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_7130873
_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 Fe1 N13, 0.667(Cl3 O12.001), 3(C2 H3 N)'
_chemical_formula_sum            'C60 H54 Cl2 Fe N16 O8'
_chemical_formula_weight         1253.94
_chemical_name_systematic        040(1.230)
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-27
_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            12
_cell_length_a                   14.7047(2)
_cell_length_b                   14.7047(2)
_cell_length_c                   99.8911(10)
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    99.96(10)
_cell_measurement_theta_max      74.5170
_cell_measurement_theta_min      2.6230
_cell_volume                     18705.5(4)
_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_environment      N~2~
_diffrn_ambient_temperature      99.96(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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     37.00 113.00   0.50    1.00    --   42.40  50.00  60.00  152
  2  \w     55.00 126.00   0.50    1.00    --   42.40  30.00  90.00  142
  3  \w     25.00  51.00   0.50    1.00    --   42.40  30.00  90.00   52
  4  \w    -47.00   5.00   0.50    1.00    --   42.40  50.00  60.00  104
  5  \w    -41.00  32.00   0.50    1.00    --   44.40  60.00 120.00  146
  6  \w     55.00 134.00   0.50    1.00    --   44.40  60.00 120.00  158
  7  \w    139.00 199.00   0.50    5.00    --  110.00  30.00  90.00  120
  8  \w     42.00 199.00   0.50    5.00    --  110.00   0.00  90.00  314
  9  \w    170.00 196.00   0.50    5.00    --  110.00  44.00  42.61   52
 10  \w     63.00 192.00   0.50    5.00    --  110.00  50.00  30.00  258
 11  \w     22.00  48.00   0.50    5.00    --  110.00  40.00  60.00   52
 12  \w     87.00 113.00   0.50    5.00    --  110.00  40.00  60.00   52
 13  \w     21.00  46.00   0.50    5.00    --  110.00  50.00  30.00   50
 14  \w     56.00 195.00   0.50    5.00    --  110.00  20.00  90.00  278
 15  \w    174.00 199.00   0.50    5.00    --  110.00  10.00 -90.00   50
 16  \w     76.00 136.00   0.50    5.00    --  110.00  44.00  42.61  120
 17  \w     21.00  53.00   0.50    5.00    --  110.00  30.00  60.00   64
 18  \w     25.00  67.00   0.50    5.00    --  110.00  50.00  60.00   84
 19  \w     21.00  47.00   0.50    5.00    --  110.00  44.00  42.61   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0972915000
_diffrn_orient_matrix_UB_12      -0.0771462000
_diffrn_orient_matrix_UB_13      -0.0081626000
_diffrn_orient_matrix_UB_21      0.0045956000
_diffrn_orient_matrix_UB_22      0.0929437000
_diffrn_orient_matrix_UB_23      -0.0077361000
_diffrn_orient_matrix_UB_31      0.0715510000
_diffrn_orient_matrix_UB_32      -0.0085809000
_diffrn_orient_matrix_UB_33      -0.0105500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       123
_diffrn_reflns_limit_l_min       -122
_diffrn_reflns_number            41454
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.180
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53999
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             7800
_exptl_crystal_preparation       MeCN/EtOEt
_exptl_crystal_recrystallization_method MeCN/EtOEt
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.199
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.611
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4330
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.635
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.1052
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3256
_refine_ls_wR_factor_ref         0.3372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3844
_reflns_number_total             4330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04624e2.cif
_cod_data_source_block           lir29
_cod_original_cell_volume        18705.5(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130873
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.735
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 C6-C1
 1.5 with sigma of 0.02
 N3-C6
 2.7 with sigma of 0.02
 N3-C1
 1.2 with sigma of 0.02
 N3-C1 \\sim N00W-C00U
 with sigma of 0.002
 C6-C1 \\sim C2-C00U
 with sigma of 0.002
 Cl02-O00R \\sim Cl02-O1
 with sigma of 0.02
 Cl02-O00T \\sim Cl02-O00U
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O00T \\sim Cl02 \\sim O00R: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
N00W \\sim C00U \\sim C1 \\sim N3 \\sim C2 \\sim C6: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
O00U \\sim O00T \\sim O1 \\sim O00R: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
O00U \\sim O00T \\sim O00R \\sim O1: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004 within 2A
4. Rigid body (RIGU) restrains
 O00T, Cl02, O00R
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O00U)=Sof(O1)=0.66667*(1-FVAR(2))
 Sof(O00R)=Sof(O00T)=0.66667*FVAR(2)
 Sof(N3)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C1)=1-FVAR(2)
 Sof(C00U)=Sof(N00W)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Fixed Sof: Cl02(0.3333)
6.a Riding coordinates:
 C6(H6A,H6B,H6C)
6.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00C), C00K(H00H,H00I)
6.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00J(H00J),
 C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              10605
_shelx_hkl_checksum              37847
_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 2.106
_oxdiff_exptl_absorpt_empirical_full_min 0.727