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_7134709
_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         'C96 H176 Cr7 F8 Ni O32, C6 H12 N'
_chemical_formula_sum            'C102 H188 Cr7 F8 N Ni O32'
_chemical_formula_weight         2515.23
_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   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                90.1198(15)
_cell_angle_beta                 90.1205(15)
_cell_angle_gamma                106.2775(17)
_cell_formula_units_Z            4
_cell_length_a                   19.0912(4)
_cell_length_b                   22.0288(4)
_cell_length_c                   30.5452(5)
_cell_measurement_reflns_used    44090
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.4820
_cell_measurement_theta_min      1.5910
_cell_volume                     12331.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_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_temperature      100.00(10)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
  2  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  3  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 120.00  169
  4  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 240.00  169
;
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0156830000
_diffrn_orient_matrix_UB_12      0.0007155000
_diffrn_orient_matrix_UB_13      0.0202160000
_diffrn_orient_matrix_UB_21      0.0334765000
_diffrn_orient_matrix_UB_22      0.0040052000
_diffrn_orient_matrix_UB_23      0.0098690000
_diffrn_orient_matrix_UB_31      0.0068190000
_diffrn_orient_matrix_UB_32      0.0323237000
_diffrn_orient_matrix_UB_33      -0.0016068000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            164196
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         1.592
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.142a (Rigaku Oxford Diffraction, 2024)
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    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             5324
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.157
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3097
_refine_ls_number_reflns         49932
_refine_ls_number_restraints     17521
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.1397
_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/[\s^2^(Fo^2^)+(0.1497P)^2^+156.0397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3853
_refine_ls_wR_factor_ref         0.4002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33139
_reflns_number_total             49932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01911g2.cif
_cod_data_source_block           m_gt-253-17_2_c1_
_cod_depositor_comments
'Adding full bibliography for 7134703--7134709.cif.'
_cod_database_code               7134709
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.773
_olex2_refinement_description
;
1. Shared sites
{Cr1A, Ni1A}
{Cr2A, Ni2A}
{Cr3A, Ni3A}
{Cr4A, Ni4A}
{Cr5A, Ni5A}
{Cr6A, Ni6A}
{Cr7A, Ni7A}
{Cr8A, Ni8A}
{Cr1B, Ni1B}
{Cr2B, Ni2B}
{Cr3B, Ni3B}
{Cr4B, Ni4B}
{Cr5B, Ni5B}
{Cr6B, Ni6B}
{Cr7B, Ni7B}
{Cr8B, Ni8B}
2. Restrained distances
 C7A-C8A \\sim C7A-C8E
 with sigma of 0.02
 C26A-C25A \\sim C26E-C25A
 with sigma of 0.02
 C35E-C32A \\sim C35A-C32A \\sim C33E-C32A \\sim C33A-C32A
 with sigma of 0.02
 C81A-C80A \\sim C81E-C80A \\sim C83E-C80A \\sim C83A-C80A
 with sigma of 0.02
 C20B-C19B \\sim C20C-C19B
 with sigma of 0.02
 C74C-C73B \\sim C74B-C73B
 with sigma of 0.02
 C92B-C91B \\sim C92C-C91B
 with sigma of 0.02
 C2C-C1C \\sim C1-C2
 with sigma of 0.02
 C3C-C2 \\sim C3C-C1C \\sim C6E-C4E \\sim C6D-C4D
 with sigma of 0.02
 C3C-C2C \\sim C3C-C1
 with sigma of 0.02
 N1D-C4D \\sim N1E-C4E
 with sigma of 0.02
 N1D-C3D \\sim N1E-C3D
 with sigma of 0.02
 C2D-C1D \\sim C2E-C1E
 with sigma of 0.02
 C3D-C2D \\sim C3D-C2E
 with sigma of 0.02
 C5E-C4E \\sim C5D-C4D
 with sigma of 0.02
 C6D-C5D \\sim C6E-C5E
 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(Cr1A) = Uanis(Ni1A)
Uanis(Cr2A) = Uanis(Ni2A)
Uanis(Cr3A) = Uanis(Ni3A)
Uanis(Cr4A) = Uanis(Ni4A)
Uanis(Cr5A) = Uanis(Ni5A)
Uanis(Cr6A) = Uanis(Ni6A)
Uanis(Cr7A) = Uanis(Ni7A)
Uanis(Cr8A) = Uanis(Ni8A)
Uanis(Cr1B) = Uanis(Ni1B)
Uanis(Cr2B) = Uanis(Ni2B)
Uanis(Cr3B) = Uanis(Ni3B)
Uanis(Cr4B) = Uanis(Ni4B)
Uanis(Cr5B) = Uanis(Ni5B)
Uanis(Cr6B) = Uanis(Ni6B)
Uanis(Cr7B) = Uanis(Ni7B)
Uanis(Cr8B) = Uanis(Ni8B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, O4A, C7A, C8A, C9A, C10A, C11A, C12A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, O8A, C19A, C20A, C21A, C22A, C23A, C24A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19A, O20A, C55A, C56A, C57A, C58A, C59A, C60A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, O6A, C13A, C14A, C15A, C16A, C17A, C18A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13A, O14A, C37A, C38A, C39A, C40A, C41A, C42A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, O10A, C25A, C26A, C27A, C28A, C29A, C30A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31A, O32A, C91A, C92A, C93A, C94A, C95A, C96A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, O12A, C31A, C32A, C33A, C34A, C35A, C36A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31B, O32B, C91B, C92B, C93B, C94B, C95B, C96B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15A, O16A, C43A, C44A, C45A, C46A, C47A, C48A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25A, O26A, C73A, C74A, C75A, C76A, C77A, C78A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17A, O18A, C49A, C50A, C51A, C52A, C53A, C54A}
{C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C33E, C34E, C35E, C36E}
{C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C81E, C82E, C83E, C84E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11B, O12B, C31B, C32B, C33B, C34B, C35B, C36B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23A, O24A, C67A, C68A, C69A, C70A, C71A, C72A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5B, O6B, C13B, C14B, C15B, C16B, C17B, C18B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27A, O28A, C79A, C80A, C81A, C82A, C83A, C84A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23B, O24B, C67B, C68B, C69B, C70B, C71B, C72B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29A, O30A, C85A, C86A, C87A, C88A, C89A, C90A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27B, O28B, C79B, C80B, C81B, C82B, C83B, C84B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1B, O2B, C1B, C2B, C3B, C4B, C5B, C6B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17B, O18B, C49B, C50B, C51B, C52B, C53B, C54B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3B, O4B, C7B, C8B, C9B, C10B, C11B, C12B}
{C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C8E, C9E, C10E, C11E, C12E}
{C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C20C, C21C, C22C, C23C, C24C}
{C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C74C, C75C, C76C, C77C, C78C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9B, O10B, C25B, C26B, C27B, C28B, C29B, C30B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29B, O30B, C85B, C86B, C87B, C88B, C89B, C90B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13B, O14B, C37B, C38B, C39B, C40B, C41B, C42B}
{N1D, C1D, C2D, C3D, C4D, C5D, C6D} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N1D, C1D, C2D, C3D, C4D, C5D, C6D}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15B, O16B, C43B, C44B, C45B, C46B, C47B, C48B}
{C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C26E, C27E, C28E, C29E, C30E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19B, O20B, C55B, C56B, C57B, C58B, C59B, C60B}
{C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C92C, C93C, C94C, C95C, C96C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21B, O22B, C61B, C62B, C63B, C64B, C65B, C66B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25B, O26B, C73B, C74B, C75B, C76B, C77B, C78B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7B, O8B, C19B, C20B, C21B, C22B, C23B, C24B}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21A, O22A, C61A, C62A, C63A, C64A, C65A, C66A}
6. Others
 Sof(H32B)=Sof(C33E)=Sof(H33C)=Sof(H33D)=Sof(C34E)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C35E)=Sof(H35C)=Sof(H35D)=Sof(C36E)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(1)
 Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
 Sof(C26E)=Sof(H26E)=Sof(C27E)=Sof(H27C)=Sof(H27D)=Sof(C28E)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C29E)=Sof(H29C)=Sof(H29D)=Sof(C30E)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=FVAR(2)
 Sof(C8E)=Sof(H8E)=Sof(C9E)=Sof(H9EA)=Sof(H9EB)=Sof(C10E)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11E)=Sof(H11C)=Sof(H11D)=Sof(C12E)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=1-FVAR(3)
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=FVAR(3)
 Sof(C92C)=Sof(H92C)=Sof(C93C)=Sof(H93E)=Sof(H93F)=Sof(C94C)=Sof(H94G)=
 Sof(H94H)=Sof(H94I)=Sof(C95C)=Sof(H95E)=Sof(H95F)=Sof(C96C)=Sof(H96G)=
 Sof(H96H)=Sof(H96I)=1-FVAR(4)
 Sof(C92B)=Sof(H92B)=Sof(C93B)=Sof(H93C)=Sof(H93D)=Sof(C94B)=Sof(H94D)=
 Sof(H94E)=Sof(H94F)=Sof(C95B)=Sof(H95C)=Sof(H95D)=Sof(C96B)=Sof(H96D)=
 Sof(H96E)=Sof(H96F)=FVAR(4)
 Sof(C74C)=Sof(H74C)=Sof(C75C)=Sof(H75E)=Sof(H75F)=Sof(C76C)=Sof(H76G)=
 Sof(H76H)=Sof(H76I)=Sof(C77C)=Sof(H77E)=Sof(H77F)=Sof(C78C)=Sof(H78G)=
 Sof(H78H)=Sof(H78I)=1-FVAR(5)
 Sof(C74B)=Sof(H74B)=Sof(C75B)=Sof(H75C)=Sof(H75D)=Sof(C76B)=Sof(H76D)=
 Sof(H76E)=Sof(H76F)=Sof(C77B)=Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78D)=
 Sof(H78E)=Sof(H78F)=FVAR(5)
 Sof(C20C)=Sof(H20C)=Sof(C21C)=Sof(H21E)=Sof(H21F)=Sof(C22C)=Sof(H22G)=
 Sof(H22H)=Sof(H22I)=Sof(C23C)=Sof(H23E)=Sof(H23F)=Sof(C24C)=Sof(H24G)=
 Sof(H24H)=Sof(H24I)=1-FVAR(6)
 Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=FVAR(6)
 Sof(H3CC)=Sof(H3CD)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2F)=Sof(H2G)=1-FVAR(7)
 Sof(C1C)=Sof(H1CC)=Sof(H1CD)=Sof(C2C)=Sof(H2C)=Sof(H3CA)=Sof(H3CB)=FVAR(7)
 Sof(H3DC)=Sof(H3DD)=Sof(C5E)=Sof(H5E)=Sof(C6E)=Sof(H6EA)=Sof(H6EB)=Sof(C4E)=
 Sof(H4EA)=Sof(H4EB)=Sof(N1E)=Sof(H1EA)=Sof(H1EB)=Sof(C2E)=Sof(H2E)=Sof(C1E)=
 Sof(H1EC)=Sof(H1ED)=1-FVAR(8)
 Sof(N1D)=Sof(H1DA)=Sof(H1DB)=Sof(C1D)=Sof(H1DC)=Sof(H1DD)=Sof(C2D)=Sof(H2D)=
 Sof(H3DA)=Sof(H3DB)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(C5D)=Sof(H5D)=Sof(C6D)=
 Sof(H6DA)=Sof(H6DB)=FVAR(8)
 Sof(H80B)=Sof(C81E)=Sof(H81C)=Sof(H81D)=Sof(C82E)=Sof(H82D)=Sof(H82E)=
 Sof(H82F)=Sof(C83E)=Sof(H83C)=Sof(H83D)=Sof(C84E)=Sof(H84D)=Sof(H84E)=
 Sof(H84F)=1-FVAR(9)
 Sof(H80A)=Sof(C81A)=Sof(H81A)=Sof(H81B)=Sof(C82A)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=Sof(C83A)=Sof(H83A)=Sof(H83B)=Sof(C84A)=Sof(H84A)=Sof(H84B)=
 Sof(H84C)=FVAR(9)
 Fixed Sof: Cr1A(0.875) Cr2A(0.875) Cr3A(0.875) Cr4A(0.875) Cr5A(0.875)
 Cr6A(0.875) Cr7A(0.875) Cr8A(0.875) Cr1B(0.875) Cr2B(0.875) Cr3B(0.875)
 Cr4B(0.875) Cr5B(0.875) Cr6B(0.875) Cr7B(0.875) Cr8B(0.875) Ni1A(0.125)
 Ni2A(0.125) Ni3A(0.125) Ni4A(0.125) Ni5A(0.125) Ni6A(0.125) Ni7A(0.125)
 Ni8A(0.125) Ni1B(0.125) Ni2B(0.125) Ni3B(0.125) Ni4B(0.125) Ni5B(0.125)
 Ni6B(0.125) Ni7B(0.125) Ni8B(0.125)
7.a Ternary CH refined with riding coordinates:
 C2A(H2A), C8A(H8A), C14A(H14A), C20A(H20A), C26A(H26A), C32A(H32A),
 C32A(H32B), C38A(H38A), C44A(H44A), C50A(H50A), C56A(H56A), C62A(H62A),
 C68A(H68A), C74A(H74A), C80A(H80A), C80A(H80B), C86A(H86A), C92A(H92A),
 C2B(H2B), C8B(H8B), C14B(H14B), C20B(H20B), C26B(H26B), C32B(H32C), C38B(H38B),
  C44B(H44B), C50B(H50B), C56B(H56B), C62B(H62B), C68B(H68B), C74B(H74B),
 C80B(H80C), C86B(H86B), C92B(H92B), C26E(H26E), C8E(H8E), C92C(H92C),
 C74C(H74C), C20C(H20C)
7.b Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C5A(H5AA,H5AB), C9A(H9AA,H9AB), C11A(H11A,H11B), C15A(H15A,
 H15B), C17A(H17A,H17B), C21A(H21A,H21B), C23A(H23A,H23B), C27A(H27A,H27B),
 C29A(H29A,H29B), C33A(H33A,H33B), C35A(H35A,H35B), C39A(H39A,H39B), C41A(H41A,
 H41B), C45A(H45A,H45B), C47A(H47A,H47B), C51A(H51A,H51B), C53A(H53A,H53B),
 C57A(H57A,H57B), C59A(H59A,H59B), C63A(H63A,H63B), C65A(H65A,H65B), C69A(H69A,
 H69B), C71A(H71A,H71B), C75A(H75A,H75B), C77A(H77A,H77B), C81A(H81A,H81B),
 C83A(H83A,H83B), C87A(H87A,H87B), C89A(H89A,H89B), C93A(H93A,H93B), C95A(H95A,
 H95B), C3B(H3BA,H3BB), C5B(H5BA,H5BB), C9B(H9BA,H9BB), C11B(H11E,H11F),
 C15B(H15C,H15D), C17B(H17C,H17D), C21B(H21C,H21D), C23B(H23C,H23D), C27B(H27E,
 H27F), C29B(H29E,H29F), C33B(H33E,H33F), C35B(H35E,H35F), C39B(H39C,H39D),
 C41B(H41C,H41D), C45B(H45C,H45D), C47B(H47C,H47D), C51B(H51C,H51D), C53B(H53C,
 H53D), C57B(H57C,H57D), C59B(H59C,H59D), C63B(H63C,H63D), C65B(H65C,H65D),
 C69B(H69C,H69D), C71B(H71C,H71D), C75B(H75C,H75D), C77B(H77C,H77D), C81B(H81E,
 H81F), C83B(H83E,H83F), C87B(H87C,H87D), C89B(H89C,H89D), C93B(H93C,H93D),
 C95B(H95C,H95D), N1C(H1CA,H1CB), C3C(H3CA,H3CB), C3C(H3CC,H3CD), C4C(H4CA,
 H4CB), N1D(H1DA,H1DB), C3D(H3DA,H3DB), C3D(H3DC,H3DD), C4D(H4DA,H4DB),
 C33E(H33C,H33D), C35E(H35C,H35D), C27E(H27C,H27D), C29E(H29C,H29D), C9E(H9EA,
 H9EB), C11E(H11C,H11D), C93C(H93E,H93F), C95C(H95E,H95F), C75C(H75E,H75F),
 C77C(H77E,H77F), C21C(H21E,H21F), C23C(H23E,H23F), C4E(H4EA,H4EB), N1E(H1EA,
 H1EB), C81E(H81C,H81D), C83E(H83C,H83D)
7.c Me refined with riding coordinates:
 C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC), C10A(H10A,H10B,H10C), C12A(H12A,
 H12B,H12C), C16A(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C22A(H22A,H22B,H22C),
 C24A(H24A,H24B,H24C), C28A(H28A,H28B,H28C), C30A(H30A,H30B,H30C), C34A(H34A,
 H34B,H34C), C36A(H36A,H36B,H36C), C40A(H40A,H40B,H40C), C42A(H42A,H42B,H42C),
 C46A(H46A,H46B,H46C), C48A(H48A,H48B,H48C), C52A(H52A,H52B,H52C), C54A(H54A,
 H54B,H54C), C58A(H58A,H58B,H58C), C60A(H60A,H60B,H60C), C64A(H64A,H64B,H64C),
 C66A(H66A,H66B,H66C), C70A(H70A,H70B,H70C), C72A(H72A,H72B,H72C), C76A(H76A,
 H76B,H76C), C78A(H78A,H78B,H78C), C82A(H82A,H82B,H82C), C84A(H84A,H84B,H84C),
 C88A(H88A,H88B,H88C), C90A(H90A,H90B,H90C), C94A(H94A,H94B,H94C), C96A(H96A,
 H96B,H96C), C4B(H4BA,H4BB,H4BC), C6B(H6BA,H6BB,H6BC), C10B(H10G,H10H,H10I),
 C12B(H12G,H12H,H12I), C16B(H16D,H16E,H16F), C18B(H18D,H18E,H18F), C22B(H22D,
 H22E,H22F), C24B(H24D,H24E,H24F), C28B(H28G,H28H,H28I), C30B(H30G,H30H,H30I),
 C34B(H34G,H34H,H34I), C36B(H36G,H36H,H36I), C40B(H40D,H40E,H40F), C42B(H42D,
 H42E,H42F), C46B(H46D,H46E,H46F), C48B(H48D,H48E,H48F), C52B(H52D,H52E,H52F),
 C54B(H54D,H54E,H54F), C58B(H58D,H58E,H58F), C60B(H60D,H60E,H60F), C64B(H64D,
 H64E,H64F), C66B(H66D,H66E,H66F), C70B(H70D,H70E,H70F), C72B(H72D,H72E,H72F),
 C76B(H76D,H76E,H76F), C78B(H78D,H78E,H78F), C82B(H82G,H82H,H82I), C84B(H84G,
 H84H,H84I), C88B(H88D,H88E,H88F), C90B(H90D,H90E,H90F), C94B(H94D,H94E,H94F),
 C96B(H96D,H96E,H96F), C34E(H34D,H34E,H34F), C36E(H36D,H36E,H36F), C28E(H28D,
 H28E,H28F), C30E(H30D,H30E,H30F), C10E(H10D,H10E,H10F), C12E(H12D,H12E,H12F),
 C94C(H94G,H94H,H94I), C96C(H96G,H96H,H96I), C76C(H76G,H76H,H76I), C78C(H78G,
 H78H,H78I), C22C(H22G,H22H,H22I), C24C(H24G,H24H,H24I), C82E(H82D,H82E,H82F),
 C84E(H84D,H84E,H84F)
7.d Aromatic/amide H refined with riding coordinates:
 C2C(H2C), C5C(H5C), C2D(H2D), C5D(H5D), C1(H1), C5E(H5E), C2E(H2E)
7.e X=CH2 refined with riding coordinates:
 C1C(H1CC,H1CD), C6C(H6CA,H6CB), C1D(H1DC,H1DD), C6D(H6DA,H6DB), C2(H2F,H2G),
 C6E(H6EA,H6EB), C1E(H1EC,H1ED)
;
_shelx_res_checksum              69632
_shelx_hkl_checksum              79488
_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 1.605
_oxdiff_exptl_absorpt_empirical_full_min 0.586