#------------------------------------------------------------------------------
#$Date: 2021-01-07 08:28:25 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260778 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/43/7704399.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_7704399
loop_
_publ_author_name
'Sanchez-Lievanos, Karla R'
'Tariq, Mehrin'
'Brennessel, William W.'
'Knowles, Kathryn E.'
_publ_section_title
;
 Heterometallic trinuclear oxo-centered clusters as single-source
 precursors for synthesis of stoichiometric monodisperse transition metal
 ferrite nanocrystals.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16348
_journal_page_last               16358
_journal_paper_doi               10.1039/d0dt01369b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C12 H6 F18 Fe2 Ni1 O16, 4(C3 H6 O), H2 O'
_chemical_formula_sum            'C24 H32 F18 Fe2 Ni O21'
_chemical_formula_weight         1168.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-23
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-04-23 deposited with the CCDC.	2020-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.6340(10)
_cell_angle_beta                 97.2410(10)
_cell_angle_gamma                111.9130(10)
_cell_formula_units_Z            2
_cell_length_a                   10.56550(10)
_cell_length_b                   11.5802(2)
_cell_length_c                   19.90320(10)
_cell_measurement_reflns_used    18978
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1320
_cell_measurement_theta_min      4.5140
_cell_volume                     2229.74(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00   4.00   0.50    0.14    --  -49.75  38.00  90.00   52
  2  ω    -31.00  21.00   0.50    0.14    --  -49.75  38.00  30.00  104
  3  ω    -46.00 -21.00   0.50    0.57    --  -84.25  96.00 -95.00   50
  4  ω    -72.00   8.00   0.50    0.14    --  -49.75  96.00 -95.00  160
  5  ω     -5.00  58.00   0.50    0.14    --   49.75 -96.00 155.00  126
  6  ω     43.00  71.00   0.50    0.57    --  105.75 -96.00 155.00   56
  7  ω     88.00 114.00   0.50    0.57    --  105.75 -77.00 150.00   52
  8  ω     72.00 106.00   0.50    0.57    --  105.75 -94.00  90.00   68
  9  ω     65.00 104.00   0.50    0.57    --  105.75 -94.00  60.00   78
 10  ω     76.00 106.00   0.50    0.57    --  105.75 -94.00   0.00   60
 11  ω     59.00 106.00   0.50    0.57    --  105.75 -94.00 -90.00   94
 12  ω     81.00 106.00   0.50    0.57    --  105.75 -94.00-150.00   50
 13  ω     38.00  94.00   0.50    0.57    --  105.75 -77.00 -90.00  112
 14  ω     41.00  72.00   0.50    0.57    --  105.75 -61.00 -90.00   62
 15  ω     46.00  76.00   0.50    0.57    --  105.75 -94.00-150.00   60
 16  ω     47.00  79.00   0.50    0.57    --  105.75 -61.00-150.00   64
 17  ω    103.00 175.00   0.50    0.57    --  105.75  15.00-120.00  144
 18  ω    106.00 167.00   0.50    0.57    --  105.75  96.00 -95.00  122
 19  ω    124.00 166.00   0.50    0.57    --  105.75  15.00  30.00   84
 20  ω    153.00 178.00   0.50    0.57    --  105.75  30.00 120.00   50
 21  ω    105.00 141.00   0.50    0.57    --  105.75  30.00 120.00   72
 22  ω    102.00 174.00   0.50    0.57    --  105.75  15.00   0.00  144
 23  ω     92.00 121.00   0.50    0.57    --  105.75  61.00-150.00   58
 24  ω     96.00 147.00   0.50    0.57    --  105.75  61.00-120.00  102
 25  ω    115.00 143.00   0.50    0.57    --  105.75  15.00-180.00   56
 26  ω     99.00 175.00   0.50    0.57    --  105.75  45.00-180.00  152
 27  ω    105.00 173.00   0.50    0.57    --  105.75  15.00 -90.00  136
 28  ω    101.00 126.00   0.50    0.57    --  105.75  15.00 -30.00   50
 29  ω     43.00  69.00   0.50    0.57    --  105.75 -61.00 -30.00   52
 30  ω     47.00 105.00   0.50    0.57    --  105.75 -94.00 -30.00  116
 31  ω     52.00 111.00   0.50    0.57    --  105.75-125.00  30.00  118
 32  ω     44.00  73.00   0.50    0.57    --  105.75-125.00 120.00   58
 33  ω     47.00 109.00   0.50    0.57    --  105.75-125.00 150.00  124
 34  ω     69.00 107.00   0.50    0.57    --  105.75-104.00 174.71   76
 35  ω     35.00  61.00   0.50    0.57    --  105.75 -77.00 150.00   52
 36  ω     43.00  88.00   0.50    0.57    --  105.75-125.00  90.00   90
 37  ω     34.00 104.00   0.50    0.57    --  105.75 -94.00  30.00  140
 38  ω     34.00  71.00   0.50    0.57    --  105.75 -61.00  60.00   74
 39  ω     35.00  60.00   0.50    0.57    --  105.75 -94.00   0.00   50
 40  ω     34.00  68.00   0.50    0.57    --  105.75 -61.00  30.00   68
 41  ω    -22.00   3.00   0.50    0.14    --   49.75 -19.00 150.00   50
 42  ω    -20.00  13.00   0.50    0.14    --   49.75 -19.00  60.00   66
 43  ω     -3.00  22.00   0.50    0.14    --  -49.75  19.00-150.00   50
 44  ω    -21.00  59.00   0.50    0.14    --   49.75 -57.00-180.00  160
 45  ω     34.00  76.00   0.50    0.57    --  105.75 -61.00-180.00   84
 46  ω     41.00 106.00   0.50    0.57    --  105.75 -94.00-180.00  130
 47  ω     45.00  82.00   0.50    0.57    --  105.75-125.00-180.00   74
 48  ω    -21.00  42.00   0.50    0.14    --   49.75 -38.00-150.00  126
 49  ω   -113.00 -80.00   0.50    0.14    --  -49.75-125.00 -60.00   66
 50  ω   -153.00-116.00   0.50    0.57    --  -84.25 -45.00   0.00   74
 51  ω   -124.00 -90.00   0.50    0.57    --  -84.25 -96.00 155.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0968565000
_diffrn_orient_matrix_UB_12      0.0805487000
_diffrn_orient_matrix_UB_13      0.0636276000
_diffrn_orient_matrix_UB_21      -0.1255337000
_diffrn_orient_matrix_UB_22      -0.0197708000
_diffrn_orient_matrix_UB_23      0.0365695000
_diffrn_orient_matrix_UB_31      0.0128525000
_diffrn_orient_matrix_UB_32      -0.1178767000
_diffrn_orient_matrix_UB_33      0.0276566000
_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  0.0731
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.059
_diffrn_reflns_theta_min         4.136
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         9354
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0522
_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)+(0.0980P)²+0.6801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8318
_reflns_number_total             9354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01369b2.cif
_cod_data_source_block           knoks17
_cod_depositor_comments
'Adding full bibliography for 7704398--7704402.cif.'
_cod_database_code               7704399
_shelx_shelxl_version_number     2018/3
_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_max   0.703
_shelx_estimated_absorpt_t_min   0.166
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{Ni1, Fe1}
{Ni2, Fe2}
{Ni3, Fe3}
3. Restrained distances
 C1-C2 \\sim C1-C2'
 with sigma of 0.01
 C2-F1 \\sim C2-F2 \\sim C2-F3 \\sim C2'-F1' \\sim C2'-F2' \\sim C2'-F3'
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1'-F2' \\sim F2'-F3' \\sim F3'-F1'
 with sigma of 0.02
 C19-O19 \\sim C19'-O19' \\sim C22-O21 \\sim C22'-O21'
 with sigma of 0.01
 C19-C20 \\sim C19-C21 \\sim C19'-C20' \\sim C19'-C21' \\sim C22-C23 \\sim
C22-C24 \\sim C22'-C23' ~
 C22'-C24'
 with sigma of 0.01
 O19-C20 \\sim O19-C21 \\sim O19'-C20' \\sim O19'-C21' \\sim O21-C23 \\sim
O21-C24 \\sim O21'-C23' ~
 O21'-C24'
 with sigma of 0.02
 C20-C21 \\sim C20'-C21' \\sim C23-C24 \\sim C23'-C24'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1A
Uanis(Ni1) = Uanis(Fe1)
Uanis(Ni2) = Uanis(Fe2)
Uanis(Ni3) = Uanis(Fe3)
5. Rigid body (RIGU) restrains
 F1, F2, F3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1', F2', F3', C2'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19', C19', C20', C21'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21', C22', C23', C24'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Ni1)+Sof(Fe1)]+1*[Sof(Ni2)+Sof(Fe2)]+1*[Sof(Ni3)+Sof(Fe3)]=2 with esd
 of 0.0001
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C2')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C2)=FVAR(1)
 Sof(O19')=Sof(C19')=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21')=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(O20')=Sof(H20I)=Sof(H20J)=Sof(O21')=
 Sof(C22')=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O19)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(O20)=Sof(H20G)=Sof(H20H)=Sof(O21)=Sof(C22)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(Ni1)=1-FVAR(3)
 Sof(Fe1)=FVAR(3)
 Sof(Ni2)=1-FVAR(4)
 Sof(Fe2)=FVAR(4)
 Sof(Ni3)=1-FVAR(5)
 Sof(Fe3)=FVAR(5)
7.a Riding coordinates:
 O1(H1A,H1B), O20(H20G,H20H), O20'(H20I,H20J)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20'(H20D,H20E,H20F),
 C21'(H21D,H21E,H21F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23'(H23D,H23E,
 H23F), C24'(H24D,H24E,H24F)
;
_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 2.728
_oxdiff_exptl_absorpt_empirical_full_min 0.401
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 0.57604(4) 0.49064(4) 0.67572(2) 0.02091(12) Uani 0.083(3) 1 d . U P A 2
Ni2 Ni 0.43617(4) 0.55968(4) 0.80221(2) 0.02034(12) Uani 0.218(3) 1 d . U P A 2
Ni3 Ni 0.75936(4) 0.57699(4) 0.83063(2) 0.01993(12) Uani 0.698(3) 1 d . U P A 2
Fe1 Fe 0.57604(4) 0.49064(4) 0.67572(2) 0.02091(12) Uani 0.917(3) 1 d . U P A 1
Fe2 Fe 0.43617(4) 0.55968(4) 0.80221(2) 0.02034(12) Uani 0.782(3) 1 d . U P A 1
Fe3 Fe 0.75936(4) 0.57699(4) 0.83063(2) 0.01993(12) Uani 0.302(3) 1 d . U P A 1
F1 F 0.1427(6) 0.1692(5) 0.6199(2) 0.070(2) Uani 0.587(12) 1 d D . P B 1
F1' F 0.1239(12) 0.1602(7) 0.7451(4) 0.086(4) Uani 0.413(12) 1 d D . P B 2
F2 F 0.2113(6) 0.1167(4) 0.7117(5) 0.085(3) Uani 0.587(12) 1 d D U P B 1
F2' F 0.0737(9) 0.2091(7) 0.6494(7) 0.108(6) Uani 0.413(12) 1 d D . P B 2
F3 F 0.0644(5) 0.2003(5) 0.7060(4) 0.079(3) Uani 0.587(12) 1 d D . P B 1
F3' F 0.2031(9) 0.1139(6) 0.6622(6) 0.081(4) Uani 0.413(12) 1 d D U P B 2
F4 F 0.3726(3) 0.7330(2) 0.56152(10) 0.0543(6) Uani 1 1 d . . . . .
F5 F 0.5052(3) 0.8723(2) 0.63964(17) 0.0727(8) Uani 1 1 d . . . . .
F6 F 0.2899(3) 0.7865(3) 0.64393(13) 0.0621(7) Uani 1 1 d . . . . .
F7 F 0.40210(18) 0.33506(19) 0.99290(9) 0.0365(4) Uani 1 1 d . . . . .
F8 F 0.4601(3) 0.22031(18) 0.92549(11) 0.0597(7) Uani 1 1 d . . . . .
F9 F 0.6079(2) 0.3415(2) 1.00726(10) 0.0431(5) Uani 1 1 d . . . . .
F10 F 0.6237(2) 0.92792(19) 0.94890(12) 0.0464(5) Uani 1 1 d . . . . .
F11 F 0.7355(3) 0.99257(18) 0.86657(11) 0.0530(6) Uani 1 1 d . . . . .
F12 F 0.8346(2) 0.94900(17) 0.95687(10) 0.0415(4) Uani 1 1 d . . . . .
F13 F 0.8546(2) 0.22117(19) 0.78267(10) 0.0434(5) Uani 1 1 d . . . . .
F14 F 0.6347(3) 0.1344(2) 0.76700(16) 0.0602(7) Uani 1 1 d . . . . .
F15 F 0.7434(3) 0.1727(2) 0.68140(10) 0.0518(6) Uani 1 1 d . . . . .
F16 F 1.08880(19) 0.84138(19) 0.71249(10) 0.0419(5) Uani 1 1 d . . . . .
F17 F 0.9244(3) 0.9002(2) 0.6787(2) 0.0797(10) Uani 1 1 d . . . . .
F18 F 0.9733(3) 0.7762(3) 0.61330(11) 0.0717(9) Uani 1 1 d . . . . .
O1 O 0.5665(2) 0.43501(19) 0.57539(10) 0.0286(4) Uani 1 1 d . . . . .
H1A H 0.626887 0.487075 0.555659 0.043 Uiso 1 1 d R U . A .
H1B H 0.517757 0.368685 0.549479 0.043 Uiso 1 1 d R U . . .
O2 O 0.2678(2) 0.5757(2) 0.83819(11) 0.0266(4) Uani 1 1 d . . . . .
H2A H 0.257(5) 0.639(5) 0.844(2) 0.050(13) Uiso 1 1 d . . . . .
H2B H 0.215(4) 0.525(4) 0.860(2) 0.036(10) Uiso 1 1 d . . . . .
O3 O 0.9415(2) 0.6150(2) 0.89543(10) 0.0239(4) Uani 1 1 d . . . . .
H3A H 1.008(5) 0.666(4) 0.883(2) 0.040(11) Uiso 1 1 d . . . . .
H3B H 0.963(4) 0.560(4) 0.900(2) 0.031(10) Uiso 1 1 d . . . . .
O4 O 0.3869(2) 0.34730(18) 0.66645(10) 0.0271(4) Uani 1 1 d . . . . .
O5 O 0.2906(2) 0.39578(18) 0.75315(10) 0.0263(4) Uani 1 1 d . . . . .
O6 O 0.4885(2) 0.61002(19) 0.64007(10) 0.0260(4) Uani 1 1 d . . . . .
O7 O 0.3946(2) 0.66104(18) 0.72715(9) 0.0256(4) Uani 1 1 d . . . . .
O8 O 0.4444(2) 0.45763(18) 0.88334(9) 0.0246(4) Uani 1 1 d . . . . .
O9 O 0.66632(19) 0.47502(18) 0.90363(9) 0.0244(4) Uani 1 1 d . . . . .
O10 O 0.54562(19) 0.72819(17) 0.85768(9) 0.0234(4) Uani 1 1 d . . . . .
O11 O 0.7655(2) 0.73988(18) 0.87812(10) 0.0255(4) Uani 1 1 d . . . . .
O12 O 0.78338(19) 0.41669(18) 0.79776(9) 0.0247(4) Uani 1 1 d . . . . .
O13 O 0.6564(2) 0.3579(2) 0.69313(10) 0.0294(4) Uani 1 1 d . . . . .
O14 O 0.8824(2) 0.69002(19) 0.76828(10) 0.0269(4) Uani 1 1 d . . . . .
O15 O 0.7600(2) 0.62343(19) 0.66319(10) 0.0284(4) Uani 1 1 d . . . . .
O16 O 0.58712(19) 0.54122(16) 0.76835(9) 0.0214(4) Uani 1 1 d . . . . .
C1 C 0.2964(3) 0.3288(2) 0.70397(13) 0.0236(5) Uani 1 1 d D . . . .
C2 C 0.1751(5) 0.2013(5) 0.6847(3) 0.0344(19) Uani 0.587(12) 1 d D U P B 1
C2' C 0.1736(7) 0.2012(6) 0.6909(4) 0.032(3) Uani 0.413(12) 1 d D U P B 2
C3 C 0.4283(3) 0.6670(2) 0.66914(14) 0.0242(5) Uani 1 1 d . . . . .
C4 C 0.3965(4) 0.7653(3) 0.62806(16) 0.0351(7) Uani 1 1 d . . . . .
C5 C 0.5434(3) 0.4337(2) 0.91082(12) 0.0202(5) Uani 1 1 d . . . . .
C6 C 0.5036(3) 0.3318(3) 0.96049(14) 0.0267(5) Uani 1 1 d . . . . .
C7 C 0.6711(3) 0.7787(2) 0.88006(13) 0.0215(5) Uani 1 1 d . . . . .
C8 C 0.7172(3) 0.9135(3) 0.91399(14) 0.0278(6) Uani 1 1 d . . . . .
C9 C 0.7271(3) 0.3445(2) 0.74521(13) 0.0225(5) Uani 1 1 d . . . . .
C10 C 0.7410(3) 0.2166(3) 0.74334(15) 0.0300(6) Uani 1 1 d . . . . .
C11 C 0.8578(3) 0.6939(2) 0.70637(14) 0.0230(5) Uani 1 1 d . . . . .
C12 C 0.9626(3) 0.8048(3) 0.67722(17) 0.0368(7) Uani 1 1 d . . . . .
O17 O 0.1930(2) 0.77421(19) 0.86592(12) 0.0327(5) Uani 1 1 d . . . . .
C13 C 0.2317(3) 0.8838(3) 0.85395(15) 0.0281(6) Uani 1 1 d . . . . .
C14 C 0.1515(4) 0.9615(3) 0.86996(18) 0.0375(7) Uani 1 1 d . . . . .
H14A H 0.068084 0.909903 0.885447 0.056 Uiso 1 1 calc R U . . .
H14B H 0.128904 0.997032 0.829763 0.056 Uiso 1 1 calc R U . . .
H14C H 0.206116 1.027461 0.904938 0.056 Uiso 1 1 calc R U . . .
C15 C 0.3603(3) 0.9428(3) 0.82382(18) 0.0353(7) Uani 1 1 d . . . . .
H15A H 0.426821 1.008878 0.855573 0.053 Uiso 1 1 calc R U . . .
H15B H 0.339409 0.976333 0.782573 0.053 Uiso 1 1 calc R U . . .
H15C H 0.397512 0.880979 0.813896 0.053 Uiso 1 1 calc R U . . .
O18 O 1.0615(2) 0.44352(19) 0.91158(11) 0.0308(4) Uani 1 1 d . . . . .
C16 C 1.0083(3) 0.3379(3) 0.92833(14) 0.0265(5) Uani 1 1 d . . . . .
C17 C 0.8700(3) 0.2947(3) 0.95081(15) 0.0291(6) Uani 1 1 d . . . . .
H17A H 0.847744 0.365823 0.961864 0.044 Uiso 1 1 calc R U . . .
H17B H 0.871604 0.250302 0.990249 0.044 Uiso 1 1 calc R U . . .
H17C H 0.801524 0.240352 0.914784 0.044 Uiso 1 1 calc R U . . .
C18 C 1.0799(4) 0.2488(3) 0.9263(2) 0.0480(9) Uani 1 1 d . . . . .
H18A H 1.162640 0.285595 0.906605 0.072 Uiso 1 1 calc R U . . .
H18B H 1.019992 0.172715 0.899167 0.072 Uiso 1 1 calc R U . . .
H18C H 1.103301 0.230671 0.971674 0.072 Uiso 1 1 calc R U . . .
O19 O 0.8249(9) 0.5268(13) 0.4038(6) 0.047(2) Uani 0.557(5) 1 d D U P C 1
C19 C 0.9441(8) 0.5579(11) 0.3943(5) 0.038(2) Uani 0.557(5) 1 d D U P C 1
C20 C 0.9754(13) 0.5077(14) 0.3311(6) 0.059(3) Uani 0.557(5) 1 d D U P C 1
H20A H 0.899907 0.431450 0.312612 0.088 Uiso 0.557(5) 1 calc R U P C 1
H20B H 1.058012 0.491383 0.341427 0.088 Uiso 0.557(5) 1 calc R U P C 1
H20C H 0.988455 0.567903 0.298344 0.088 Uiso 0.557(5) 1 calc R U P C 1
C21 C 1.0618(8) 0.6482(9) 0.4432(4) 0.057(2) Uani 0.557(5) 1 d D U P C 1
H21A H 1.027365 0.690417 0.474571 0.086 Uiso 0.557(5) 1 calc R U P C 1
H21B H 1.123555 0.708423 0.418767 0.086 Uiso 0.557(5) 1 calc R U P C 1
H21C H 1.110195 0.603931 0.467927 0.086 Uiso 0.557(5) 1 calc R U P C 1
O19' O 0.8384(10) 0.511(2) 0.3933(8) 0.057(4) Uani 0.443(5) 1 d D U P C 2
C19' C 0.9517(9) 0.5313(12) 0.3780(5) 0.026(2) Uani 0.443(5) 1 d D U P C 2
C20' C 0.9651(14) 0.4946(13) 0.3074(4) 0.032(2) Uani 0.443(5) 1 d D U P C 2
H20D H 0.895516 0.413413 0.291648 0.048 Uiso 0.443(5) 1 calc R U P C 2
H20E H 1.054832 0.492226 0.306928 0.048 Uiso 0.443(5) 1 calc R U P C 2
H20F H 0.953580 0.554594 0.277979 0.048 Uiso 0.443(5) 1 calc R U P C 2
C21' C 1.0786(8) 0.5837(10) 0.4300(4) 0.0432(19) Uani 0.443(5) 1 d D U P C 2
H21D H 1.149685 0.647442 0.411618 0.065 Uiso 0.443(5) 1 calc R U P C 2
H21E H 1.109602 0.518218 0.441949 0.065 Uiso 0.443(5) 1 calc R U P C 2
H21F H 1.058394 0.619282 0.469770 0.065 Uiso 0.443(5) 1 calc R U P C 2
O20 O 0.6849(4) 0.6041(4) 0.49313(19) 0.0340(10) Uani 0.557(5) 1 d . . P C 1
H20G H 0.714664 0.683296 0.500315 0.051 Uiso 0.557(5) 1 d R U P C 1
H20H H 0.732514 0.577326 0.469985 0.051 Uiso 0.557(5) 1 d R U P C 1
O20' O 0.7801(6) 0.5738(5) 0.5176(3) 0.0408(14) Uani 0.443(5) 1 d . . P C 2
H20I H 0.774528 0.539147 0.478150 0.061 Uiso 0.443(5) 1 d R U P C 2
H20J H 0.759938 0.637017 0.510150 0.061 Uiso 0.443(5) 1 d R U P C 2
O21 O 0.2174(9) 0.1394(6) 0.4837(4) 0.093(3) Uani 0.557(5) 1 d D . P C 1
C22 C 0.2683(9) 0.0666(7) 0.5039(4) 0.059(2) Uani 0.557(5) 1 d D U P C 1
C23 C 0.4009(16) 0.1094(13) 0.5518(12) 0.062(3) Uani 0.557(5) 1 d D U P C 1
H23A H 0.455679 0.194499 0.546075 0.092 Uiso 0.557(5) 1 calc R U P C 1
H23B H 0.450372 0.057217 0.542572 0.092 Uiso 0.557(5) 1 calc R U P C 1
H23C H 0.382004 0.103871 0.597775 0.092 Uiso 0.557(5) 1 calc R U P C 1
C24 C 0.1950(15) -0.0703(7) 0.4852(7) 0.107(5) Uani 0.557(5) 1 d D . P C 1
H24A H 0.129101 -0.104129 0.515299 0.161 Uiso 0.557(5) 1 calc R U P C 1
H24B H 0.260596 -0.109746 0.488945 0.161 Uiso 0.557(5) 1 calc R U P C 1
H24C H 0.147964 -0.085325 0.439162 0.161 Uiso 0.557(5) 1 calc R U P C 1
O21' O 0.3307(6) 0.2359(5) 0.5087(3) 0.0434(15) Uani 0.443(5) 1 d D . P C 2
C22' C 0.3152(10) 0.1292(7) 0.5175(5) 0.048(2) Uani 0.443(5) 1 d D U P C 2
C23' C 0.423(2) 0.0987(16) 0.5602(17) 0.063(4) Uani 0.443(5) 1 d D U P C 2
H23D H 0.483534 0.083755 0.531808 0.094 Uiso 0.443(5) 1 calc R U P C 2
H23E H 0.379530 0.025163 0.582199 0.094 Uiso 0.443(5) 1 calc R U P C 2
H23F H 0.475390 0.167550 0.593951 0.094 Uiso 0.443(5) 1 calc R U P C 2
C24' C 0.1850(13) 0.0231(9) 0.4865(7) 0.080(4) Uani 0.443(5) 1 d D U P C 2
H24D H 0.117585 0.055349 0.468540 0.120 Uiso 0.443(5) 1 calc R U P C 2
H24E H 0.150069 -0.031184 0.520590 0.120 Uiso 0.443(5) 1 calc R U P C 2
H24F H 0.203860 -0.023087 0.450369 0.120 Uiso 0.443(5) 1 calc R U P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
O4 Ni1 O1 84.06(8) . . ?
O6 Ni1 O1 85.69(8) . . ?
O6 Ni1 O4 91.39(8) . . ?
O6 Ni1 O13 169.43(8) . . ?
O13 Ni1 O1 83.86(8) . . ?
O13 Ni1 O4 86.00(9) . . ?
O15 Ni1 O1 83.71(8) . . ?
O15 Ni1 O4 167.72(8) . . ?
O15 Ni1 O6 86.61(8) . . ?
O15 Ni1 O13 93.78(9) . . ?
O16 Ni1 O1 179.15(8) . . ?
O16 Ni1 O4 96.32(8) . . ?
O16 Ni1 O6 95.05(8) . . ?
O16 Ni1 O13 95.41(8) . . ?
O16 Ni1 O15 95.92(8) . . ?
O5 Ni2 O2 82.91(9) . . ?
O5 Ni2 O8 85.54(8) . . ?
O7 Ni2 O2 84.32(8) . . ?
O7 Ni2 O5 92.08(8) . . ?
O7 Ni2 O8 169.26(8) . . ?
O8 Ni2 O2 85.00(8) . . ?
O10 Ni2 O2 84.83(8) . . ?
O10 Ni2 O5 167.71(8) . . ?
O10 Ni2 O7 85.89(8) . . ?
O10 Ni2 O8 94.21(8) . . ?
O16 Ni2 O2 178.62(9) . . ?
O16 Ni2 O5 95.72(8) . . ?
O16 Ni2 O7 95.87(8) . . ?
O16 Ni2 O8 94.79(7) . . ?
O16 Ni2 O10 96.55(8) . . ?
O9 Ni3 O3 85.61(8) . . ?
O9 Ni3 O11 92.30(8) . . ?
O9 Ni3 O12 84.72(8) . . ?
O9 Ni3 O14 170.62(8) . . ?
O11 Ni3 O3 84.05(8) . . ?
O11 Ni3 O12 168.94(8) . . ?
O11 Ni3 O14 85.37(8) . . ?
O12 Ni3 O3 85.11(8) . . ?
O12 Ni3 O14 95.86(8) . . ?
O14 Ni3 O3 85.11(8) . . ?
O16 Ni3 O3 179.50(8) . . ?
O16 Ni3 O9 94.85(7) . . ?
O16 Ni3 O11 96.13(8) . . ?
O16 Ni3 O12 94.74(8) . . ?
O16 Ni3 O14 94.43(7) . . ?
O4 Fe1 O1 84.06(8) . . ?
O6 Fe1 O1 85.69(8) . . ?
O6 Fe1 O4 91.39(8) . . ?
O6 Fe1 O13 169.43(8) . . ?
O13 Fe1 O1 83.86(8) . . ?
O13 Fe1 O4 86.00(9) . . ?
O15 Fe1 O1 83.71(8) . . ?
O15 Fe1 O4 167.72(8) . . ?
O15 Fe1 O6 86.61(8) . . ?
O15 Fe1 O13 93.78(9) . . ?
O16 Fe1 O1 179.15(8) . . ?
O16 Fe1 O4 96.32(8) . . ?
O16 Fe1 O6 95.05(8) . . ?
O16 Fe1 O13 95.41(8) . . ?
O16 Fe1 O15 95.92(8) . . ?
O5 Fe2 O2 82.91(9) . . ?
O5 Fe2 O8 85.54(8) . . ?
O7 Fe2 O2 84.32(8) . . ?
O7 Fe2 O5 92.08(8) . . ?
O7 Fe2 O8 169.26(8) . . ?
O8 Fe2 O2 85.00(8) . . ?
O10 Fe2 O2 84.83(8) . . ?
O10 Fe2 O5 167.71(8) . . ?
O10 Fe2 O7 85.89(8) . . ?
O10 Fe2 O8 94.21(8) . . ?
O16 Fe2 O2 178.62(9) . . ?
O16 Fe2 O5 95.72(8) . . ?
O16 Fe2 O7 95.87(8) . . ?
O16 Fe2 O8 94.79(7) . . ?
O16 Fe2 O10 96.55(8) . . ?
O9 Fe3 O3 85.61(8) . . ?
O9 Fe3 O11 92.30(8) . . ?
O9 Fe3 O12 84.72(8) . . ?
O9 Fe3 O14 170.62(8) . . ?
O11 Fe3 O3 84.05(8) . . ?
O11 Fe3 O12 168.94(8) . . ?
O11 Fe3 O14 85.37(8) . . ?
O12 Fe3 O3 85.11(8) . . ?
O12 Fe3 O14 95.86(8) . . ?
O14 Fe3 O3 85.11(8) . . ?
O16 Fe3 O3 179.50(8) . . ?
O16 Fe3 O9 94.85(7) . . ?
O16 Fe3 O11 96.13(8) . . ?
O16 Fe3 O12 94.74(8) . . ?
O16 Fe3 O14 94.43(7) . . ?
Ni1 O1 H1A 113.9 . . ?
Ni1 O1 H1B 133.7 . . ?
Fe1 O1 H1A 113.9 . . ?
Fe1 O1 H1B 133.7 . . ?
H1A O1 H1B 112.3 . . ?
Ni2 O2 H2A 124(4) . . ?
Ni2 O2 H2B 126(3) . . ?
Fe2 O2 H2A 124(4) . . ?
Fe2 O2 H2B 126(3) . . ?
H2A O2 H2B 107(4) . . ?
Ni3 O3 H3A 113(3) . . ?
Ni3 O3 H3B 116(3) . . ?
Fe3 O3 H3A 113(3) . . ?
Fe3 O3 H3B 116(3) . . ?
H3A O3 H3B 103(4) . . ?
C1 O4 Ni1 128.69(19) . . ?
C1 O4 Fe1 128.69(19) . . ?
C1 O5 Ni2 129.82(18) . . ?
C1 O5 Fe2 129.82(18) . . ?
C3 O6 Ni1 130.38(17) . . ?
C3 O6 Fe1 130.38(17) . . ?
C3 O7 Ni2 128.07(18) . . ?
C3 O7 Fe2 128.07(18) . . ?
C5 O8 Ni2 128.72(17) . . ?
C5 O8 Fe2 128.72(17) . . ?
C5 O9 Ni3 129.56(16) . . ?
C5 O9 Fe3 129.56(16) . . ?
C7 O10 Ni2 129.99(18) . . ?
C7 O10 Fe2 129.99(18) . . ?
C7 O11 Ni3 129.24(18) . . ?
C7 O11 Fe3 129.24(18) . . ?
C9 O12 Ni3 129.53(17) . . ?
C9 O12 Fe3 129.53(17) . . ?
C9 O13 Ni1 130.09(19) . . ?
C9 O13 Fe1 130.09(19) . . ?
C11 O14 Ni3 128.90(18) . . ?
C11 O14 Fe3 128.90(18) . . ?
C11 O15 Ni1 130.18(17) . . ?
C11 O15 Fe1 130.18(17) . . ?
Ni1 O16 Ni2 121.27(9) . . ?
Ni1 O16 Ni3 119.44(10) . . ?
Ni2 O16 Ni3 119.29(9) . . ?
Fe1 O16 Fe2 121.27(9) . . ?
Fe1 O16 Fe3 119.44(10) . . ?
Fe2 O16 Fe3 119.29(9) . . ?
O4 C1 C2 112.8(3) . . ?
O4 C1 C2' 116.8(4) . . ?
O5 C1 O4 130.2(3) . . ?
O5 C1 C2 117.0(3) . . ?
O5 C1 C2' 112.9(3) . . ?
F1 C2 F2 107.3(6) . . ?
F1 C2 C1 113.6(4) . . ?
F2 C2 C1 108.0(4) . . ?
F3 C2 F1 106.4(6) . . ?
F3 C2 F2 109.5(6) . . ?
F3 C2 C1 111.9(4) . . ?
F1' C2' F3' 106.9(7) . . ?
F1' C2' C1 114.0(6) . . ?
F2' C2' F1' 106.8(8) . . ?
F2' C2' F3' 105.2(8) . . ?
F2' C2' C1 110.1(6) . . ?
F3' C2' C1 113.2(6) . . ?
O6 C3 O7 130.4(2) . . ?
O6 C3 C4 114.6(2) . . ?
O7 C3 C4 114.9(2) . . ?
F4 C4 C3 112.3(3) . . ?
F5 C4 F4 106.7(3) . . ?
F5 C4 C3 109.1(3) . . ?
F6 C4 F4 107.3(3) . . ?
F6 C4 F5 107.9(3) . . ?
F6 C4 C3 113.3(2) . . ?
O8 C5 C6 114.1(2) . . ?
O9 C5 O8 131.0(2) . . ?
O9 C5 C6 114.9(2) . . ?
F7 C6 C5 112.2(2) . . ?
F8 C6 F7 107.6(3) . . ?
F8 C6 C5 108.9(2) . . ?
F9 C6 F7 107.1(2) . . ?
F9 C6 F8 108.1(2) . . ?
F9 C6 C5 112.7(2) . . ?
O10 C7 C8 114.4(2) . . ?
O11 C7 O10 130.7(3) . . ?
O11 C7 C8 114.9(2) . . ?
F10 C8 C7 112.3(2) . . ?
F11 C8 F10 107.3(2) . . ?
F11 C8 C7 109.6(2) . . ?
F12 C8 F10 106.9(2) . . ?
F12 C8 F11 107.7(3) . . ?
F12 C8 C7 112.8(2) . . ?
O12 C9 O13 129.8(2) . . ?
O12 C9 C10 116.4(2) . . ?
O13 C9 C10 113.7(2) . . ?
F13 C10 C9 112.2(3) . . ?
F14 C10 F13 106.7(2) . . ?
F14 C10 C9 109.2(2) . . ?
F15 C10 F13 107.6(3) . . ?
F15 C10 F14 108.3(3) . . ?
F15 C10 C9 112.6(2) . . ?
O14 C11 O15 130.4(2) . . ?
O14 C11 C12 115.5(2) . . ?
O15 C11 C12 114.2(2) . . ?
F16 C12 F18 106.3(3) . . ?
F16 C12 C11 112.0(2) . . ?
F17 C12 F16 108.1(3) . . ?
F17 C12 F18 108.2(3) . . ?
F17 C12 C11 109.9(3) . . ?
F18 C12 C11 112.2(3) . . ?
O17 C13 C14 120.6(3) . . ?
O17 C13 C15 120.7(3) . . ?
C15 C13 C14 118.8(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O18 C16 C17 120.8(3) . . ?
O18 C16 C18 120.7(3) . . ?
C18 C16 C17 118.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O19 C19 C20 119.7(7) . . ?
O19 C19 C21 122.3(8) . . ?
C20 C19 C21 118.0(7) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O19' C19' C20' 120.1(8) . . ?
O19' C19' C21' 121.2(8) . . ?
C20' C19' C21' 118.6(7) . . ?
C19' C20' H20D 109.5 . . ?
C19' C20' H20E 109.5 . . ?
C19' C20' H20F 109.5 . . ?
H20D C20' H20E 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C19' C21' H21D 109.5 . . ?
C19' C21' H21E 109.5 . . ?
C19' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
H20G O20 H20H 114.3 . . ?
H20I O20' H20J 104.3 . . ?
O21 C22 C23 121.8(8) . . ?
O21 C22 C24 120.8(7) . . ?
C24 C22 C23 117.3(8) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O21' C22' C23' 121.6(9) . . ?
O21' C22' C24' 120.6(7) . . ?
C23' C22' C24' 117.8(9) . . ?
C22' C23' H23D 109.5 . . ?
C22' C23' H23E 109.5 . . ?
C22' C23' H23F 109.5 . . ?
H23D C23' H23E 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C22' C24' H24D 109.5 . . ?
C22' C24' H24E 109.5 . . ?
C22' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
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 2.048(2) . ?
Ni1 O4 2.046(2) . ?
Ni1 O6 2.0366(18) . ?
Ni1 O13 2.0385(19) . ?
Ni1 O15 2.032(2) . ?
Ni1 O16 1.8844(18) . ?
Ni2 O2 2.066(2) . ?
Ni2 O5 2.048(2) . ?
Ni2 O7 2.0454(18) . ?
Ni2 O8 2.0565(17) . ?
Ni2 O10 2.040(2) . ?
Ni2 O16 1.8856(19) . ?
Ni3 O3 2.0621(19) . ?
Ni3 O9 2.0305(18) . ?
Ni3 O11 2.046(2) . ?
Ni3 O12 2.0542(19) . ?
Ni3 O14 2.0566(18) . ?
Ni3 O16 1.9599(18) . ?
Fe1 O1 2.048(2) . ?
Fe1 O4 2.046(2) . ?
Fe1 O6 2.0366(18) . ?
Fe1 O13 2.0385(19) . ?
Fe1 O15 2.032(2) . ?
Fe1 O16 1.8844(18) . ?
Fe2 O2 2.066(2) . ?
Fe2 O5 2.048(2) . ?
Fe2 O7 2.0454(18) . ?
Fe2 O8 2.0565(17) . ?
Fe2 O10 2.040(2) . ?
Fe2 O16 1.8856(19) . ?
Fe3 O3 2.0621(19) . ?
Fe3 O9 2.0305(18) . ?
Fe3 O11 2.046(2) . ?
Fe3 O12 2.0542(19) . ?
Fe3 O14 2.0566(18) . ?
Fe3 O16 1.9599(18) . ?
F1 C2 1.292(6) . ?
F1' C2' 1.291(6) . ?
F2 C2 1.293(6) . ?
F2' C2' 1.290(7) . ?
F3 C2 1.290(6) . ?
F3' C2' 1.293(6) . ?
F4 C4 1.326(4) . ?
F5 C4 1.324(4) . ?
F6 C4 1.311(4) . ?
F7 C6 1.331(3) . ?
F8 C6 1.325(4) . ?
F9 C6 1.316(3) . ?
F10 C8 1.331(4) . ?
F11 C8 1.327(3) . ?
F12 C8 1.326(3) . ?
F13 C10 1.330(4) . ?
F14 C10 1.328(4) . ?
F15 C10 1.318(4) . ?
F16 C12 1.329(4) . ?
F17 C12 1.310(4) . ?
F18 C12 1.329(4) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8500 . ?
O2 H2A 0.79(5) . ?
O2 H2B 0.83(4) . ?
O3 H3A 0.82(5) . ?
O3 H3B 0.76(4) . ?
O4 C1 1.249(3) . ?
O5 C1 1.242(3) . ?
O6 C3 1.243(3) . ?
O7 C3 1.248(3) . ?
O8 C5 1.247(3) . ?
O9 C5 1.235(3) . ?
O10 C7 1.243(3) . ?
O11 C7 1.242(3) . ?
O12 C9 1.240(3) . ?
O13 C9 1.249(3) . ?
O14 C11 1.233(3) . ?
O15 C11 1.247(3) . ?
C1 C2 1.543(6) . ?
C1 C2' 1.544(7) . ?
C3 C4 1.542(4) . ?
C5 C6 1.545(3) . ?
C7 C8 1.543(4) . ?
C9 C10 1.542(4) . ?
C11 C12 1.543(4) . ?
O17 C13 1.225(4) . ?
C13 C14 1.497(4) . ?
C13 C15 1.490(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O18 C16 1.223(3) . ?
C16 C17 1.492(4) . ?
C16 C18 1.492(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O19 C19 1.216(7) . ?
C19 C20 1.488(7) . ?
C19 C21 1.489(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O19' C19' 1.213(7) . ?
C19' C20' 1.489(7) . ?
C19' C21' 1.491(7) . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
O20 H20G 0.8500 . ?
O20 H20H 0.8501 . ?
O20' H20I 0.8500 . ?
O20' H20J 0.8499 . ?
O21 C22 1.215(7) . ?
C22 C23 1.490(7) . ?
C22 C24 1.486(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O21' C22' 1.208(7) . ?
C22' C23' 1.493(7) . ?
C22' C24' 1.496(7) . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
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
_geom_hbond_publ_flag
O1 H1A O20 0.85 1.87 2.657(4) 153.9 . yes
O1 H1A O20' 0.85 1.84 2.667(6) 165.8 . yes
O1 H1B O21' 0.85 2.03 2.807(6) 150.7 . yes
O2 H2A O17 0.79(5) 1.97(5) 2.750(3) 167(5) . yes
O2 H2B O18 0.83(4) 1.99(4) 2.783(3) 162(4) 1_455 yes
O3 H3A O17 0.82(5) 1.96(5) 2.764(3) 167(4) 1_655 yes
O3 H3B O18 0.76(4) 1.99(4) 2.736(3) 167(4) . yes
O20 H20G O21 0.85 1.90 2.752(8) 179.6 2_666 yes
O20 H20H O19 0.85 1.93 2.767(11) 169.6 . yes
O20' H20I O19' 0.85 1.95 2.751(15) 156.4 . yes
O20' H20J O21' 0.85 2.06 2.895(8) 168.0 2_666 yes
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 O4 C1 O5 6.6(4) . . . . ?
Ni1 O4 C1 C2' -170.3(3) . . . . ?
Ni1 O6 C3 O7 -6.0(5) . . . . ?
Ni1 O6 C3 C4 170.7(2) . . . . ?
Ni1 O13 C9 O12 -10.6(4) . . . . ?
Ni1 O13 C9 C10 167.38(19) . . . . ?
Ni1 O15 C11 O14 14.0(5) . . . . ?
Ni1 O15 C11 C12 -164.7(2) . . . . ?
Ni2 O5 C1 O4 -7.3(4) . . . . ?
Ni2 O5 C1 C2' 169.6(3) . . . . ?
Ni2 O7 C3 O6 4.1(5) . . . . ?
Ni2 O7 C3 C4 -172.6(2) . . . . ?
Ni2 O8 C5 O9 10.0(4) . . . . ?
Ni2 O8 C5 C6 -167.74(17) . . . . ?
Ni2 O10 C7 O11 -3.8(4) . . . . ?
Ni2 O10 C7 C8 174.25(16) . . . . ?
Ni3 O9 C5 O8 -13.2(4) . . . . ?
Ni3 O9 C5 C6 164.55(18) . . . . ?
Ni3 O11 C7 O10 4.8(4) . . . . ?
Ni3 O11 C7 C8 -173.19(16) . . . . ?
Ni3 O12 C9 O13 11.9(4) . . . . ?
Ni3 O12 C9 C10 -166.04(18) . . . . ?
Ni3 O14 C11 O15 -8.6(4) . . . . ?
Ni3 O14 C11 C12 170.08(19) . . . . ?
Fe1 O4 C1 O5 6.6(4) . . . . ?
Fe1 O4 C1 C2 -173.0(3) . . . . ?
Fe1 O6 C3 O7 -6.0(5) . . . . ?
Fe1 O6 C3 C4 170.7(2) . . . . ?
Fe1 O13 C9 O12 -10.6(4) . . . . ?
Fe1 O13 C9 C10 167.38(19) . . . . ?
Fe1 O15 C11 O14 14.0(5) . . . . ?
Fe1 O15 C11 C12 -164.7(2) . . . . ?
Fe2 O5 C1 O4 -7.3(4) . . . . ?
Fe2 O5 C1 C2 172.2(3) . . . . ?
Fe2 O7 C3 O6 4.1(5) . . . . ?
Fe2 O7 C3 C4 -172.6(2) . . . . ?
Fe2 O8 C5 O9 10.0(4) . . . . ?
Fe2 O8 C5 C6 -167.74(17) . . . . ?
Fe2 O10 C7 O11 -3.8(4) . . . . ?
Fe2 O10 C7 C8 174.25(16) . . . . ?
Fe3 O9 C5 O8 -13.2(4) . . . . ?
Fe3 O9 C5 C6 164.55(18) . . . . ?
Fe3 O11 C7 O10 4.8(4) . . . . ?
Fe3 O11 C7 C8 -173.19(16) . . . . ?
Fe3 O12 C9 O13 11.9(4) . . . . ?
Fe3 O12 C9 C10 -166.04(18) . . . . ?
Fe3 O14 C11 O15 -8.6(4) . . . . ?
Fe3 O14 C11 C12 170.08(19) . . . . ?
O4 Ni1 O16 Ni2 -45.78(11) . . . . ?
O4 Ni1 O16 Ni3 134.83(10) . . . . ?
O4 Fe1 O16 Fe2 -45.78(11) . . . . ?
O4 Fe1 O16 Fe3 134.83(10) . . . . ?
O4 C1 C2 F1 -37.0(6) . . . . ?
O4 C1 C2 F2 81.9(7) . . . . ?
O4 C1 C2 F3 -157.5(6) . . . . ?
O4 C1 C2' F1' 147.4(8) . . . . ?
O4 C1 C2' F2' -92.6(9) . . . . ?
O4 C1 C2' F3' 24.9(9) . . . . ?
O5 Ni2 O16 Ni1 45.17(11) . . . . ?
O5 Ni2 O16 Ni3 -135.44(10) . . . . ?
O5 Fe2 O16 Fe1 45.17(11) . . . . ?
O5 Fe2 O16 Fe3 -135.44(10) . . . . ?
O5 C1 C2 F1 143.5(5) . . . . ?
O5 C1 C2 F2 -97.7(6) . . . . ?
O5 C1 C2 F3 22.9(7) . . . . ?
O5 C1 C2' F1' -29.9(9) . . . . ?
O5 C1 C2' F2' 90.1(9) . . . . ?
O5 C1 C2' F3' -152.5(8) . . . . ?
O6 Ni1 O16 Ni2 46.18(11) . . . . ?
O6 Ni1 O16 Ni3 -133.21(10) . . . . ?
O6 Fe1 O16 Fe2 46.18(11) . . . . ?
O6 Fe1 O16 Fe3 -133.21(10) . . . . ?
O6 C3 C4 F4 31.9(4) . . . . ?
O6 C3 C4 F5 -86.1(4) . . . . ?
O6 C3 C4 F6 153.7(3) . . . . ?
O7 Ni2 O16 Ni1 -47.52(12) . . . . ?
O7 Ni2 O16 Ni3 131.87(10) . . . . ?
O7 Fe2 O16 Fe1 -47.52(12) . . . . ?
O7 Fe2 O16 Fe3 131.87(10) . . . . ?
O7 C3 C4 F4 -150.8(3) . . . . ?
O7 C3 C4 F5 91.2(3) . . . . ?
O7 C3 C4 F6 -29.0(4) . . . . ?
O8 Ni2 O16 Ni1 131.16(11) . . . . ?
O8 Ni2 O16 Ni3 -49.45(11) . . . . ?
O8 Fe2 O16 Fe1 131.16(11) . . . . ?
O8 Fe2 O16 Fe3 -49.45(11) . . . . ?
O8 C5 C6 F7 -33.8(3) . . . . ?
O8 C5 C6 F8 85.2(3) . . . . ?
O8 C5 C6 F9 -154.9(2) . . . . ?
O9 C5 C6 F7 148.1(2) . . . . ?
O9 C5 C6 F8 -92.9(3) . . . . ?
O9 C5 C6 F9 27.0(3) . . . . ?
O10 Ni2 O16 Ni1 -134.03(10) . . . . ?
O10 Ni2 O16 Ni3 45.35(10) . . . . ?
O10 Fe2 O16 Fe1 -134.03(10) . . . . ?
O10 Fe2 O16 Fe3 45.35(10) . . . . ?
O10 C7 C8 F10 37.2(3) . . . . ?
O10 C7 C8 F11 -82.0(3) . . . . ?
O10 C7 C8 F12 158.1(2) . . . . ?
O11 C7 C8 F10 -144.5(2) . . . . ?
O11 C7 C8 F11 96.4(3) . . . . ?
O11 C7 C8 F12 -23.6(3) . . . . ?
O12 C9 C10 F13 -27.0(4) . . . . ?
O12 C9 C10 F14 91.1(3) . . . . ?
O12 C9 C10 F15 -148.6(3) . . . . ?
O13 Ni1 O16 Ni2 -132.34(11) . . . . ?
O13 Ni1 O16 Ni3 48.27(11) . . . . ?
O13 Fe1 O16 Fe2 -132.34(11) . . . . ?
O13 Fe1 O16 Fe3 48.27(11) . . . . ?
O13 C9 C10 F13 154.8(2) . . . . ?
O13 C9 C10 F14 -87.1(3) . . . . ?
O13 C9 C10 F15 33.2(4) . . . . ?
O14 C11 C12 F16 30.2(4) . . . . ?
O14 C11 C12 F17 -89.9(3) . . . . ?
O14 C11 C12 F18 149.6(3) . . . . ?
O15 Ni1 O16 Ni2 133.28(11) . . . . ?
O15 Ni1 O16 Ni3 -46.11(11) . . . . ?
O15 Fe1 O16 Fe2 133.28(11) . . . . ?
O15 Fe1 O16 Fe3 -46.11(11) . . . . ?
O15 C11 C12 F16 -150.9(3) . . . . ?
O15 C11 C12 F17 88.9(4) . . . . ?
O15 C11 C12 F18 -31.5(4) . . . . ?
