Energetics of carboxylate-metal bonds in polymetallic rings.
Geue, Niklas; Renningholtz, Tim; Whitehead, George F. S.; Timco, Grigore A.; Trujillo, Cristina; Barran, Perdita E.; Winpenny, Richard E. P.; Chemical communications (Cambridge, England) 61 (2025) 11049–11052; doi:10.1039/d5cc01911g

data_7134708
_publ_section_title
;
 Energetics of carboxylate-metal bonds in polymetallic rings.
;
_journal_issue                   59
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11049
_journal_page_last               11052
_journal_paper_doi               10.1039/d5cc01911g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C80 H144 Cr7 F8 Ni O32, 1(C6 H12 N)'
_chemical_formula_sum            'C86 H160 Cr7 F8 N Ni O32'
_chemical_formula_weight         2294.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-17
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-17 deposited with the CCDC.	2025-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.138(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1697(5)
_cell_length_b                   29.3283(8)
_cell_length_c                   20.8382(7)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      51.0250
_cell_measurement_theta_min      2.3800
_cell_volume                     11360.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    130.00 171.00   1.00    5.00    --   82.70  43.00 -44.00   41
  2  \w     -6.00 103.00   1.00    5.00    --   82.70  43.00 -44.00  109
  3  \w    -74.00  72.00   1.00    1.00    --    0.00  30.00-180.00  146
  4  \w    -24.00   1.00   1.00    1.00    --    0.00  43.00 -44.00   25
  5  \w     -7.00 141.00   1.00    5.00    --   82.70  30.00-120.00  148
  6  \w     70.00  95.00   1.00    5.00    --   82.70  40.00  60.00   25
  7  \w     75.00 105.00   1.00    5.00    --   82.70  50.00  60.00   30
  8  \w     11.00  40.00   1.00    5.00    --   82.70  50.00  60.00   29
  9  \w     -7.00  25.00   1.00    5.00    --   82.70  40.00  60.00   32
 10  \w     -3.00 166.00   1.00    5.00    --   82.70  40.00-150.00  169
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0253208000
_diffrn_orient_matrix_UB_12      0.0253428000
_diffrn_orient_matrix_UB_13      -0.0550588000
_diffrn_orient_matrix_UB_21      -0.0722012000
_diffrn_orient_matrix_UB_22      0.0256934000
_diffrn_orient_matrix_UB_23      -0.0189207000
_diffrn_orient_matrix_UB_31      0.0317085000
_diffrn_orient_matrix_UB_32      0.0381816000
_diffrn_orient_matrix_UB_33      0.0492310000
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54250
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        64.072
_diffrn_reflns_theta_max         64.072
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             4828
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1786
_refine_ls_number_reflns         18420
_refine_ls_number_restraints     7908
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2708
_refine_ls_wR_factor_ref         0.3357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8441
_reflns_number_total             18420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01911g2.cif
_cod_data_source_block           lrepw483
_cod_depositor_comments
'Adding full bibliography for 7134703--7134709.cif.'
_cod_database_code               7134708
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.555
_olex2_refinement_description
;
1. Shared sites
{Cr1, Ni1}
{Cr2, Ni2}
{Cr3, Ni3}
{Cr4, Ni4}
{Cr5, Ni5}
{Cr6, Ni6}
{Cr7, Ni7}
{Cr8, Ni8}
2. Restrained distances
 C3-C2 = C4-C3 = C5-C2
 1.5 with sigma of 0.02
 C29-C28 = C28-C27 = C30-C27 = C24-C23 = C23-C22 = C25A-C22A = C25-C22 = C24A-
 C23A = C23A-C22A = C19-C18 = C20A-C17A = C20-C17 = C18A-C17A = C18-C17 = C19A-
 C18A = C14-C13 = C13-C12 = C15A-C12A = C15-C12 = C13A-C12A = C14A-C13A = C5-C2
 = C3A-C2A = C4A-C3A = C5A-C2A = C4-C3 = C3-C2 = C80-C77 = C79A-C78A = C78A-
 C77A = C78-C77 = C80A-C77A = C79-C78 = C74-C73 = C73-C72 = C75A-C72A = C75-C72
 = C73A-C72A = C74A-C73A = C9-C8 = C7A-C10A = C8-C7 = C7-C10 = C8A-C7A = C9A-
 C8A = C70-C67 = C70A-C67A = C68-C67 = C68A-C67A = C69A-C68A = C69-C68 = C65A-
 C62A = C63-C62 = C64-C63 = C63A-C62A = C65-C62 = C64A-C63A = C59A-C58A = C60-
 C57 = C58A-C57A = C58-C57 = C60A-C57A = C59-C58 = C55A-C52A = C53A-C52A = C54A-
 C53A = C54-C53 = C53-C52 = C55-C52 = C43A-C42A = C45-C42 = C44A-C43A = C45A-
 C42A = C43-C42 = C44-C43 = C39A-C38A = C39-C38 = C38A-C37A = C38-C37 = C40A-
 C37A = C40-C37 = C34-C33 = C35A-C32A = C33-C32 = C33A-C32A = C34A-C33A = C35-
 C32 = C50-C47 = C48-C47 = C49-C48
 1.5 with sigma of 0.02
 C83A-C82A = C83A-N1A
 1.45 with sigma of 0.02
 C57-C56 \\sim C57A-C56 \\sim C52-C51 \\sim C52A-C51 \\sim C62-C61 \\sim
C62A-C61 \\sim C42-C41 \\sim C42A-
 C41 \\sim C32A-C31 \\sim C32-C31 \\sim C47-C46 \\sim C27-C26 \\sim C22-C21
\\sim C22A-C21 \\sim C12-C11 ~
 C12A-C11 \\sim C17-C16 \\sim C17A-C16 \\sim C2-C1 \\sim C2A-C1 \\sim C7-C6
\\sim C7A-C6 \\sim C72-C71 ~
 C72A-C71 \\sim C67-C66 \\sim C67A-C66 \\sim C37A-C36 \\sim C37-C36 \\sim
C77A-C76 \\sim C77-C76
 with sigma of 0.02
 C37A-C36 \\sim C37-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(Cr1) = Uanis(Ni1)
Uanis(Cr2) = Uanis(Ni2)
Uanis(Cr3) = Uanis(Ni3)
Uanis(Cr4) = Uanis(Ni4)
Uanis(Cr5) = Uanis(Ni5)
Uanis(Cr6) = Uanis(Ni6)
Uanis(Cr7) = Uanis(Ni7)
Uanis(Cr8) = Uanis(Ni8)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C42A, C43A, C44A, C45A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19, O20, C46, C47, C48, C49, C50}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23, O24, C56, C57, C58, C59, C60}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, O6, C11, C12, C13, C14, C15}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C2A, C3A, C4A, C5A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, O10, C21, C22, C23, C24, C25}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C37A, C38A, C39A, C40A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21, O22, C51, C52, C53, C54, C55}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C72A, C73A, C74A, C75A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C52A, C53A, C54A, C55A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, O12, C26, C27, C28, C29, C30}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C22A, C23A, C24A, C25A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31, O32, C76, C77, C78, C79, C80}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C12A, C13A, C14A, C15A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29, O30, C71, C72, C73, C74, C75}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C57A, C58A, C59A, C60A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, O8, C16, C17, C18, C19, C20}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25, O26, C61, C62, C63, C64, C65}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C77A, C78A, C79A, C80A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C7A, C8A, C9A, C10A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, O4, C6, C7, C8, C9, C10}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13, O14, C31, C32, C33, C34, C35}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15, O16, C36, C37, C38, C39, C40}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27, O28, C66, C67, C68, C69, C70}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C17A, C18A, C19A, C20A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C67A, C68A, C69A, C70A}
{O1, O2, C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17, O18, C41, C42, C43, C44, C45}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C32A, C33A, C34A, C35A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C62A, C63A, C64A, C65A}
6. Others
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23C)=
 Sof(H23D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=
 Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C69A)=Sof(H69D)=
 Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C72A)=
 Sof(H72A)=Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74D)=Sof(H74E)=
 Sof(H74F)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C77A)=Sof(H77A)=
 Sof(C78A)=Sof(H78C)=Sof(H78D)=Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=
 Sof(C80A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(C81)=
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C37A)=
 Sof(H37A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C32)=Sof(H32)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C67)=Sof(H67)=Sof(C68)=
 Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70A)=
 Sof(H70B)=Sof(H70C)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=
 Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=
 Sof(H82A)=Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(C84A)=
 Sof(H84C)=Sof(H84D)=Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86C)=Sof(H86D)=FVAR(1)
 Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C57A)=
 Sof(H57A)=Sof(C58A)=Sof(H58C)=Sof(H58D)=Sof(C59A)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C62A)=Sof(H62A)=
 Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=
 Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=1-FVAR(2)
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C57)=Sof(H57)=Sof(C58)=
 Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=FVAR(2)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=1-FVAR(3)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=FVAR(3)
 Fixed Sof: Cr1(0.875) Cr2(0.875) Cr3(0.875) Cr4(0.875) Cr5(0.875) Cr6(0.875)
 Cr7(0.875) Cr8(0.875) Ni1(0.125) Ni2(0.125) Ni3(0.125) Ni4(0.125) Ni5(0.125)
 Ni6(0.125) Ni7(0.125) Ni8(0.125)
7.a Ternary CH refined with riding coordinates:
 C2(H2), C2A(H2A), C7(H7), C7A(H7A), C12(H12), C12A(H12A), C17(H17),
 C17A(H17A), C22(H22), C22A(H22A), C27(H27), C32(H32), C32A(H32A), C37(H37),
 C42(H42), C42A(H42A), C47(H47), C52(H52), C52A(H52A), C57(H57), C57A(H57A),
 C62(H62), C62A(H62A), C67(H67), C67A(H67A), C72(H72), C72A(H72A), C77(H77),
 C77A(H77A), C37A(H37A)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C3A(H3AA,H3AB), C8(H8A,H8B), C8A(H8AA,H8AB), C13(H13A,H13B),
 C13A(H13C,H13D), C18(H18A,H18B), C18A(H18C,H18D), C23(H23A,H23B), C23A(H23C,
 H23D), C28(H28A,H28B), C33(H33A,H33B), C33A(H33C,H33D), C38(H38A,H38B),
 C43(H43A,H43B), C43A(H43C,H43D), C48(H48A,H48B), C53(H53A,H53B), C53A(H53C,
 H53D), C58(H58A,H58B), C58A(H58C,H58D), C63(H63A,H63B), C63A(H63C,H63D),
 C68(H68A,H68B), C68A(H68C,H68D), C73(H73A,H73B), C73A(H73C,H73D), C78(H78A,
 H78B), C78A(H78C,H78D), N1(H1A,H1B), C83(H83A,H83B), C84(H84A,H84B), C83A(H83C,
 H83D), N1A(H1AA,H1AB), C84A(H84C,H84D), C38A(H38C,H38D)
7.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,
 H10F), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F),
 C15A(H15D,H15E,H15F), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C19A(H19D,H19E,
 H19F), C20A(H20D,H20E,H20F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C34A(H34D,H34E,H34F),
 C35A(H35D,H35E,H35F), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C64A(H64D,H64E,H64F), C65A(H65D,H65E,H65F),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C69A(H69D,H69E,H69F), C70A(H70D,H70E,
 H70F), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C74A(H74D,H74E,H74F),
 C75A(H75D,H75E,H75F), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C79A(H79D,H79E,
 H79F), C80A(H80D,H80E,H80F), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F)
7.d Aromatic/amide H refined with riding coordinates:
 C82(H82), C85(H85), C82A(H82A), C85A(H85A)
7.e X=CH2 refined with riding coordinates:
 C81(H81A,H81B), C86(H86A,H86B), C81A(H81C,H81D), C86A(H86C,H86D)
;
_shelx_res_checksum              84565
_shelx_hkl_checksum              20169
_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 3.326
_oxdiff_exptl_absorpt_empirical_full_min 0.689