#------------------------------------------------------------------------------
#$Date: 2024-12-06 21:08:46 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296601 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717425.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_7717425
loop_
_publ_author_name
'Li, Yue'
'Xu, Mingming'
'Liu, Hongyan'
'Wang, Xiaokang'
'Wang, Yutong'
'Sun, Meng'
'Fan, Weidong'
'Sun, Daofeng'
_publ_section_title
;
 Two amino-functionalized metal-organic frameworks with different
 topologies for C₂H₂/C₂H₄
 separation.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18094
_journal_page_last               18098
_journal_paper_doi               10.1039/d4dt02592j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H33 N4 Ni3 O13'
_chemical_formula_sum            'C38 H33 N4 Ni3 O13'
_chemical_formula_weight         929.81
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-08-12 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   23.5121(12)
_cell_length_b                   23.5121(12)
_cell_length_c                   38.3738(12)
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      57.1980
_cell_measurement_theta_min      4.4790
_cell_volume                     18371.7(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  -6.00   1.00   35.00    --    0.00 130.00 -85.00   55
  2  ω    -24.00  33.00   1.00   35.00    --    0.00 -80.00 145.00   57
  3  ω    -15.00  75.00   1.00   35.00    --   53.63 -57.00-150.00   90
  4  ω     32.00 102.00   1.00   35.00    --   53.63-140.00  28.00   70
  5  ω     26.00 109.00   1.00   35.00    --   53.63-125.00-180.00   83
  6  ω    111.00 176.00   1.00   40.00    --  107.26 111.00 120.00   65
  7  ω     85.00 159.00   1.00   40.00    --  107.26  63.00-120.00   74
  8  ω    100.00 177.00   1.00   40.00    --  107.26  80.00 -90.00   77
  9  ω    121.00 162.00   1.00   40.00    --  107.26 111.00-120.00   41
 10  ω     52.00  87.00   1.00   40.00    --  107.26 -50.00 150.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155281000
_diffrn_orient_matrix_UB_12      0.0402973000
_diffrn_orient_matrix_UB_13      0.0260628000
_diffrn_orient_matrix_UB_21      0.0567202000
_diffrn_orient_matrix_UB_22      0.0639845000
_diffrn_orient_matrix_UB_23      -0.0151350000
_diffrn_orient_matrix_UB_31      -0.0475773000
_diffrn_orient_matrix_UB_32      0.0029064000
_diffrn_orient_matrix_UB_33      -0.0265497000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            15185
_diffrn_reflns_point_group_measured_fraction_full 0.611
_diffrn_reflns_point_group_measured_fraction_max 0.594
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.616
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.756
_exptl_crystal_description       block
_exptl_crystal_F_000             4293
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0970P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.217
_reflns_Friedel_fraction_full    0.225
_reflns_Friedel_fraction_max     0.212
_reflns_number_gt                5493
_reflns_number_total             9324
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02592j2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7717425--7717426.cif.'
_cod_original_cell_volume        18371.7(19)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7717425
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Ni'
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(5)
 0.48(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 O1(H1), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C31(H31),
  C33(H33), C34(H34), C36(H36), C37(H37)
5.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N10(H10A,H10B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.468
_oxdiff_exptl_absorpt_empirical_full_min 0.682
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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 0.65779(7) 0.91530(7) 0.43507(3) 0.0727(4) Uani 1 1 d . . . . .
Ni2 Ni 0.65315(8) 0.85220(8) 0.36447(3) 0.0791(5) Uani 1 1 d . . . . .
Ni3 Ni 0.78396(8) 1.00843(9) 0.39737(4) 0.0913(6) Uani 1 1 d . . . . .
O1 O 0.7175(3) 0.9103(3) 0.40097(14) 0.0841(17) Uani 1 1 d . . . . .
H1 H 0.741814 0.893225 0.402686 0.126 Uiso 1 1 d R U . . .
O2 O 0.6119(3) 0.8226(3) 0.44917(15) 0.105(3) Uani 1 1 d . . . . .
O3 O 0.6222(3) 0.7774(3) 0.39829(16) 0.0829(19) Uani 1 1 d . . . . .
O4 O 0.7144(3) 0.8234(4) 0.34465(18) 0.105(2) Uani 1 1 d . . . . .
H4A H 0.723093 0.793084 0.352807 0.158 Uiso 1 1 d R U . . .
H4B H 0.738753 0.838094 0.325506 0.158 Uiso 1 1 d R U . . .
O5 O 0.8628(4) 0.9970(5) 0.38086(19) 0.145(3) Uani 1 1 d . . . . .
H5A H 0.890187 0.992824 0.393498 0.218 Uiso 1 1 d R U . . .
H5B H 0.874287 0.995234 0.360088 0.218 Uiso 1 1 d R U . . .
O6 O 0.8421(3) 1.1071(3) 0.39508(16) 0.104(2) Uani 1 1 d . . . . .
H6A H 0.858312 1.134453 0.411725 0.155 Uiso 1 1 d R U . . .
H6B H 0.855982 1.130494 0.376765 0.155 Uiso 1 1 d R U . . .
O7 O 0.7044(3) 1.0104(3) 0.41829(14) 0.0818(19) Uani 1 1 d . . . . .
H7A H 0.713769 1.038811 0.434229 0.123 Uiso 1 1 d R U . . .
H7B H 0.682659 1.018711 0.403469 0.123 Uiso 1 1 d R U . . .
O8 O 0.5482(3) 0.9433(3) 0.14004(13) 0.0780(18) Uani 1 1 d . . . . .
O9 O 0.5350(3) 0.8514(3) 0.11455(15) 0.0831(19) Uani 1 1 d . . . . .
O10 O 0.3758(4) 0.3910(3) 0.37587(16) 0.091(2) Uani 1 1 d . . . . .
O11 O 0.2949(3) 0.4047(3) 0.39047(15) 0.0759(17) Uani 1 1 d . . . . .
O12 O 0.3506(4) 0.2540(3) 0.66157(13) 0.084(2) Uani 1 1 d . . . . .
O13 O 0.4256(3) 0.3537(3) 0.68114(18) 0.099(2) Uani 1 1 d . . . . .
N1 N 0.4901(6) 0.5217(6) 0.5299(3) 0.166(5) Uani 1 1 d . . . . .
H1A H 0.496421 0.506126 0.548821 0.199 Uiso 1 1 calc R U . . .
H1B H 0.518544 0.560591 0.523097 0.199 Uiso 1 1 calc R U . . .
N5 N 0.5759(4) 0.7920(4) 0.33091(17) 0.071(2) Uani 1 1 d . . . . .
N10 N 0.4235(4) 0.6608(4) 0.26442(17) 0.087(3) Uani 1 1 d . . . . .
H10A H 0.400545 0.619873 0.269840 0.104 Uiso 1 1 calc R U . . .
H10B H 0.415684 0.674786 0.245329 0.104 Uiso 1 1 calc R U . . .
N14 N 0.3334(4) 0.4055(4) 0.46883(18) 0.075(2) Uani 1 1 d . . . . .
C1 C 0.5572(5) 0.7030(5) 0.4427(2) 0.091(3) Uani 1 1 d . . . . .
C2 C 0.5453(5) 0.6479(5) 0.4208(2) 0.094(3) Uani 1 1 d . . . . .
H2 H 0.563810 0.654181 0.398769 0.113 Uiso 1 1 calc R U . . .
C3 C 0.5070(5) 0.5882(5) 0.4335(3) 0.098(3) Uani 1 1 d . . . . .
H3 H 0.502665 0.553057 0.420228 0.117 Uiso 1 1 calc R U . . .
C4 C 0.4717(8) 0.5729(7) 0.4659(4) 0.139(4) Uani 1 1 d . U . . .
C5 C 0.4901(7) 0.6299(6) 0.4866(3) 0.126(4) Uani 1 1 d . . . . .
H5 H 0.475952 0.622632 0.509666 0.151 Uiso 1 1 calc R U . . .
C6 C 0.5282(6) 0.6972(6) 0.4757(3) 0.118(4) Uani 1 1 d . . . . .
H6 H 0.533104 0.732678 0.488841 0.142 Uiso 1 1 calc R U . . .
C7 C 0.6040(5) 0.7732(5) 0.4282(2) 0.085(3) Uani 1 1 d . . . . .
C8 C 0.3771(6) 0.4697(5) 0.4611(2) 0.083(3) Uani 1 1 d . . . . .
H8 H 0.367855 0.487465 0.441667 0.099 Uiso 1 1 calc R U . . .
C9 C 0.4286(6) 0.5070(6) 0.4778(3) 0.095(3) Uani 1 1 d . . . . .
C10 C 0.4357(6) 0.4850(6) 0.5107(3) 0.096(3) Uani 1 1 d . . . . .
C11 C 0.3941(5) 0.4268(5) 0.5218(2) 0.081(3) Uani 1 1 d . . . . .
C12 C 0.3449(5) 0.3877(5) 0.5000(2) 0.084(3) Uani 1 1 d . . . . .
H12 H 0.316605 0.344852 0.507183 0.101 Uiso 1 1 calc R U . . .
C13 C 0.3926(6) 0.3978(5) 0.5581(3) 0.095(3) Uani 1 1 d . . . . .
C14 C 0.3778(6) 0.3324(6) 0.5615(3) 0.121(4) Uani 1 1 d . . . . .
H14 H 0.368494 0.306773 0.541573 0.145 Uiso 1 1 calc R U . . .
C15 C 0.3764(6) 0.3049(6) 0.5932(2) 0.102(3) Uani 1 1 d . . . . .
H15 H 0.366673 0.261379 0.594344 0.123 Uiso 1 1 calc R U . . .
C16 C 0.3892(5) 0.3406(5) 0.6233(2) 0.091(3) Uani 1 1 d . . . . .
C17 C 0.4173(6) 0.4082(6) 0.6165(4) 0.123(4) Uani 1 1 d . U . . .
H17 H 0.439522 0.437801 0.634388 0.148 Uiso 1 1 calc R U . . .
C18 C 0.4133(7) 0.4321(6) 0.5851(3) 0.126(5) Uani 1 1 d . . . . .
H18 H 0.426584 0.476460 0.583521 0.151 Uiso 1 1 calc R U . . .
C19 C 0.3901(4) 0.3129(6) 0.6594(2) 0.079(3) Uani 1 1 d . . . . .
C20 C 0.3488(5) 0.4204(4) 0.3751(2) 0.067(2) Uani 1 1 d . . . . .
C21 C 0.3835(5) 0.4868(5) 0.3581(2) 0.072(2) Uani 1 1 d . . . . .
C22 C 0.3540(5) 0.5309(4) 0.3648(2) 0.079(3) Uani 1 1 d . . . . .
H22 H 0.315872 0.517556 0.377617 0.095 Uiso 1 1 calc R U . . .
C23 C 0.3920(6) 0.5964(5) 0.3489(2) 0.094(3) Uani 1 1 d . . . . .
H23 H 0.379693 0.627620 0.353290 0.113 Uiso 1 1 calc R U . . .
C24 C 0.4436(5) 0.6121(4) 0.3284(2) 0.072(3) Uani 1 1 d . . . . .
C25 C 0.4632(6) 0.5669(6) 0.3221(3) 0.110(4) Uani 1 1 d . . . . .
H25 H 0.499822 0.578729 0.308230 0.132 Uiso 1 1 calc R U . . .
C26 C 0.4291(5) 0.5032(6) 0.3362(3) 0.092(3) Uani 1 1 d . . . . .
H26 H 0.440486 0.472350 0.329086 0.110 Uiso 1 1 calc R U . . .
C27 C 0.5370(5) 0.7305(6) 0.3377(2) 0.098(3) Uani 1 1 d . . . . .
H27 H 0.543510 0.715984 0.359059 0.118 Uiso 1 1 calc R U . . .
C28 C 0.4850(5) 0.6816(5) 0.3165(2) 0.075(3) Uani 1 1 d . . . . .
C29 C 0.4714(5) 0.7026(5) 0.2857(2) 0.079(3) Uani 1 1 d . . . . .
C30 C 0.5207(5) 0.7702(4) 0.2758(2) 0.070(2) Uani 1 1 d . . . . .
C31 C 0.5706(4) 0.8138(4) 0.3008(2) 0.075(3) Uani 1 1 d . . . . .
H31 H 0.598770 0.857590 0.295064 0.090 Uiso 1 1 calc R U . . .
C32 C 0.5180(5) 0.7975(4) 0.2400(2) 0.075(3) Uani 1 1 d . . . . .
C33 C 0.5165(5) 0.8533(5) 0.2372(2) 0.084(3) Uani 1 1 d . . . . .
H33 H 0.511087 0.872414 0.257222 0.101 Uiso 1 1 calc R U . . .
C34 C 0.5225(5) 0.8829(5) 0.2060(2) 0.084(3) Uani 1 1 d . . . . .
H34 H 0.521642 0.921903 0.204553 0.101 Uiso 1 1 calc R U . . .
C35 C 0.5302(5) 0.8532(5) 0.1757(2) 0.075(3) Uani 1 1 d . . . . .
C36 C 0.5299(5) 0.7997(5) 0.1775(3) 0.099(3) Uani 1 1 d . . . . .
H36 H 0.530101 0.777886 0.157337 0.119 Uiso 1 1 calc R U . . .
C37 C 0.5292(6) 0.7713(5) 0.2128(2) 0.092(3) Uani 1 1 d . . . . .
H37 H 0.536475 0.736066 0.215062 0.110 Uiso 1 1 calc R U . . .
C38 C 0.5389(5) 0.8879(5) 0.1414(2) 0.075(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Ni Ni -3.0029 0.5091 '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'
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
O1 Ni1 O7 81.2(2) . . ?
O1 Ni1 O8 91.6(2) . 5_665 ?
O1 Ni1 O11 82.1(2) . 2_665 ?
O1 Ni1 N14 174.7(3) . 2_665 ?
O2 Ni1 O1 97.4(3) . . ?
O2 Ni1 O7 177.6(3) . . ?
O2 Ni1 O8 91.1(3) . 5_665 ?
O2 Ni1 O11 89.6(2) . 2_665 ?
O2 Ni1 N14 87.2(3) . 2_665 ?
O7 Ni1 O11 88.2(2) . 2_665 ?
O7 Ni1 N14 94.0(3) . 2_665 ?
O8 Ni1 O7 91.0(2) 5_665 . ?
O8 Ni1 O11 173.8(3) 5_665 2_665 ?
O8 Ni1 N14 90.8(3) 5_665 2_665 ?
N14 Ni1 O11 95.4(3) 2_665 2_665 ?
O1 Ni2 O4 94.0(3) . . ?
O1 Ni2 O11 79.4(2) . 2_665 ?
O1 Ni2 N5 171.9(3) . . ?
O3 Ni2 O1 88.0(3) . . ?
O3 Ni2 O4 87.5(3) . . ?
O3 Ni2 O11 92.1(3) . 2_665 ?
O3 Ni2 N5 89.6(3) . . ?
O4 Ni2 O11 173.4(3) . 2_665 ?
O4 Ni2 N5 93.7(3) . . ?
O12 Ni2 O1 95.3(2) 7_554 . ?
O12 Ni2 O3 175.1(3) 7_554 . ?
O12 Ni2 O4 88.6(3) 7_554 . ?
O12 Ni2 O11 92.2(3) 7_554 2_665 ?
O12 Ni2 N5 87.6(3) 7_554 . ?
N5 Ni2 O11 92.9(3) . 2_665 ?
O1 Ni3 O5 95.8(3) . . ?
O1 Ni3 O7 79.0(3) . . ?
O1 Ni3 O9 94.7(2) . 5_665 ?
O1 Ni3 O13 96.1(2) . 7_554 ?
O6 Ni3 O1 174.2(3) . . ?
O6 Ni3 O5 90.0(4) . . ?
O6 Ni3 O7 95.3(3) . . ?
O6 Ni3 O9 85.7(3) . 5_665 ?
O6 Ni3 O13 83.0(3) . 7_554 ?
O7 Ni3 O5 172.6(3) . . ?
O9 Ni3 O5 90.0(3) 5_665 . ?
O9 Ni3 O7 85.1(3) 5_665 . ?
O9 Ni3 O13 168.0(3) 5_665 7_554 ?
O13 Ni3 O5 93.9(3) 7_554 . ?
O13 Ni3 O7 91.9(3) 7_554 . ?
Ni1 O1 Ni2 100.8(3) . . ?
Ni1 O1 Ni3 98.2(3) . . ?
Ni1 O1 H1 130.3 . . ?
Ni2 O1 Ni3 127.6(3) . . ?
Ni2 O1 H1 100.9 . . ?
Ni3 O1 H1 102.9 . . ?
C7 O2 Ni1 123.7(6) . . ?
C7 O3 Ni2 130.0(8) . . ?
Ni2 O4 H4A 128.5 . . ?
Ni2 O4 H4B 127.5 . . ?
H4A O4 H4B 104.0 . . ?
Ni3 O5 H5A 127.6 . . ?
Ni3 O5 H5B 127.8 . . ?
H5A O5 H5B 104.6 . . ?
Ni3 O6 H6A 128.8 . . ?
Ni3 O6 H6B 126.8 . . ?
H6A O6 H6B 104.5 . . ?
Ni1 O7 Ni3 95.4(3) . . ?
Ni1 O7 H7A 114.9 . . ?
Ni1 O7 H7B 114.0 . . ?
Ni3 O7 H7A 114.7 . . ?
Ni3 O7 H7B 113.7 . . ?
H7A O7 H7B 104.5 . . ?
C38 O8 Ni1 127.8(6) . 9_564 ?
C38 O9 Ni3 125.9(5) . 9_564 ?
Ni1 O11 Ni2 89.8(3) 3_565 3_565 ?
C20 O11 Ni1 125.3(5) . 3_565 ?
C20 O11 Ni2 122.1(6) . 3_565 ?
C19 O12 Ni2 137.1(6) . 4_445 ?
C19 O13 Ni3 130.7(7) . 4_445 ?
H1A N1 H1B 120.0 . . ?
C10 N1 H1A 120.0 . . ?
C10 N1 H1B 120.0 . . ?
C27 N5 Ni2 121.4(6) . . ?
C27 N5 C31 117.9(8) . . ?
C31 N5 Ni2 120.2(6) . . ?
H10A N10 H10B 120.0 . . ?
C29 N10 H10A 120.0 . . ?
C29 N10 H10B 120.0 . . ?
C8 N14 Ni1 123.4(6) . 3_565 ?
C12 N14 Ni1 124.2(7) . 3_565 ?
C12 N14 C8 112.5(8) . . ?
C2 C1 C7 117.5(8) . . ?
C6 C1 C2 124.4(9) . . ?
C6 C1 C7 118.1(10) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 C1 117.6(10) . . ?
C3 C2 H2 121.2 . . ?
C2 C3 H3 117.2 . . ?
C2 C3 C4 125.6(12) . . ?
C4 C3 H3 117.2 . . ?
C5 C4 C3 112.5(12) . . ?
C5 C4 C9 123.7(13) . . ?
C9 C4 C3 123.4(13) . . ?
C4 C5 H5 116.5 . . ?
C4 C5 C6 127.0(11) . . ?
C6 C5 H5 116.5 . . ?
C1 C6 C5 111.8(11) . . ?
C1 C6 H6 124.1 . . ?
C5 C6 H6 124.1 . . ?
O2 C7 C1 114.9(8) . . ?
O3 C7 O2 127.2(9) . . ?
O3 C7 C1 117.2(9) . . ?
N14 C8 H8 117.0 . . ?
C9 C8 N14 125.9(9) . . ?
C9 C8 H8 117.0 . . ?
C8 C9 C4 120.2(11) . . ?
C8 C9 C10 116.8(11) . . ?
C10 C9 C4 122.2(12) . . ?
N1 C10 C9 120.3(11) . . ?
C11 C10 N1 118.1(10) . . ?
C11 C10 C9 121.2(11) . . ?
C10 C11 C12 117.0(9) . . ?
C10 C11 C13 127.0(10) . . ?
C12 C11 C13 115.9(8) . . ?
N14 C12 C11 125.5(9) . . ?
N14 C12 H12 117.3 . . ?
C11 C12 H12 117.3 . . ?
C14 C13 C11 120.4(10) . . ?
C18 C13 C11 123.2(11) . . ?
C18 C13 C14 115.7(12) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 C13 122.3(12) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(11) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C17 111.8(10) . . ?
C15 C16 C19 123.1(9) . . ?
C17 C16 C19 123.3(10) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 C16 123.0(12) . . ?
C18 C17 H17 118.5 . . ?
C13 C18 C17 123.7(14) . . ?
C13 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
O12 C19 O13 132.2(9) . . ?
O12 C19 C16 112.2(7) . . ?
O13 C19 C16 115.4(10) . . ?
O10 C20 O11 125.6(8) . . ?
O10 C20 C21 117.3(9) . . ?
O11 C20 C21 116.6(8) . . ?
C20 C21 C22 115.9(8) . . ?
C26 C21 C20 123.0(10) . . ?
C26 C21 C22 120.5(9) . . ?
C21 C22 H22 123.3 . . ?
C23 C22 C21 113.4(8) . . ?
C23 C22 H22 123.3 . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.8(10) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 C25 119.9(9) . . ?
C23 C24 C28 119.3(9) . . ?
C25 C24 C28 120.3(10) . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.6(11) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 121.7(11) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
N5 C27 H27 115.7 . . ?
N5 C27 C28 128.6(8) . . ?
C28 C27 H27 115.7 . . ?
C27 C28 C24 122.0(7) . . ?
C29 C28 C24 120.8(9) . . ?
C29 C28 C27 117.0(8) . . ?
N10 C29 C28 121.4(8) . . ?
N10 C29 C30 123.6(8) . . ?
C28 C29 C30 114.1(9) . . ?
C29 C30 C32 120.6(8) . . ?
C31 C30 C29 120.5(7) . . ?
C31 C30 C32 118.8(7) . . ?
N5 C31 C30 120.6(8) . . ?
N5 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C33 C32 C30 120.7(9) . . ?
C37 C32 C30 117.4(9) . . ?
C37 C32 C33 120.7(9) . . ?
C32 C33 H33 119.1 . . ?
C32 C33 C34 121.8(9) . . ?
C34 C33 H33 119.1 . . ?
C33 C34 H34 120.7 . . ?
C33 C34 C35 118.7(9) . . ?
C35 C34 H34 120.7 . . ?
C34 C35 C38 117.8(9) . . ?
C36 C35 C34 120.7(10) . . ?
C36 C35 C38 121.5(9) . . ?
C35 C36 H36 120.4 . . ?
C35 C36 C37 119.2(10) . . ?
C37 C36 H36 120.4 . . ?
C32 C37 C36 118.1(9) . . ?
C32 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
O8 C38 O9 125.9(7) . . ?
O8 C38 C35 121.5(8) . . ?
O9 C38 C35 112.5(8) . . ?
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 O1 1.965(6) . ?
Ni1 O2 1.964(7) . ?
Ni1 O7 2.041(7) . ?
Ni1 O8 1.999(5) 5_665 ?
Ni1 O11 2.137(6) 2_665 ?
Ni1 N14 2.103(7) 2_665 ?
Ni2 O1 2.012(6) . ?
Ni2 O3 2.007(6) . ?
Ni2 O4 2.023(7) . ?
Ni2 O11 2.204(7) 2_665 ?
Ni2 O12 1.970(5) 7_554 ?
Ni2 N5 2.095(7) . ?
Ni3 O1 2.045(6) . ?
Ni3 O5 2.099(9) . ?
Ni3 O6 2.022(7) . ?
Ni3 O7 2.057(6) . ?
Ni3 O9 2.048(6) 5_665 ?
Ni3 O13 2.051(6) 7_554 ?
O1 H1 0.8493 . ?
O2 C7 1.347(12) . ?
O3 C7 1.212(10) . ?
O4 H4A 0.8897 . ?
O4 H4B 0.8880 . ?
O5 H5A 0.8503 . ?
O5 H5B 0.8493 . ?
O6 H6A 0.8493 . ?
O6 H6B 0.8507 . ?
O7 H7A 0.8494 . ?
O7 H7B 0.8500 . ?
O8 C38 1.209(10) . ?
O9 C38 1.315(11) . ?
O10 C20 1.150(10) . ?
O11 C20 1.274(11) . ?
O12 C19 1.226(11) . ?
O13 C19 1.229(10) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C10 1.348(14) . ?
N5 C27 1.293(11) . ?
N5 C31 1.294(10) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N10 C29 1.341(11) . ?
N14 C8 1.368(12) . ?
N14 C12 1.338(11) . ?
C1 C2 1.447(14) . ?
C1 C6 1.416(15) . ?
C1 C7 1.557(13) . ?
C2 H2 0.9300 . ?
C2 C3 1.323(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.438(17) . ?
C4 C5 1.426(17) . ?
C4 C9 1.438(16) . ?
C5 H5 0.9300 . ?
C5 C6 1.437(14) . ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.259(14) . ?
C9 C10 1.406(13) . ?
C10 C11 1.294(13) . ?
C11 C12 1.349(13) . ?
C11 C13 1.545(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.402(14) . ?
C13 C18 1.253(15) . ?
C14 H14 0.9300 . ?
C14 C15 1.371(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.370(13) . ?
C16 C17 1.408(14) . ?
C16 C19 1.535(12) . ?
C17 H17 0.9300 . ?
C17 C18 1.350(15) . ?
C18 H18 0.9300 . ?
C20 C21 1.501(12) . ?
C21 C22 1.529(13) . ?
C21 C26 1.263(12) . ?
C22 H22 0.9300 . ?
C22 C23 1.472(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.332(13) . ?
C24 C25 1.376(14) . ?
C24 C28 1.495(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.405(13) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.439(13) . ?
C28 C29 1.379(12) . ?
C29 C30 1.473(12) . ?
C30 C31 1.466(12) . ?
C30 C32 1.532(11) . ?
C31 H31 0.9300 . ?
C32 C33 1.334(12) . ?
C32 C37 1.305(13) . ?
C33 H33 0.9300 . ?
C33 C34 1.357(12) . ?
C34 H34 0.9300 . ?
C34 C35 1.413(13) . ?
C35 C36 1.257(12) . ?
C35 C38 1.508(12) . ?
C36 H36 0.9300 . ?
C36 C37 1.504(13) . ?
C37 H37 0.9300 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C7 O3 -1.3(16) . . . . ?
Ni1 O2 C7 C1 -171.2(6) . . . . ?
Ni1 O8 C38 O9 -23.3(15) 9_564 . . . ?
Ni1 O8 C38 C35 156.8(7) 9_564 . . . ?
Ni1 O11 C20 O10 23.2(13) 3_565 . . . ?
Ni1 O11 C20 C21 -149.1(6) 3_565 . . . ?
Ni1 N14 C8 C9 -169.2(9) 3_565 . . . ?
Ni1 N14 C12 C11 178.3(8) 3_565 . . . ?
Ni2 O3 C7 O2 -14.3(17) . . . . ?
Ni2 O3 C7 C1 155.4(7) . . . . ?
Ni2 O11 C20 O10 -92.8(11) 3_565 . . . ?
Ni2 O11 C20 C21 94.9(8) 3_565 . . . ?
Ni2 O12 C19 O13 -3(2) 4_445 . . . ?
Ni2 O12 C19 C16 -176.6(7) 4_445 . . . ?
Ni2 N5 C27 C28 -175.2(9) . . . . ?
Ni2 N5 C31 C30 174.0(6) . . . . ?
Ni3 O9 C38 O8 10.2(16) 9_564 . . . ?
Ni3 O9 C38 C35 -169.9(6) 9_564 . . . ?
Ni3 O13 C19 O12 12.8(18) 4_445 . . . ?
Ni3 O13 C19 C16 -173.5(7) 4_445 . . . ?
O10 C20 C21 C22 -166.4(9) . . . . ?
O10 C20 C21 C26 22.3(14) . . . . ?
O11 C20 C21 C22 6.5(11) . . . . ?
O11 C20 C21 C26 -164.7(10) . . . . ?
N1 C10 C11 C12 -171.0(12) . . . . ?
N1 C10 C11 C13 12(2) . . . . ?
N5 C27 C28 C24 -179.2(11) . . . . ?
N5 C27 C28 C29 -4.2(17) . . . . ?
N10 C29 C30 C31 178.4(9) . . . . ?
N10 C29 C30 C32 2.3(15) . . . . ?
N14 C8 C9 C4 177.5(11) . . . . ?
N14 C8 C9 C10 -12.7(17) . . . . ?
C1 C2 C3 C4 5.5(17) . . . . ?
C2 C1 C6 C5 5.5(17) . . . . ?
C2 C1 C7 O2 178.2(9) . . . . ?
C2 C1 C7 O3 7.2(14) . . . . ?
C2 C3 C4 C5 -10(2) . . . . ?
C2 C3 C4 C9 177.4(12) . . . . ?
C3 C4 C5 C6 13(2) . . . . ?
C3 C4 C9 C8 -65(2) . . . . ?
C3 C4 C9 C10 126.1(15) . . . . ?
C4 C5 C6 C1 -11(2) . . . . ?
C4 C9 C10 N1 -12(2) . . . . ?
C4 C9 C10 C11 175.9(12) . . . . ?
C5 C4 C9 C8 123.2(16) . . . . ?
C5 C4 C9 C10 -46(2) . . . . ?
C6 C1 C2 C3 -3.3(17) . . . . ?
C6 C1 C7 O2 -0.5(14) . . . . ?
C6 C1 C7 O3 -171.5(11) . . . . ?
C7 C1 C2 C3 178.1(9) . . . . ?
C7 C1 C6 C5 -175.9(9) . . . . ?
C8 N14 C12 C11 -1.1(15) . . . . ?
C8 C9 C10 N1 178.7(12) . . . . ?
C8 C9 C10 C11 6.3(18) . . . . ?
C9 C4 C5 C6 -174.3(13) . . . . ?
C9 C10 C11 C12 1.6(18) . . . . ?
C9 C10 C11 C13 -175.3(11) . . . . ?
C10 C11 C12 N14 -4.1(17) . . . . ?
C10 C11 C13 C14 -140.3(13) . . . . ?
C10 C11 C13 C18 29(2) . . . . ?
C11 C13 C14 C15 179.5(11) . . . . ?
C11 C13 C18 C17 -174.3(12) . . . . ?
C12 N14 C8 C9 10.2(15) . . . . ?
C12 C11 C13 C14 42.9(17) . . . . ?
C12 C11 C13 C18 -147.7(14) . . . . ?
C13 C11 C12 N14 173.1(10) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C13 C18 C17 -4(2) . . . . ?
C14 C15 C16 C17 -13.5(18) . . . . ?
C14 C15 C16 C19 -178.5(11) . . . . ?
C15 C16 C17 C18 19(2) . . . . ?
C15 C16 C19 O12 -32.7(16) . . . . ?
C15 C16 C19 O13 152.4(12) . . . . ?
C16 C17 C18 C13 -10(3) . . . . ?
C17 C16 C19 O12 164.1(11) . . . . ?
C17 C16 C19 O13 -10.9(16) . . . . ?
C18 C13 C14 C15 9(2) . . . . ?
C19 C16 C17 C18 -176.3(12) . . . . ?
C20 C21 C22 C23 177.2(8) . . . . ?
C20 C21 C26 C25 -176.5(10) . . . . ?
C21 C22 C23 C24 5.4(13) . . . . ?
C22 C21 C26 C25 12.6(16) . . . . ?
C22 C23 C24 C25 -1.1(15) . . . . ?
C22 C23 C24 C28 -172.7(8) . . . . ?
C23 C24 C25 C26 1.5(16) . . . . ?
C23 C24 C28 C27 83.9(12) . . . . ?
C23 C24 C28 C29 -91.0(12) . . . . ?
C24 C25 C26 C21 -7.8(18) . . . . ?
C24 C28 C29 N10 -4.4(16) . . . . ?
C24 C28 C29 C30 -173.8(8) . . . . ?
C25 C24 C28 C27 -87.7(13) . . . . ?
C25 C24 C28 C29 97.5(12) . . . . ?
C26 C21 C22 C23 -11.3(13) . . . . ?
C27 N5 C31 C30 1.6(14) . . . . ?
C27 C28 C29 N10 -179.5(9) . . . . ?
C27 C28 C29 C30 11.2(13) . . . . ?
C28 C24 C25 C26 173.0(10) . . . . ?
C28 C29 C30 C31 -12.6(13) . . . . ?
C28 C29 C30 C32 171.4(9) . . . . ?
C29 C30 C31 N5 6.3(14) . . . . ?
C29 C30 C32 C33 125.2(10) . . . . ?
C29 C30 C32 C37 -66.8(13) . . . . ?
C30 C32 C33 C34 171.4(10) . . . . ?
C30 C32 C37 C36 -177.2(9) . . . . ?
C31 N5 C27 C28 -2.9(17) . . . . ?
C31 C30 C32 C33 -50.9(14) . . . . ?
C31 C30 C32 C37 117.0(11) . . . . ?
C32 C30 C31 N5 -177.6(9) . . . . ?
C32 C33 C34 C35 0.5(17) . . . . ?
C33 C32 C37 C36 -9.2(17) . . . . ?
C33 C34 C35 C36 1.6(17) . . . . ?
C33 C34 C35 C38 -178.2(9) . . . . ?
C34 C35 C36 C37 -7.0(17) . . . . ?
C34 C35 C38 O8 10.1(15) . . . . ?
C34 C35 C38 O9 -169.8(9) . . . . ?
C35 C36 C37 C32 11.1(18) . . . . ?
C36 C35 C38 O8 -169.6(11) . . . . ?
C36 C35 C38 O9 10.4(15) . . . . ?
C37 C32 C33 C34 3.9(18) . . . . ?
C38 C35 C36 C37 172.7(9) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.014 -0.007 0.006 11417 3149 ' '
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.52(5)
2 0.48(5)
