Synthesis and characterisation of an integratively self-sorted [Fe4L6]8+ tetrahedron
Taylor, Lauren L. K.; Andrews, Rebecca; Sung, April C. Y.; Vitorica-Yrezabal, Iñigo J.; Riddell, Imogen A.; Chemical Communications  (2022) –; doi:10.1039/D2CC04624E

data_7130875
_publ_section_title
;
 Synthesis and characterisation of an integratively self-sorted [Fe4L6]8+
 tetrahedron
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04624E
_journal_year                    2022
_chemical_formula_moiety
'C54 H45 Fe N13, 2(C2 F6 N O4 S2), 3.929(C2 H3 N)'
_chemical_formula_sum            'C65.86 H56.79 F12 Fe N18.93 O8 S4'
_chemical_formula_weight         1653.52
_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             2021-09-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-09-28 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.413(2)
_cell_angle_beta                 72.158(2)
_cell_angle_gamma                77.821(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5031(2)
_cell_length_b                   15.5665(3)
_cell_length_c                   19.8576(4)
_cell_measurement_reflns_used    39020
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.0570
_cell_measurement_theta_min      1.5750
_cell_volume                     3574.56(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.866
_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       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0059181000
_diffrn_orient_matrix_UB_12      -0.0437456000
_diffrn_orient_matrix_UB_13      0.0042606000
_diffrn_orient_matrix_UB_21      0.0286072000
_diffrn_orient_matrix_UB_22      -0.0089261000
_diffrn_orient_matrix_UB_23      0.0256842000
_diffrn_orient_matrix_UB_31      -0.0509619000
_diffrn_orient_matrix_UB_32      0.0090156000
_diffrn_orient_matrix_UB_33      0.0258168000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            77550
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         36.267
_diffrn_reflns_theta_min         1.683
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             1693
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         32879
_refine_ls_number_restraints     724
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0673P)^2^+0.4660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27666
_reflns_number_total             32879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04624e2.cif
_cod_data_source_block           m_ir_lt_040_1235_c2_col1_
_cod_original_cell_volume        3574.56(13)
_cod_database_code               7130875
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.980
_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
 S3-O6 \\sim S5-O10
 with sigma of 0.02
 S3-C69 \\sim S5-C67
 with sigma of 0.02
 O6-N20 \\sim O10-N21
 with sigma of 0.04
 O5-C69 \\sim O9-C67
 with sigma of 0.04
 F7-F9 \\sim F15-F13
 with sigma of 0.04
 F10-F11 \\sim F17-F18
 with sigma of 0.04
 S3-O5 \\sim S5-O9
 with sigma of 0.02
 F8-C69 \\sim F14-C67
 with sigma of 0.02
 N20-C68 \\sim N21-C66
 with sigma of 0.04
 F7-C69 \\sim F15-C67
 with sigma of 0.02
 S3-N20 \\sim S5-N21
 with sigma of 0.02
 F9-C69 \\sim F13-C67
 with sigma of 0.02
 O7-N20 \\sim O12-N21
 with sigma of 0.04
 O6-C69 \\sim O10-C67
 with sigma of 0.04
 S4-O7 \\sim S6-O12
 with sigma of 0.02
 S3-F8 \\sim S5-F14
 with sigma of 0.04
 S3-F7 \\sim S5-F15
 with sigma of 0.04
 S4-O8 \\sim S6-O11
 with sigma of 0.02
 S4-N20 \\sim S6-N21
 with sigma of 0.02
 S3-F9 \\sim S5-F13
 with sigma of 0.04
 N20-C69 \\sim N21-C67
 with sigma of 0.04
 S4-C68 \\sim S6-C66
 with sigma of 0.02
 F8-F7 \\sim F14-F15
 with sigma of 0.04
 F8-F9 \\sim F14-F13
 with sigma of 0.04
 F10-C68 \\sim F17-C66
 with sigma of 0.02
 F12-C68 \\sim F16-C66
 with sigma of 0.02
 O8-N20 \\sim O11-N21
 with sigma of 0.04
 F12-F11 \\sim F16-F18
 with sigma of 0.04
 F11-C68 \\sim F18-C66
 with sigma of 0.02
 O7-O8 \\sim O12-O11
 with sigma of 0.04
 O7-C68 \\sim O12-C66
 with sigma of 0.04
 O6-O5 \\sim O10-O9
 with sigma of 0.04
 S3-S4 \\sim S5-S6
 with sigma of 0.04
 O5-N20 \\sim O9-N21
 with sigma of 0.04
 O8-C68 \\sim O11-C66
 with sigma of 0.04
 S4-F10 \\sim S6-F17
 with sigma of 0.04
 S4-F12 \\sim S6-F16
 with sigma of 0.04
 S4-F11 \\sim S6-F18
 with sigma of 0.04
 F10-F12 \\sim F17-F16
 with sigma of 0.04
 N15-C30 \\sim N12-C33 \\sim N14-C35 \\sim N13-C37
 with sigma of 0.02
 N15-C32 \\sim N12-C32 \\sim N14-C019 \\sim N13-C019
 with sigma of 0.02
 C39-C37 \\sim C35-C34 \\sim C38-C33 \\sim C30-C31
 with sigma of 0.02
 C34-C019 \\sim C39-C019 \\sim C32-C31 \\sim C38-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C67 \\sim S3 \\sim O6 \\sim O5 \\sim N20 \\sim C69 \\sim S4 \\sim F8 \\sim F7
\\sim F9 \\sim S5 \\sim O9 \\sim F12 \\sim C68 \\sim C66 \\sim F17 \\sim O7
\\sim O8 \\sim O10 \\sim N21 \\sim F11 \\sim F10 \\sim S6 \\sim F18 \\sim F16
\\sim O12 \\sim O11 \\sim F14 \\sim F15 \\sim F13: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C34 \\sim N14 \\sim N13 \\sim C39 \\sim N15 \\sim C31 \\sim N12 \\sim C38:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
4. Rigid body (RIGU) restrains
 N21, C67, S5, F14, F15, F13, O10, O9, S6, O12, O11, C66, F18, F17, F16, F8,
 S3, O6, O5, N20, C69, S4, F7, F9, O7, O8, C68, F11, F10, F12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C65, S2, O3, O4, N19, C64, F4, F6, F5, O1, O2, F2, F3, F1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C67)=Sof(S5)=Sof(O10)=Sof(O9)=Sof(N21)=Sof(S6)=Sof(F14)=Sof(F15)=Sof(F13)=
 Sof(O12)=Sof(O11)=Sof(C66)=Sof(F18)=Sof(F17)=Sof(F16)=1-FVAR(1)
 Sof(S3)=Sof(S4)=Sof(F8)=Sof(F10)=Sof(F12)=Sof(F7)=Sof(O7)=Sof(F9)=Sof(O6)=
 Sof(O5)=Sof(O8)=Sof(F11)=Sof(N20)=Sof(N18)=Sof(C58)=Sof(C69)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C68)=FVAR(1)
 Sof(H30A)=Sof(H33A)=Sof(H35A)=Sof(H37A)=Sof(N14)=Sof(N15)=Sof(C39)=Sof(H39)=
 Sof(C38)=Sof(H38)=1-FVAR(2)
 Sof(N12)=Sof(N13)=Sof(C31)=Sof(H31)=Sof(C34)=Sof(H34)=Sof(H30)=Sof(H33)=
 Sof(H35)=Sof(H37)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C40(H40), C28(H28), C31(H31), C34(H34), C26(H26),
 C45(H45), C25(H25), C23(H23), C19(H19), C42(H42), C7(H7), C15(H15), C14(H14),
 C30(H30), C30(H30A), C10(H10), C33(H33), C33(H33A), C20(H20), C9(H9), C49(H49),
  C48(H48), C36(H36), C43(H43), C21(H21), C22(H22), C52(H52), C47(H47),
 C35(H35A), C35(H35), C37(H37), C37(H37A), C54(H54), C55(H55), C53(H53),
 C39(H39), C38(H38)
6.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C), C63(H63A,H63B,
 H63C)
;
_shelx_res_checksum              55623
_shelx_hkl_checksum              3228
_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 1.597
_oxdiff_exptl_absorpt_empirical_full_min 0.387