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_7130872
_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
'C114 H84 Fe4 N25, 7.999(Cl O4), 3.182(C2 H3 N1), H1 O1'
_chemical_formula_sum            'C120.39 H94.58 Cl8 Fe4 N28.2 O32.99'
_chemical_formula_weight         2971.07
_chemical_name_systematic        C1
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-05-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.1400(7)
_cell_length_b                   21.1400(7)
_cell_length_c                   67.0247(16)
_cell_measurement_reflns_used    7566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.6570
_cell_measurement_theta_min      1.6050
_cell_volume                     25940.3(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_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  24.00   1.00    0.20    --   30.00   0.00   0.00  169
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0343958000
_diffrn_orient_matrix_UB_12      -0.0237389000
_diffrn_orient_matrix_UB_13      -0.0036567000
_diffrn_orient_matrix_UB_21      0.0030649000
_diffrn_orient_matrix_UB_22      0.0264952000
_diffrn_orient_matrix_UB_23      -0.0065474000
_diffrn_orient_matrix_UB_31      0.0150038000
_diffrn_orient_matrix_UB_32      -0.0123730000
_diffrn_orient_matrix_UB_33      -0.0070272000
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            60877
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.517
_diffrn_reflns_theta_min         1.597
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             9109
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10558
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.1947
_refine_ls_R_factor_gt           0.1384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3692
_refine_ls_wR_factor_ref         0.4153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4295
_reflns_number_total             10558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04624e2.cif
_cod_data_source_block           m_ir_lt_040_1_172_c1_col1_
_cod_original_cell_volume        25940.3(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C120.39 H94.58 Cl8 Fe4 N28.20 O32.99'
_cod_database_code               7130872
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.927
_reflns_odcompleteness_completeness 88.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.16
_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, All O(H,H) groups
2. Restrained distances
 O12A-O13A = O14A-O13A = O14A-O15A = O13A-O15A = O12A-O15A = O12A-O14A = O8A-
 O10A = O8A-O9A = O10A-O9A = O8A-O7A = O7A-O10A = O7A-O9A
 2.375 with sigma of 0.02
 C2S-C3S
 1.456 with sigma of 0.01
 C3S-N1S
 2.593 with sigma of 0.02
 C2S-N1S
 1.137 with sigma of 0.01
 Cl1A-O3A \\sim Cl1A-O4A \\sim Cl1A-O5A \\sim Cl1A-O2A \\sim Cl6A-O7A \\sim
Cl6A-O8A \\sim Cl6A-O10A ~
 Cl6A-O9A \\sim Cl11-O12A \\sim Cl11-O13A \\sim Cl11-O15A \\sim Cl11-O14A
 with sigma of 0.02
 C5S-C6S \\sim C3S-C2S
 with sigma of 0.002
 N1S-C2S \\sim N4S-C5S
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
N4S \\sim C5S \\sim C6S \\sim N1S \\sim C2S \\sim C3S: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
O10A \\sim O9A \\sim Cl6A \\sim O8A \\sim O7A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
N1S \\sim C2S \\sim C3S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N1S: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within
2A
C4 \\sim C3 \\sim C2 \\sim N1 \\sim C6 \\sim C5: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
Uanis(N4S) \\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(C6S) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 Cl11, O15A, O14A, O12A, O13A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1S, C2S, C3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, Cl6A, O9A, O8A, O10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N37, C42, C41, C40, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(Cl11)+Sof(O15A)+Sof(O14A)+Sof(O12A)+Sof(O13A)]+1*[Sof(Cl1A)+Sof(O4A)+
 Sof(O5A)+Sof(O2A)+Sof(O3A)]+1*[Sof(Cl6A)+Sof(O9A)+Sof(O8A)+Sof(O10A)+Sof(O7A)]=
 2.6667 with esd of 0.001
 Sof(Cl11)=Sof(O15A)=Sof(O14A)=Sof(O12A)=Sof(O13A)=FVAR(1)
 Sof(Cl1A)=Sof(O4A)=Sof(O5A)=Sof(O2A)=Sof(O3A)=FVAR(2)
 Sof(Cl6A)=Sof(O9A)=Sof(O8A)=Sof(O10A)=Sof(O7A)=FVAR(3)
 Sof(N1S)=Sof(C2S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=FVAR(4)
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=Sof(N4S)=Sof(C5S)=0.33333*FVAR(6)
 Fixed Sof: H7SA(0.16667) H7SB(0.16667)
6.a Riding coordinates:
 C3S(H3SA,H3SB,H3SC), O7S(H7SA,H7SB), C6S(H6SA,H6SB,H6SC)
6.b Free rotating group:
 N1S(C2S,C3S)
6.c Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B)
6.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C14(H14), C42(H42), C34(H34), C17(H17), C5(H5), C33(H33), C10(H10),
 C23(H23), C16(H16), C27(H27), C2(H2), C22(H22), C3(H3), C26(H26), C43(H43),
 C9(H9), C39(H39), C4(H4), C20(H20), C21(H21), C28(H28), C29(H29), C40(H40)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97508
_shelx_hkl_checksum              20326
_shelx_fab_checksum              9144
_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 1.609
_oxdiff_exptl_absorpt_empirical_full_min 0.621