ni2 O6 1.986(3) .
Ni2 O10 2.047(3) .
Ni2 O11 2.123(3) .
Ni3 O3 2.117(3) .
Ni3 O6 2.086(3) .
Ni3 O7 1.965(3) .
Ni3 O12 2.032(3) .
Ni3 O13 2.025(3) .
Ni3 O14 2.077(3) .
O1 C1 1.291(5) .
O2 C7 1.279(5) .
O3 C11 1.320(5) .
O4 C10 1.226(6) .
O5 Ni1 2.122(2) 2_655
O5 C15 1.368(4) .
O6 C21 1.272(5) .
O7 C25 1.270(5) .
O8 C24 1.222(5) .
O9 C29 1.260(5) .
O10 C29 1.267(5) .
O11 Ni1 2.063(3) 2_655
O11 C31 1.291(5) .
O12 C31 1.249(5) .
O13 C33 1.236(5) .
O14 C36 1.244(6) .
O15 C39 1.198(16) .
O16 C42 1.280(9) .
O17 C42 1.272(9) .
N1 C33 1.312(6) .
N1 C34 1.452(6) .
N1 C35 1.447(7) .
N2 C36 1.321(6) .
N2 C37 1.448(7) .
N2 C38 1.443(8) .
N3 C39 1.366(13) .
N3 C40 1.441(11) .
N3 C41 1.422(10) .
N4 C42 1.338(9) .
N4 C43 1.421(9) .
N4 C44 1.437(9) .
C1 C2 1.425(6) .
C1 C6 1.450(6) .
C2 C3 1.369(7) .
C3 C4 1.390(7) .
C4 C5 1.372(6) .
C5 C6 1.431(6) .
C5 C10 1.470(7) .
C6 C7 1.442(5) .
C7 C8 1.472(6) .
C8 C9 1.435(6) .
C8 C11 1.437(6) .
C9 C10 1.483(6) .
C9 C14 1.373(7) .
C11 C12 1.405(6) .
C12 C13 1.365(7) .
C13 C14 1.392(7) .
C15 C16 1.400(5) .
C15 C20 1.424(5) .
C16 C17 1.366(6) .
C17 C18 1.391(6) .
C18 C19 1.378(6) .
C19 C20 1.422(6) .
C19 C24 1.483(5) .
C20 C21 1.487(5) .
C21 C22 1.434(5) .
C22 C23 1.432(6) .
C22 C25 1.447(6) .
C23 C24 1.473(6) .
C23 C28 1.378(6) .
C25 C26 1.440(6) .
C26 C27 1.358(7) .
C27 C28 1.399(7) .
C29 C30 1.512(5) .
C31 C32 1.489(6) .
