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_7134703
_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_absolute_configuration ad
_chemical_formula_moiety
'C3 H10 N, 1.977(C48.559 H89.024 Cr3.541 F4.047 Ni0.506 O16.186), 1.245(H2 O1), C2 H3 N'
_chemical_formula_sum            'C101 H191.49 Cr7 F8 N2 Ni O33.24'
_chemical_formula_weight         2540.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4235(2)
_cell_length_b                   21.7382(2)
_cell_length_c                   31.1018(3)
_cell_measurement_reflns_used    44559
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.7480
_cell_measurement_theta_min      2.4670
_cell_volume                     13132.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.134a 64-bit (release 09-08-2024))'
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.990
_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     94.00 144.00   0.50    0.88    --  107.75  13.00 -33.00  100
  2  \w     96.00 145.00   0.50    0.88    --  107.75  45.00  30.00   98
  3  \w    107.00 174.00   0.50    0.88    --  107.75  30.00-120.00  134
  4  \w     58.00  84.00   0.50    0.22    --   46.69  13.00 -33.00   52
  5  \w     36.00 100.00   0.50    0.88    --  107.75 -95.00 120.00  128
  6  \w    -27.00  -2.00   0.50    0.22    --   46.69 -13.00 155.00   50
  7  \w     58.00  93.00   0.50    0.88    --  107.75 -95.00  30.00   70
  8  \w    -23.00  43.00   0.50    0.22    --   46.69 -38.00  30.00  132
  9  \w   -116.00 -90.00   0.50    0.22    --  -46.69 -38.00 -90.00   52
 10  \w    -79.00 -35.00   0.50    0.22    --  -46.69 -38.00 -90.00   88
 11  \w   -118.00 -93.00   0.50    0.88    -- -109.00 -61.00 -90.00   50
 12  \w   -128.00-102.00   0.50    0.88    -- -109.00 -30.00-180.00   52
 13  \w   -174.00-149.00   0.50    0.88    -- -109.00 -61.00 -90.00   50
 14  \w   -135.00-101.00   0.50    0.88    -- -109.00 -30.00 -60.00   68
 15  \w   -113.00 -32.00   0.50    0.22    --  -46.69 -13.00 155.00  162
 16  \w   -167.00 -94.00   0.50    0.88    -- -109.00 -13.00 155.00  146
 17  \w    -93.00 -38.00   0.50    0.88    -- -109.00  77.00 150.00  110
 18  \w    -65.00 -40.00   0.50    0.88    -- -109.00  61.00  90.00   50
 19  \w    -71.00 -40.00   0.50    0.88    -- -109.00  61.00  30.00   62
 20  \w    -68.00 -37.00   0.50    0.88    -- -109.00  61.00 -60.00   62
 21  \w    -63.00 -38.00   0.50    0.88    -- -109.00  61.00 -90.00   50
 22  \w    -70.00 -45.00   0.50    0.88    -- -109.00  61.00-120.00   50
 23  \w    -68.00 -36.00   0.50    0.88    -- -109.00  77.00-180.00   64
 24  \w    -67.00 -36.00   0.50    0.88    -- -109.00  61.00-180.00   62
 25  \w   -106.00 -78.00   0.50    0.88    -- -109.00  77.00-180.00   56
 26  \w    -18.00   7.00   0.50    0.22    --  -46.69  13.00 -33.00   50
 27  \w    -69.00 -44.00   0.50    0.88    -- -109.00  61.00 -30.00   50
 28  \w    -71.00 -44.00   0.50    0.88    -- -109.00  61.00  60.00   54
 29  \w    -66.00 -36.00   0.50    0.88    -- -109.00  61.00 150.00   60
 30  \w   -119.00 -52.00   0.50    0.88    -- -109.00 135.00  27.05  134
 31  \w   -112.00 -82.00   0.50    0.88    -- -109.00 125.00  30.00   60
 32  \w   -108.00 -56.00   0.50    0.88    -- -109.00 109.00  18.84  104
 33  \w    -89.00 -23.00   0.50    0.22    --  -46.69 125.00-120.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0693635000
_diffrn_orient_matrix_UB_12      0.0062814000
_diffrn_orient_matrix_UB_13      0.0235961000
_diffrn_orient_matrix_UB_21      0.0364812000
_diffrn_orient_matrix_UB_22      0.0110022000
_diffrn_orient_matrix_UB_23      -0.0432963000
_diffrn_orient_matrix_UB_31      -0.0120595000
_diffrn_orient_matrix_UB_32      0.0697489000
_diffrn_orient_matrix_UB_33      0.0046926000
_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  0.0602
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            114583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.887
_diffrn_reflns_theta_min         2.480
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03106
_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    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             5382
_exptl_crystal_size_max          0.687
_exptl_crystal_size_mid          0.525
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 9276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2734
_refine_ls_number_reflns         27486
_refine_ls_number_restraints     17182
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+2.6486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                23857
_reflns_number_total             27486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01911g2.cif
_cod_data_source_block           s6639r
_cod_depositor_comments
'Adding full bibliography for 7134703--7134709.cif.'
_cod_database_code               7134703
_shelx_shelxl_version_number     2019/3
_diffrn_oxdiff_ac3_digest_hkl    411e07dfc35fb2f4876d8c5d45ec3bc03ade0b
_diffrn_oxdiff_digest_hkl
;
4335d36467fd29a71c308bf104abd8fa6f8ea3
;
_olex2_refinement_description
;
1. Shared sites
{Cr1, Ni1}
{Cr2, Ni2}
{Cr3, Ni3}
{Cr4, Ni4}
{Cr5, Ni5}
{Cr6, Ni6}
{Cr7, Ni7}
{Cr8, Ni8}
{Cr1A, Ni1A}
{Cr2A, Ni2A}
{Cr3A, Ni3A}
{Cr4A, Ni4A}
{Cr5A, Ni5A}
{Cr6A, Ni6A}
{Cr7A, Ni7A}
{Cr8A, Ni8A}
2. Restrained distances
 C102-C100
 1.446 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 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)
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)
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
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, O4, C7, C8, C9, C10, C11, C12}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19, O20, C55, C56, C57, C58, C59, C60}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, O8, C19, C20, C21, C22, C23, C24}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, O4A, C7A, C8A, C9A, C10A, C11A, C12A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, O8A, C19A, C20A, C21A, C22A, C23A, C24A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, O6A, C13A, C14A, C15A, C16A, C17A, C18A}
{N1, C97, C98, C99} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N1A, C97A, C98A, C99A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, O12, C31, C32, C33, C34, C35, C36}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17, O18, C49, C50, C51, C52, C53, C54}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21, O22, C61, C62, C63, C64, C65, C66}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13A, O14A, C37A, C38A, C39A, C40A, C41A, C42A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, O10A, C25A, C26A, C27A, C28A, C29A, C30A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29, O30, C85, C86, C87, C88, C89, C90}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, O12A, C31A, C32A, C33A, C34A, C35A, C36A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27, O28, C79, C80, C81, C82, C83, C84}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23, O24, C67, C68, C69, C70, C71, C72}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19A, O20A, C55A, C56A, C57A, C58A, C59A, C60A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13, O14, C37, C38, C39, C40, C41, C42}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, O10, C25, C26, C27, C28, C29, C30}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15A, O16A, C43A, C44A, C45A, C46A, C47A, C48A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31, O32, C91, C92, C93, C94, C95, C96}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1A, O2A, C1A, C2A, C3A, C4A, C5A, C6A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25A, O26A, C73A, C74A, C75A, C76A, C77A, C78A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25, O26, C73, C74, C75, C76, C77, C78}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27A, O28A, C79A, C80A, C81A, C82A, C83A, C84A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, O6, C13, C14, C15, C16, C17, C18}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29A, O30A, C85A, C86A, C87A, C88A, C89A, C90A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21A, O22A, C61A, C62A, C63A, C64A, C65A, C66A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31A, O32A, C91A, C92A, C93A, C94A, C95A, C96A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23A, O24A, C67A, C68A, C69A, C70A, C71A, C72A}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15, O16, C43, C44, C45, C46, C47, C48}
{O1, O2, C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17A, O18A, C49A, C50A, C51A, C52A, C53A, C54A}
6. Others
 1*[Sof(O35)+Sof(H35G)+Sof(H35H)]+1*[Sof(O33)+Sof(H33A)+Sof(H33B)]+1*[Sof(O34)+
 Sof(H34G)+Sof(H34H)]=1 with esd of 0
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=
 Sof(O1A)=Sof(O2A)=Sof(C1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(O3A)=Sof(O4A)=Sof(C7A)=Sof(C8A)=Sof(H8AA)=
 Sof(H8AB)=Sof(C9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(O5A)=Sof(O6A)=
 Sof(C13A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O7A)=Sof(O8A)=Sof(C19A)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=Sof(C21A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(O9A)=
 Sof(O10A)=Sof(C25A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(O11A)=Sof(O12A)=Sof(C31A)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=Sof(O13A)=Sof(O14A)=Sof(C37A)=Sof(C38A)=Sof(H38C)=
 Sof(H38D)=Sof(C39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=
 Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=
 Sof(O15A)=Sof(O16A)=Sof(C43A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(O17A)=Sof(O18A)=
 Sof(C49A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=
 Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(O19A)=Sof(O20A)=Sof(C55A)=Sof(C56A)=
 Sof(H56C)=Sof(H56D)=Sof(C57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=
 Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=
 Sof(H60F)=Sof(O21A)=Sof(O22A)=Sof(C61A)=Sof(C62A)=Sof(H62C)=Sof(H62D)=
 Sof(C63A)=Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C65A)=Sof(H65D)=
 Sof(H65E)=Sof(H65F)=Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(O23A)=
 Sof(O24A)=Sof(C67A)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C69A)=Sof(C70A)=
 Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=
 Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(O25A)=Sof(O26A)=Sof(C73A)=
 Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(C76A)=Sof(H76D)=Sof(H76E)=
 Sof(H76F)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78A)=Sof(H78D)=
 Sof(H78E)=Sof(H78F)=Sof(O27A)=Sof(O28A)=Sof(C79A)=Sof(C80A)=Sof(H80C)=
 Sof(H80D)=Sof(C81A)=Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C83A)=
 Sof(H83D)=Sof(H83E)=Sof(H83F)=Sof(C84A)=Sof(H84D)=Sof(H84E)=Sof(H84F)=
 Sof(O29A)=Sof(O30A)=Sof(C85A)=Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(C87A)=
 Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C89A)=Sof(H89D)=Sof(H89E)=
 Sof(H89F)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=Sof(O31A)=Sof(O32A)=
 Sof(C91A)=Sof(C92A)=Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(C94A)=Sof(H94D)=
 Sof(H94E)=Sof(H94F)=Sof(C95A)=Sof(H95D)=Sof(H95E)=Sof(H95F)=Sof(C96A)=
 Sof(H96D)=Sof(H96E)=Sof(H96F)=1-FVAR(1)
 Sof(Cr1A)=Sof(Cr2A)=Sof(Cr3A)=Sof(Cr4A)=Sof(Cr5A)=Sof(Cr6A)=Sof(Cr7A)=
 Sof(Cr8A)=0.875*(1-FVAR(2))
 Sof(Ni1A)=Sof(Ni2A)=Sof(Ni3A)=Sof(Ni4A)=Sof(Ni5A)=Sof(Ni6A)=Sof(Ni7A)=
 Sof(Ni8A)=0.125*(1-FVAR(2))
 Sof(Ni1)=Sof(Ni2)=Sof(Ni3)=Sof(Ni4)=Sof(Ni5)=Sof(Ni6)=Sof(Ni7)=Sof(Ni8)=0.125*
 FVAR(2)
 Sof(Cr1)=Sof(Cr2)=Sof(Cr3)=Sof(Cr4)=Sof(Cr5)=Sof(Cr6)=Sof(Cr7)=Sof(Cr8)=0.875*
 FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(O1)=
 Sof(O2)=Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(O3)=Sof(O4)=Sof(C7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(O5)=Sof(O6)=Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O7)=Sof(O8)=Sof(C19)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(O9)=Sof(O10)=Sof(C25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(O11)=Sof(O12)=Sof(C31)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(O13)=Sof(O14)=
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(O15)=Sof(O16)=Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(O17)=Sof(O18)=Sof(C49)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=
 Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(O19)=
 Sof(O20)=Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=Sof(O21)=Sof(O22)=Sof(C61)=Sof(C62)=Sof(H62A)=Sof(H62B)=
 Sof(C63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(O23)=Sof(O24)=Sof(C67)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(O25)=Sof(O26)=Sof(C73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(C76)=
 Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=
 Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(O27)=Sof(O28)=Sof(C79)=Sof(C80)=Sof(H80A)=
 Sof(H80B)=Sof(C81)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=
 Sof(H83B)=Sof(H83C)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(O29)=Sof(O30)=
 Sof(C85)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C87)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(H88C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=Sof(C90)=Sof(H90A)=Sof(H90B)=
 Sof(H90C)=Sof(O31)=Sof(O32)=Sof(C91)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=FVAR(1)
 Sof(O35)=Sof(H35G)=Sof(H35H)=FVAR(2)
 Sof(O33)=Sof(H33A)=Sof(H33B)=FVAR(3)
 Sof(O34)=Sof(H34G)=Sof(H34H)=FVAR(4)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C97A)=Sof(H97C)=Sof(H97D)=
 Sof(C98A)=Sof(H98C)=Sof(H98D)=Sof(C99A)=Sof(H99D)=Sof(H99E)=Sof(H99F)=1-FVAR(5)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=
 Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=FVAR(5)
 Sof(O36)=Sof(H36G)=Sof(H36H)=FVAR(6)
7.a Riding coordinates:
 O33(H33A,H33B), O34(H34G,H34H), O35(H35G,H35H), O36(H36G,H36H)
7.b Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B), C98(H98A,H98B), C2(H2A,H2B), C8(H8A,H8B), C14(H14A,H14B),
 C20(H20A,H20B), C26(H26A,H26B), C32(H32A,H32B), C38(H38A,H38B), C44(H44A,H44B),
  C50(H50A,H50B), C56(H56A,H56B), C62(H62A,H62B), C68(H68A,H68B), C74(H74A,
 H74B), C80(H80A,H80B), C86(H86A,H86B), C92(H92A,H92B), C2A(H2AA,H2AB),
 C8A(H8AA,H8AB), C14A(H14C,H14D), C20A(H20C,H20D), C26A(H26C,H26D), C32A(H32C,
 H32D), C38A(H38C,H38D), C44A(H44C,H44D), C50A(H50C,H50D), C56A(H56C,H56D),
 C62A(H62C,H62D), C68A(H68C,H68D), C74A(H74C,H74D), C80A(H80C,H80D), C86A(H86C,
 H86D), C92A(H92C,H92D), C97A(H97C,H97D), C98A(H98C,H98D)
7.c Me refined with riding coordinates:
 N1(H1A,H1B,H1C), C99(H99A,H99B,H99C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
  C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C88(H88A,H88B,
 H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C94(H94A,H94B,H94C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC),
 C6A(H6AA,H6AB,H6AC), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C12A(H12D,
 H12E,H12F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F),
 C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C28A(H28D,
 H28E,H28F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C34A(H34D,H34E,H34F),
 C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C42A(H42D,H42E,H42F), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F),
 C48A(H48D,H48E,H48F), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C54A(H54D,
 H54E,H54F), C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F),
 C64A(H64D,H64E,H64F), C65A(H65D,H65E,H65F), C66A(H66D,H66E,H66F), C70A(H70D,
 H70E,H70F), C71A(H71D,H71E,H71F), C72A(H72D,H72E,H72F), C76A(H76D,H76E,H76F),
 C77A(H77D,H77E,H77F), C78A(H78D,H78E,H78F), C82A(H82D,H82E,H82F), C83A(H83D,
 H83E,H83F), C84A(H84D,H84E,H84F), C88A(H88D,H88E,H88F), C89A(H89D,H89E,H89F),
 C90A(H90D,H90E,H90F), C94A(H94D,H94E,H94F), C95A(H95D,H95E,H95F), C96A(H96D,
 H96E,H96F), N1A(H1AA,H1AB,H1AC), C99A(H99D,H99E,H99F)
7.d Idealised Me refined with riding coordinates:
 C102(H10G,H10H,H10I)
;
_shelx_res_checksum              57283
_shelx_hkl_checksum              47095
_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 14.985
_oxdiff_exptl_absorpt_empirical_full_min 0.593