The kinetics and mechanism of interconversion within a system of [Fe<sub>2</sub>L<sub>3</sub>]<sup>4+</sup> helicates and [Fe<sub>4</sub>L<sub>6</sub>]<sup>8+</sup> cages.
Siddique, Rashid G.; Arachchige, Kasun S. A.; Al-Fayaad, Hydar A; Brock, Aidan J.; Micallef, Aaron S.; Luis, Ena T.; Thoburn, John D.; McMurtrie, John C.; Clegg, Jack K.; Chemical communications (Cambridge, England) 57 (2021) 4918–4921; doi:10.1039/d1cc01583d

data_7128165
_publ_section_title
;
 The kinetics and mechanism of interconversion within a system of
 [Fe<sub>2</sub>L<sub>3</sub>]<sup>4+</sup> helicates and
 [Fe<sub>4</sub>L<sub>6</sub>]<sup>8+</sup> cages.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4918
_journal_page_last               4921
_journal_paper_doi               10.1039/d1cc01583d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C156 H126 Fe4 N24, 8(F6 P), 9(C4 H8 O), 13.5(C2 H3 N)'
_chemical_formula_sum            'C219 H238.5 F48 Fe4 N37.5 O9 P8'
_chemical_formula_weight         4923.1401
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   21.2196(8)
_cell_length_b                   21.2196(8)
_cell_length_c                   30.9753(11)
_cell_measurement_reflns_used    20489
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      29.5260
_cell_measurement_theta_min      2.3220
_cell_volume                     12078.7(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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    -11.00  85.00   0.50  120.00    --    8.20  43.00  85.00  192
  2  \w     -2.00  46.00   0.50  120.00    --    8.20 -99.00 120.00   96
  3  \w     24.00  53.00   0.50  120.00    --    8.20-112.00 159.61   58
  4  \w     -2.00  34.00   0.50  120.00    --    8.20 -99.00  30.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0374532000
_diffrn_orient_matrix_UB_12      0.0206089000
_diffrn_orient_matrix_UB_13      0.0054225000
_diffrn_orient_matrix_UB_21      -0.0093791000
_diffrn_orient_matrix_UB_22      0.0040065000
_diffrn_orient_matrix_UB_23      0.0213845000
_diffrn_orient_matrix_UB_31      -0.0003196000
_diffrn_orient_matrix_UB_32      -0.0323936000
_diffrn_orient_matrix_UB_33      0.0060716000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            85859
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             4210
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         19903
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.1300
_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^)+(0.1000P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3195
_refine_ls_wR_factor_ref         0.3394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11901
_reflns_number_total             19903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01583d2.cif
_cod_data_source_block           fe4l'6
_cod_depositor_comments
'Adding full bibliography for 7128164--7128169.cif.'
_cod_original_cell_volume        12078.7(10)
_cod_original_formula_sum        'C219 H238.50 F48 Fe4 N37.50 O9 P8'
_cod_database_code               7128165
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C240 H200 N12 Fe4 P8 F48'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.946
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2-F13
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F12) \\sim
Ueq, Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.005
Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(O2) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) = Uanis(O1) =
Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56)
4. Rigid body (RIGU) restrains
 C61, C62, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F14, F13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C53(0.75) H53A(0.75) H53B(0.75) C54(0.75) H54A(0.75) H54B(0.75)
 C55(0.75) H55A(0.75) H55B(0.75) C56(0.75) H56A(0.75) H56B(0.75) O1(0.75)
 O2(0.75) C57(0.75) H57A(0.75) H57B(0.75) C58(0.75) H58A(0.75) H58B(0.75)
 C59(0.75) H59A(0.75) H59B(0.75) C60(0.75) H60A(0.75) H60B(0.75) N9(0.5)
 C62(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
6.a Free rotating group:
 O2(C57,C58,C59,C60)
6.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
6.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C36(H36), C39(H39), C21(H21), C44(H44), C26(H26), C10(H10),
 C45(H45), C30(H30), C23(H23), C29(H29), C27(H27), C38(H38), C49(H49), C28(H28),
  C52(H52), C3(H3), C50(H50), C42(H42), C34(H34), C15(H15), C25(H25), C2(H2),
 C4(H4), C41(H41), C51(H51), C16(H16), C33(H33), C1(H1), C24(H24), C19(H19),
 C18(H18), C13(H13), C8(H8), C7(H7), C12(H12)
6.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77170
_shelx_hkl_checksum              66497
_shelx_fab_checksum              55438
_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 1.633
_oxdiff_exptl_absorpt_empirical_full_min 0.639