One-, two- and three-dimensional interlocked polymers based on hybrid inorganic-organic rotaxanes.
Lockyer, Selena J.; Whitehead, George F. S.; Timco, Grigore A.; McInnes, Eric J. L.; Winpenny, Richard E. P.; Chemical communications (Cambridge, England) 60 (2024) 10124–10127; doi:10.1039/d4cc03566f

data_7133814
_publ_section_title
;
 One-, two- and three-dimensional interlocked polymers based on hybrid
 inorganic-organic rotaxanes.
;
_journal_issue                   74
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10124
_journal_page_last               10127
_journal_paper_doi               10.1039/d4cc03566f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'2(C80 H144 Cr7 F8 Ni1 O32), C83 H119 Cu4 N6 O20 S2, 5.5(C7 H8), C7 H7, C5 H10 O2, [+ solvents]'
_chemical_formula_sum            'C325 H504 Cr14 Cu4 F16 N6 Ni2 O86 S2'
_chemical_formula_weight         7339.01
_chemical_name_common            '[Cr7Ni(O2CBu)16][Cu2(O2CBu)4](N3O2SC21H22)'
_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
_audit_creation_date             2024-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-01 deposited with the CCDC.	2024-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                80.444(2)
_cell_angle_beta                 88.909(2)
_cell_angle_gamma                85.438(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5060(4)
_cell_length_b                   34.2036(11)
_cell_length_c                   35.1533(10)
_cell_measurement_reflns_used    18513
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      21.6140
_cell_measurement_theta_min      1.7310
_cell_volume                     19508.6(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.108a (Rigaku OD, 2024)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'CrysAlisPro 1.171.43.108a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 -65.00   1.00    0.20    --   30.00   0.00   0.00   80
  3  \f      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
;
_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      -0.0086480000
_diffrn_orient_matrix_UB_12      -0.0170944000
_diffrn_orient_matrix_UB_13      -0.0065541000
_diffrn_orient_matrix_UB_21      -0.0038902000
_diffrn_orient_matrix_UB_22      0.0104566000
_diffrn_orient_matrix_UB_23      -0.0184736000
_diffrn_orient_matrix_UB_31      0.0407816000
_diffrn_orient_matrix_UB_32      -0.0042569000
_diffrn_orient_matrix_UB_33      -0.0032731000
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            136794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.148
_diffrn_reflns_theta_max         20.148
_diffrn_reflns_theta_min         1.454
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.108a (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    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             7736
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone, Toluene'
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.084
_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     3828
_refine_ls_number_reflns         40744
_refine_ls_number_restraints     20612
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1014
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1725P)^2^+29.1357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2826
_refine_ls_wR_factor_ref         0.3093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25618
_reflns_number_total             40744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03566f2.cif
_cod_data_source_block           merge2
_cod_database_code               7133814
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1. Shared sites
{Cr2A, Ni2A}
{Cr3A, Ni3A}
{Cr4A, Ni4A}
{Cr5A, Ni5A}
{Cr6A, Ni6A}
{Cr2C, Ni2C}
{Cr3C, Ni3C}
{Cr4C, Ni4C}
{Cr5C, Ni5C}
{Cr6C, Ni6C}
{Cr7C, Ni7C}
2. Restrained distances
 C189-C0AP
 1.54 with sigma of 0.02
 C0AQ-C080
 1.54 with sigma of 0.02
 C7-C084
 1.54 with sigma of 0.02
 C183-C0B0
 1.54 with sigma of 0.02
 C38-C0BK
 1.54 with sigma of 0.02
 C3-C0AR
 1.54 with sigma of 0.02
 C9-C12
 1.54 with sigma of 0.02
 C30-C189 \\sim C189-C77
 with sigma of 0.02
 O1E-C6F \\sim O1E-C6E
 with sigma of 0.02
 S21F-C79 \\sim S21F-C18F \\sim S21E-C18 \\sim S21E-C18E
 with sigma of 0.02
 S21E-C18 \\sim S21E-C18E \\sim S21F-C18F \\sim S21F-C79 \\sim S42E-C313 \\sim
S42F-C93
 with sigma of 0.02
 C18E-C18 \\sim C79-C18F
 with sigma of 0.02
 C93-C39F \\sim C313-C39E \\sim C18E-C18 \\sim C18F-C79
 with sigma of 0.02
 C076-C0AQ \\sim C0AQ-C0BJ
 with sigma of 0.02
 C07W-C7 \\sim C7-C08L
 with sigma of 0.02
 C0AK-C0B0 \\sim C0B0-C0A4
 with sigma of 0.02
 C0BL-C38 \\sim C38-C09Q
 with sigma of 0.02
 C4-C0AR \\sim C0AR-C8
 with sigma of 0.02
 C10-C12 \\sim C12-C11
 with sigma of 0.02
3. Restrained planarity
 C0AP, C30, C77, C189, C0A1, C0BB, C2
 with sigma of 0.1
 C12E, C8E, C10E, C9E, C7E, C11E, C6E, O1E
 with sigma of 0.01
 C12F, C9F, C6F, C7F, C8F, C10F, C11F, O1E
 with sigma of 0.01
 C14E, C16E, C17E, C18E, C19E, C20E, C15E, S21E
 with sigma of 0.01
 O3E, C27F, C28F, C29F, C30F, C32F, C31F, C33F
 with sigma of 0.01
 C27E, C28E, C29E, C32E, C30E, C31E, C33E, O3E
 with sigma of 0.01
 C36E, C37E, C38E, C39E, C40E, C41E, C35E, S42E
 with sigma of 0.01
 C080, C0AQ, C0BJ, C076, C06Z, C092, C08S
 with sigma of 0.1
 C084, C07W, C08L, C7, C07V, C0AY, C09W
 with sigma of 0.1
 C0B0, C0AK, C0A4, C160, C170, C0B3, C183
 with sigma of 0.1
 C0BK, C09Q, C38, C0BL, C098, C09R, C0
 with sigma of 0.1
 C14F, C15F, C16F, C17F, C18F, C19F, C20F, S21F
 with sigma of 0.01
 C35F, C36F, C37F, C38F, C40F, C41F, C39F, S42F
 with sigma of 0.01
 C3, C4, C8, C0AR, C5, C6, C08T
 with sigma of 0.1
 C12, C9, C10, C11, C13, C0BC, C14
 with sigma of 0.1
4. 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(Cr2A) = Uanis(Ni2A)
Uanis(Cr3A) = Uanis(Ni3A)
Uanis(Cr4A) = Uanis(Ni4A)
Uanis(Cr5A) = Uanis(Ni5A)
Uanis(Cr6A) = Uanis(Ni6A)
Uanis(Cr2C) = Uanis(Ni2C)
Uanis(Cr3C) = Uanis(Ni3C)
Uanis(Cr4C) = Uanis(Ni4C)
Uanis(Cr5C) = Uanis(Ni5C)
Uanis(Cr6C) = Uanis(Ni6C)
Uanis(Cr7C) = Uanis(Ni7C)
5. 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
6. Same fragment restrains
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, O4A, C6A, C7A, C8A, C9A, C10A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, O8A, C16A, C17A, C18A, C19A, C20A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19A, O20A, C46A, C47A, C48A, C49A, C50A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, O6A, C11A, C12A, C13A, C14A, C15A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13A, O14A, C31A, C32A, C33A, C34A, C35A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, O10A, C21A, C22A, C23A, C24A, C25A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31A, O32A, C76A, C77A, C78A, C79A, C80A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, O12A, C26A, C27A, C28A, C29A, C30A}
{C6E, C7E, C8E, C9E, C10E, C11E, C12E, C13E, N3E, C14E, C15E, C16E, C17E, C18E,
C19E, C20E, S21E} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C6F, C7F, C8F, C9F, C10F, C11F, C12F, C13F, N3F, C14F, C15F, C16F, C17F, C18F,
C19F, C20F, S21F}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15A, O16A, C36A, C37A, C38A, C39A, C40A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25A, O26A, C61A, C62A, C63A, C64A, C65A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17A, O18A, C41A, C42A, C43A, C44A, C45A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5E, O6E, C43E, C44E, C45E, C46E, C47E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21A, O22A, C51A, C52A, C53A, C54A, C55A}
{C6E, C7E, C8E, C9E, C10E, C11E, C12E, C13E, N3E, C14E, C15E, C16E, C17E, C18E,
C19E, C20E, S21E} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C27F, C28F, C29F, C30F, C31F, C32F, C33F, C34F, N6F, C35F, C36F, C37F, C38F,
C39F, C40F, C41F, S42F}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1S, O2S, C1S, C2S, C3S, C4S, C5S}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5C, O6C, C11C, C12C, C13C, C14C, C15C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27A, O28A, C66A, C67A, C68A, C69A, C70A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23C, O24C, C56C, C57C, C58C, C59C, C60C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29A, O30A, C71A, C72A, C73A, C74A, C75A}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17E, O18E, C73E, C74E, C75E, C76E, C77E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1C, O2C, C1C, C2C, C3C, C4C, C5C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O17C, O18C, C41C, C42C, C43C, C44C, C45C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3C, O4C, C6C, C7C, C8C, C9C, C10C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9E, O10E, C53E, C54E, C55E, C56E, C57E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7C, O8C, C16C, C17C, C18C, C19C, C20C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13E, O14E, C63E, C64E, C65E, C66E, C67E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9C, O10C, C21C, C22C, C23C, C24C, C25C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O29C, O30C, C71C, C72C, C73C, C74C, C75C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O13C, O14C, C31C, C32C, C33C, C34C, C35C}
{O1E, O2E, N1E, N2E, C1E, C2E, C3E, C4E, C5E, C6E, C7E, C8E, C9E, C10E, C11E,
C12E, C13E, N3E, C14E, C15E, C16E, C17E, C18E, C19E, C20E, S21E} sigma for 1-2:
0.02, 1-3: 0.04
as in
{O3E, O4E, N4E, N5E, C22E, C23E, C24E, C25E, C26E, C27E, C28E, C29E, C30E,
C31E, C32E, C33E, C34E, N6E, C35E, C36E, C37E, C38E, C39E, C40E, C41E, S42E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15C, O16C, C36C, C37C, C38C, C39C, C40C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7E, O8E, C48E, C49E, C50E, C51E, C52E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19C, O20C, C46C, C47C, C48C, C49C, C50C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11E, O12E, C58E, C59E, C60E, C61E, C62E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O21C, O22C, C51C, C52C, C53C, C54C, C55C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O15E, O16E, C68E, C69E, C70E, C71E, C72E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O25C, O26C, C61C, C62C, C63C, C64C, C65C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O19E, O20E, C78E, C79E, C80E, C81E, C82E}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O27C, O28C, C66C, C67C, C68C, C69C, C70C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O31C, O32C, C76C, C77C, C78C, C79C, C80C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11C, O12C, C26C, C27C, C28C, C29C, C30C}
{O1A, O2A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O23A, O24A, C56A, C57A, C58A, C59A, C60A}
7. Others
 1*[Sof(Cr2A)+Sof(Ni2A)]+1*[Sof(Cr3A)+Sof(Ni3A)]+1*[Sof(Cr4A)+Sof(Ni4A)]+1*
 [Sof(Cr5A)+Sof(Ni5A)]+1*[Sof(Cr6A)+Sof(Ni6A)]=4 with esd of 0
 1*[Sof(Cr2C)+Sof(Ni2C)]+1*[Sof(Cr3C)+Sof(Ni3C)]+1*[Sof(Cr4C)+Sof(Ni4C)]+1*
 [Sof(Cr5C)+Sof(Ni5C)]+1*[Sof(Cr6C)+Sof(Ni6C)]+1*[Sof(Cr7C)+Sof(Ni7C)]=5 with
 esd of 0
 Sof(C6F)=Sof(C7F)=Sof(H7F)=Sof(C8F)=Sof(H8F)=Sof(C9F)=Sof(C10F)=Sof(H10F)=
 Sof(C11F)=Sof(H11F)=Sof(C12F)=Sof(H12C)=Sof(H12D)=Sof(C13F)=Sof(H13C)=
 Sof(H13D)=Sof(N3F)=Sof(H3FA)=Sof(H3FB)=Sof(C14F)=Sof(H14C)=Sof(H14D)=Sof(C15F)=
 Sof(C16F)=Sof(H16F)=Sof(C17F)=Sof(H17F)=Sof(C18F)=Sof(C19F)=Sof(H19F)=
 Sof(C20F)=Sof(H20F)=Sof(S21F)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(C6E)=Sof(C7E)=Sof(H7E)=Sof(C8E)=Sof(H8E)=Sof(C9E)=Sof(C10E)=Sof(H10E)=
 Sof(C11E)=Sof(H11E)=Sof(C12E)=Sof(H12A)=Sof(H12B)=Sof(C13E)=Sof(H13A)=
 Sof(H13B)=Sof(N3E)=Sof(H3EA)=Sof(H3EB)=Sof(C14E)=Sof(H14A)=Sof(H14B)=Sof(C15E)=
 Sof(C16E)=Sof(H16E)=Sof(C17E)=Sof(H17E)=Sof(C18E)=Sof(C19E)=Sof(H19E)=
 Sof(C20E)=Sof(H20E)=Sof(S21E)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(1)
 Sof(C27F)=Sof(C28F)=Sof(H28F)=Sof(C29F)=Sof(H29F)=Sof(C30F)=Sof(C31F)=
 Sof(H31F)=Sof(C32F)=Sof(H32F)=Sof(C33F)=Sof(H33C)=Sof(H33D)=Sof(C34F)=
 Sof(H34C)=Sof(H34D)=Sof(N6F)=Sof(H6FA)=Sof(H6FB)=Sof(C35F)=Sof(H35C)=Sof(H35D)=
 Sof(C36F)=Sof(C37F)=Sof(H37F)=Sof(C38F)=Sof(H38F)=Sof(C39F)=Sof(C40F)=
 Sof(H40F)=Sof(C41F)=Sof(H41F)=Sof(S42F)=1-FVAR(2)
 Sof(C27E)=Sof(C28E)=Sof(H28E)=Sof(C29E)=Sof(H29E)=Sof(C30E)=Sof(C31E)=
 Sof(H31E)=Sof(C32E)=Sof(H32E)=Sof(C33E)=Sof(H33A)=Sof(H33B)=Sof(C34E)=
 Sof(H34A)=Sof(H34B)=Sof(N6E)=Sof(H6EA)=Sof(H6EB)=Sof(C35E)=Sof(H35A)=Sof(H35B)=
 Sof(C36E)=Sof(C37E)=Sof(H37E)=Sof(C38E)=Sof(H38E)=Sof(C39E)=Sof(C40E)=
 Sof(H40E)=Sof(C41E)=Sof(H41E)=Sof(S42E)=FVAR(2)
 Sof(C0B6)=Sof(H0BD)=Sof(H0BE)=Sof(H0BF)=1-FVAR(3)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(3)
 Sof(C3)=Sof(C8)=Sof(H8)=Sof(C6)=Sof(H6)=Sof(C08T)=Sof(H08T)=Sof(C5)=Sof(H5)=
 Sof(C4)=Sof(H4)=Sof(C0AR)=Sof(H0AD)=Sof(H0AE)=Sof(H0AF)=1-FVAR(4)
 Sof(C0AQ)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C080)=Sof(C0BJ)=Sof(H0BJ)=
 Sof(C06Z)=Sof(H06Z)=Sof(C08S)=Sof(H08S)=Sof(C092)=Sof(H092)=Sof(C076)=
 Sof(H076)=FVAR(4)
 Sof(H81)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(5)
 Sof(C0B5)=Sof(H0BA)=Sof(H0BB)=Sof(H0BC)=Sof(H83)=FVAR(5)
 Sof(C9)=Sof(C10)=Sof(H10)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C0BC)=
 Sof(H0BM)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12E)=Sof(H12F)=Sof(H12G)=1-FVAR(6)
 Sof(C0AP)=Sof(C30)=Sof(H30)=Sof(C0A1)=Sof(H0A1)=Sof(C2)=Sof(H2)=Sof(C0BB)=
 Sof(H0BG)=Sof(C77)=Sof(H77)=Sof(C189)=Sof(H18J)=Sof(H18K)=Sof(H18L)=FVAR(6)
 Sof(Ni2A)=1-FVAR(7)
 Sof(Cr2A)=FVAR(7)
 Sof(Ni3A)=1-FVAR(8)
 Sof(Cr3A)=FVAR(8)
 Sof(Ni4A)=1-FVAR(9)
 Sof(Cr4A)=FVAR(9)
 Sof(Ni5A)=1-FVAR(10)
 Sof(Cr5A)=FVAR(10)
 Sof(Ni6A)=1-FVAR(11)
 Sof(Cr6A)=FVAR(11)
 Sof(Ni2C)=1-FVAR(12)
 Sof(Cr2C)=FVAR(12)
 Sof(Ni3C)=1-FVAR(13)
 Sof(Cr3C)=FVAR(13)
 Sof(Ni4C)=1-FVAR(14)
 Sof(Cr4C)=FVAR(14)
 Sof(Ni5C)=1-FVAR(15)
 Sof(Cr5C)=FVAR(15)
 Sof(Ni6C)=1-FVAR(16)
 Sof(Cr6C)=FVAR(16)
 Sof(Ni7C)=1-FVAR(17)
 Sof(Cr7C)=FVAR(17)
 Fixed Sof: C0BK(0.5) C09Q(0.5) H09Q(0.5) C098(0.5) H098(0.5) C0(0.5) H0(0.5)
 C09R(0.5) H09R(0.5) C0BL(0.5) H0BL(0.5) C38(0.5) H38I(0.5) H38J(0.5) H38K(0.5)
8.a Riding coordinates:
 O1S(H1S)
8.b Secondary CH2 refined with riding coordinates:
 C12E(H12A,H12B), C13E(H13A,H13B), N3E(H3EA,H3EB), C14E(H14A,H14B), C33E(H33A,
 H33B), C34E(H34A,H34B), N6E(H6EA,H6EB), C35E(H35A,H35B), C12F(H12C,H12D),
 C13F(H13C,H13D), N3F(H3FA,H3FB), C14F(H14C,H14D), C33F(H33C,H33D), C34F(H34C,
 H34D), N6F(H6FA,H6FB), C35F(H35C,H35D)
8.c Me refined with riding coordinates:
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C8A(H8AA,H8AB,
 H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10G,H10H), C13A(H13H,H13I,H13J),
 C14A(H14H,H14I,H14J), C15A(H15D,H15E,H15F), C18A(H18G,H18H,H18I), C19A(H19D,
 H19G,H19H), C20A(H20D,H20G,H20H), C23A(H23D,H23F,H23G), C24A(H24D,H24E,H24F),
 C25A(H25D,H25F,H25G), C28A(H28D,H28G,H28H), C29A(H29D,H29G,H29H), C30A(H30D,
 H30E,H30F), C33A(H33H,H33I,H33J), C34A(H34H,H34I,H34J), C35A(H35H,H35I,H35J),
 C38A(H38D,H38G,H38H), C39A(H39D,H39E,H39F), C40A(H40D,H40G,H40H), C43A(H43D,
 H43E,H43F), C44A(H44D,H44E,H44F), C45A(H45G,H45H,H45I), C48A(H48D,H48E,H48F),
 C49A(H49D,H49E,H49F), C50A(H50G,H50H,H50I), C53A(H53D,H53E,H53F), C54A(H54D,
 H54E,H54F), C55A(H55G,H55H,H55I), C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F),
 C60A(H60G,H60H,H60I), C63A(H63D,H63E,H63F), C64A(H64D,H64E,H64F), C65A(H65G,
 H65H,H65I), C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F), C70A(H70G,H70H,H70I),
 C73A(H73D,H73E,H73F), C74A(H74D,H74E,H74F), C75A(H75G,H75H,H75I), C78A(H78D,
 H78E,H78F), C79A(H79G,H79H,H79I), C80A(H80G,H80H,H80I), C3C(H3CA,H3CB,H3CC),
 C4C(H4CA,H4CB,H4CC), C5C(H5CA,H5CB,H5CC), C8C(H8CA,H8CB,H8CC), C9C(H9CA,H9CB,
 H9CC), C10C(H10A,H10B,H10C), C13C(H13E,H13F,H13G), C14C(H14E,H14F,H14G),
 C15C(H15A,H15B,H15C), C18C(H18D,H18E,H18F), C19C(H19A,H19B,H19C), C20C(H20A,
 H20B,H20C), C23C(H23A,H23B,H23C), C24C(H24A,H24B,H24C), C25C(H25A,H25B,H25C),
 C28C(H28A,H28B,H28C), C29C(H29A,H29B,H29C), C30C(H30A,H30B,H30C), C33C(H33E,
 H33F,H33G), C34C(H34E,H34F,H34G), C35C(H35E,H35F,H35G), C38C(H38A,H38B,H38C),
 C39C(H39A,H39B,H39C), C40C(H40A,H40B,H40C), C43C(H43A,H43B,H43C), C44C(H44A,
 H44B,H44C), C45C(H45D,H45E,H45F), C48C(H48A,H48B,H48C), C49C(H49A,H49B,H49C),
 C50C(H50D,H50E,H50F), C53C(H53A,H53B,H53C), C54C(H54A,H54B,H54C), C55C(H55D,
 H55E,H55F), C58C(H58A,H58B,H58C), C59C(H59A,H59B,H59C), C60C(H60D,H60E,H60F),
 C63C(H63A,H63B,H63C), C64C(H64A,H64B,H64C), C65C(H65D,H65E,H65F), C68C(H68A,
 H68B,H68C), C69C(H69A,H69B,H69C), C70C(H70D,H70E,H70F), C73C(H73A,H73B,H73C),
 C74C(H74A,H74B,H74C), C75C(H75D,H75E,H75F), C78C(H78A,H78B,H78C), C79C(H79D,
 H79E,H79F), C80C(H80D,H80E,H80F), C45E(H45A,H45B,H45C), C46E(H46A,H46B,H46C),
 C47E(H47A,H47B,H47C), C50E(H50A,H50B,H50C), C51E(H51A,H51B,H51C), C52E(H52A,
 H52B,H52C), C55E(H55A,H55B,H55C), C56E(H56A,H56B,H56C), C57E(H57A,H57B,H57C),
 C60E(H60A,H60B,H60C), C61E(H61A,H61B,H61C), C62E(H62A,H62B,H62C), C65E(H65A,
 H65B,H65C), C66E(H66A,H66B,H66C), C67E(H67A,H67B,H67C), C70E(H70A,H70B,H70C),
 C71E(H71A,H71B,H71C), C72E(H72A,H72B,H72C), C75E(H75A,H75B,H75C), C76E(H76A,
 H76B,H76C), C77E(H77A,H77B,H77C), C80E(H80A,H80B,H80C), C81E(H81A,H81B,H81C),
 C82E(H82A,H82B,H82C), C0AQ(H0AA,H0AB,H0AC), C0B0(H0BH,H0BI,H0BK), C0B5(H0BA,
 H0BB,H0BC), C84(H84A,H84B,H84C), C0B6(H0BD,H0BE,H0BF), C1(H1A,H1B,H1C), C7(H7A,
 H7B,H7C), C189(H18J,H18K,H18L), C38(H38I,H38J,H38K), C18(H18A,H18B,H18C),
 C79(H79A,H79B,H79C), C93(H93A,H93B,H93C), C313(H31A,H31B,H31C), C3S(H3SA,H3SB,
 H3SC), C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C0AR(H0AD,H0AE,H0AF),
 C12(H12E,H12F,H12G)
8.d Aromatic/amide H refined with riding coordinates:
 C30(H30), C0A1(H0A1), C2(H2), C0BB(H0BG), C77(H77), C1E(H1E), C2E(H2E),
 C4E(H4E), C7E(H7E), C8E(H8E), C10E(H10E), C11E(H11E), C16E(H16E), C17E(H17E),
 C19E(H19E), C20E(H20E), C22E(H22E), C23E(H23E), C25E(H25E), C28E(H28E),
 C29E(H29E), C31E(H31E), C32E(H32E), C37E(H37E), C38E(H38E), C40E(H40E),
 C41E(H41E), C0BJ(H0BJ), C06Z(H06Z), C08S(H08S), C092(H092), C076(H076),
 C07W(H07W), C07V(H07V), C09W(H09W), C0AY(H0AY), C08L(H08L), C04Y(H04Y),
 C05B(H05B), C058(H058), C81(H81), C82(H82), C83(H83), C05X(H05X), C06M(H06M),
 C06O(H06O), C06R(H06R), C09Q(H09Q), C098(H098), C0(H0), C09R(H09R), C0BL(H0BL),
  C7F(H7F), C8F(H8F), C10F(H10F), C11F(H11F), C16F(H16F), C17F(H17F),
 C19F(H19F), C20F(H20F), C28F(H28F), C29F(H29F), C31F(H31F), C32F(H32F),
 C37F(H37F), C38F(H38F), C40F(H40F), C41F(H41F), C0AK(H0AK), C160(H160),
 C0B3(H0B3), C170(H170), C0A4(H0A4), C8(H8), C6(H6), C08T(H08T), C5(H5), C4(H4),
  C10(H10), C13(H13), C14(H14), C0BC(H0BM), C11(H11)
8.e Fitted hexagon refined as free rotating group:
 C0AP(C30,C0A1,C2,C0BB,C77), C15E(C16E,C17E,C18E,C19E,C20E), C36E(C37E,C38E,
 C39E,C40E,C41E), C080(C0BJ,C06Z,C08S,C092,C076), C084(C07W,C07V,C09W,C0AY,
 C08L), C0BK(C09Q,C098,C0,C09R,C0BL), C15F(C16F,C17F,C18F,C19F,C20F), C36F(C37F,
 C38F,C39F,C40F,C41F), C183(C0AK,C160,C0B3,C170,C0A4), C3(C8,C6,C08T,C5,C4),
 C9(C10,C13,C14,C0BC,C11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 524 electrons were 
found in a volume of 3009\%A^3^ in 10 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Unit Cell 
which account for 450 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1867
_shelx_hkl_checksum              14720
_shelx_fab_checksum              92122
_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.523