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_7130874
_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         'C120 H84 Fe4 N24, 8(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C132 H90 F24 Fe4 N26 O24 S8'
_chemical_formula_weight         3360.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.492(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.990(3)
_cell_length_b                   18.5196(12)
_cell_length_c                   28.075(2)
_cell_measurement_reflns_used    3054
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      19.9260
_cell_measurement_theta_min      3.0280
_cell_volume                     15136(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_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  \w    -13.00  77.00   2.00  129.96    --    9.09  57.00-150.00   45
  2  \w    -10.00  52.00   2.00  129.96    --    9.09 -99.00 -30.00   31
  3  \w    -64.00  42.00   2.00  129.96    --    9.09 -19.00  30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0201066000
_diffrn_orient_matrix_UB_12      0.0141057000
_diffrn_orient_matrix_UB_13      0.0013478000
_diffrn_orient_matrix_UB_21      0.0134117000
_diffrn_orient_matrix_UB_22      0.0138830000
_diffrn_orient_matrix_UB_23      0.0253586000
_diffrn_orient_matrix_UB_31      0.0029549000
_diffrn_orient_matrix_UB_32      0.0328013000
_diffrn_orient_matrix_UB_33      -0.0112264000
_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  0.1191
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27222
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.814
_diffrn_reflns_theta_max         20.814
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26151
_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    1.475
_exptl_crystal_description       plate
_exptl_crystal_F_000             6816
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     586
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.2015
_refine_ls_R_factor_gt           0.1348
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3475
_refine_ls_wR_factor_ref         0.3981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4281
_reflns_number_total             7890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04624e2.cif
_cod_data_source_block           air18
_cod_database_code               7130874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.825
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.77
_olex2_refinement_description
;
1. Others
 Fixed Sof: C13A(0.5) F14A(0.5) F16A(0.5) F15A(0.5) S9A(0.5) O10A(0.5)
 O11A(0.5) O12A(0.5)
 Fixed Uiso: H9(0.061) H68(0.061) H33(0.061) H50(0.061) H38(0.056) H14(0.065)
 H35(0.07) H17(0.08) H48(0.108) H57(0.088) H36(0.078) H42(0.089) H61(0.091)
 H18(0.082) H45(0.071) H12(0.078) H11(0.083) H70(0.09) H21(0.094) H46(0.096)
 H41(0.085) H24(0.088) H71(0.102) H2(0.104) H58(0.106) H47(0.11) H26(0.096)
 H59(0.099) H23(0.1) H60(0.109) H29(0.097) H22(0.103) H53(0.152) H64(0.108)
 H63(0.124) H5(0.13) H28(0.099) H52(0.138) H62(0.114) H27(0.099) H3(0.128)
 H4(0.158) H8A(0.24) H8B(0.24) H8C(0.24)
 Fixed X: H9(0.333575) H68(0.280914) H33(0.379807) H50(0.26231) H38(0.364885)
 H14(0.201331) H35(0.432167) H17(0.316158) H48(0.423348) H57(0.440384)
 H36(0.443752) H42(0.434711) H61(0.4828) H18(0.333454) H45(0.34905)
 H12(0.249716) H11(0.230438) H70(0.286834) H21(0.136335) H46(0.379792)
 H41(0.430396) H24(0.290669) H71(0.365603) H2(0.405026) H58(0.504036)
 H47(0.418249) H26(0.423805) H59(0.505699) H23(0.256996) H60(0.440874)
 H29(0.460369) H22(0.177648) H53(0.374506) H64(0.438376) H63(0.515481)
 H5(0.272236) H28(0.481831) H52(0.306124) H62(0.534682) H27(0.456462)
 H3(0.369285) H4(0.300152) H8A(0.374714) H8B(0.3703) H8C(0.353202)
 Fixed Y: H9(0.433828) H68(0.27267) H33(0.363758) H50(0.656562) H38(0.5761)
 H14(0.502754) H35(0.558855) H17(0.659847) H48(0.467216) H57(0.681605)
 H36(0.524706) H42(0.394159) H61(0.246146) H18(0.540063) H45(0.681135)
 H12(0.272038) H11(0.393236) H70(0.164723) H21(0.802414) H46(0.632338)
 H41(0.426045) H24(0.771911) H71(0.156047) H2(0.124561) H58(0.743451)
 H47(0.52151) H26(0.240872) H59(0.793033) H23(0.883371) H60(0.788844)
 H29(0.47814) H22(0.896449) H53(0.777941) H64(0.14763) H63(0.132702)
 H5(0.158807) H28(0.41656) H52(0.763627) H62(0.185481) H27(0.299892)
 H3(0.02741) H4(0.042587) H8A(0.428663) H8B(0.444894) H8C(0.370865)
 Fixed Z: H9(0.428319) H68(0.453612) H33(0.562783) H50(0.574599) H38(0.596131)
 H14(0.336697) H35(0.561146) H17(0.354085) H48(0.809549) H57(0.764913)
 H36(0.489677) H42(0.6613) H61(0.505438) H18(0.369037) H45(0.789632)
 H12(0.299706) H11(0.290361) H70(0.578732) H21(0.274547) H46(0.867822)
 H41(0.737693) H24(0.324101) H71(0.606349) H2(0.460449) H58(0.770951)
 H47(0.882913) H26(0.388777) H59(0.69482) H23(0.295503) H60(0.620715)
 H29(0.427763) H22(0.264562) H53(0.548756) H64(0.624991) H63(0.634721)
 H5(0.319236) H28(0.366138) H52(0.481655) H62(0.571512) H27(0.345276)
 H3(0.412428) H4(0.33416) H8A(0.263213) H8B(0.315737) H8C(0.287216)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36167
_shelx_hkl_checksum              32601
_shelx_fab_checksum              90408
_olex2_submission_original_sample_id C3
_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 1.988
_oxdiff_exptl_absorpt_empirical_full_min 0.401