Tuning the spin-crossover properties of FeII4L<sub>6</sub> cages <i>via</i> the interplay of coordination motif and linker modifications.
Paschelke, Tobias; Trumpf, Eicke; Grantz, David; Pankau, Malte; Grocholski, Niclas; Näther, Christian; Sönnichsen, Frank D; McConnell, Anna J.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01569f

data_7713780
_publ_section_title
;
 Tuning the spin-crossover properties of FeII4L<sub>6</sub> cages
 <i>via</i> the interplay of coordination motif and linker modifications.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01569f
_journal_year                    2023
_chemical_formula_moiety         'C156 H120 Fe4 N36, 6(C F3 O3 S)'
_chemical_formula_sum            'C162 H120 F24 Fe4 N36 O24 S8'
_chemical_formula_weight         3890.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2d2tt4
_audit_creation_date             2022-09-06
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   67.4664(11)
_cell_length_b                   17.1648(4)
_cell_length_c                   32.7981(2)
_cell_measurement_reflns_used    44051
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.5530
_cell_measurement_theta_min      2.3800
_cell_volume                     37981.7(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.40a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.946
_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    -16.00  26.18   0.38  100.00    --  -43.21  37.00 129.00  111
  2  \w    -59.00 -27.84   0.38  100.00    --  -43.21  94.00 -31.00   82
  3  \w    -63.00 -31.84   0.38  100.00    --  -43.21 103.00-132.00   82
  4  \w   -142.00-114.64   0.38  580.00    --  -96.00 -37.00 -25.00   72
  5  \w    128.00 154.22   0.38  580.00    --  117.50  94.00 -31.00   69
  6  \w     48.00  92.08   0.38  580.00    --  117.50 -94.00-142.00  116
  7  \w     43.00  92.40   0.38  580.00    --  117.50-103.00 124.00  130
  8  \w    -19.00  30.02   0.38  100.00    --  -43.21  38.00  30.00  129
  9  \w    -32.00  17.02   0.38  100.00    --   43.21 -38.00 -90.00  129
 10  \w     44.00  69.08   0.38  580.00    --  117.50 -77.00-120.00   66
 11  \w    114.00 141.74   0.38  580.00    --  117.50  61.00-150.00   73
 12  \w    147.00 171.70   0.38  580.00    --  117.50  61.00-150.00   65
 13  \w    106.00 134.88   0.38  580.00    --  117.50  15.00   0.00   76
 14  \w    106.00 132.22   0.38  580.00    --  117.50  15.00-120.00   69
 15  \w    103.00 128.08   0.38  580.00    --  117.50  15.00-180.00   66
 16  \w    103.00 128.08   0.38  580.00    --  117.50  15.00  30.00   66
 17  \w    105.00 129.70   0.38  580.00    --  117.50  15.00 120.00   65
 18  \w    105.00 133.88   0.38  580.00    --  117.50  15.00 -30.00   76
 19  \w     56.00  94.00   0.38  580.00    --  117.50-125.00 -90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449098000
_diffrn_orient_matrix_UB_12      0.0010609000
_diffrn_orient_matrix_UB_13      0.0259912000
_diffrn_orient_matrix_UB_21      -0.0031405000
_diffrn_orient_matrix_UB_22      -0.0211677000
_diffrn_orient_matrix_UB_23      0.0331536000
_diffrn_orient_matrix_UB_31      0.0133995000
_diffrn_orient_matrix_UB_32      -0.0085090000
_diffrn_orient_matrix_UB_33      -0.0792405000
_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  0.0882
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       84
_diffrn_reflns_limit_h_min       -86
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            115736
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.854
_diffrn_reflns_theta_min         2.620
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.40a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             15872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2210
_refine_ls_number_reflns         39182
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.815
_refine_ls_R_factor_all          0.1790
_refine_ls_R_factor_gt           0.1603
_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          0.4349
_refine_ls_wR_factor_ref         0.4511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29968
_reflns_number_total             39182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01569f2.cif
_cod_data_source_block           mcconnell33n
_cod_database_code               7713780
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C164H120N36F24S8O24Fe4
_chemical_oxdiff_usercomment     'tobias paschelke tp114'
_reflns_odcompleteness_completeness 96.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C151-F53
 1.3 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C121, F21, F22, F23
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 S41, O41, O42, O43, C141, F41, F42, F43
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 S51, O51, O52, O53, C151, F51, F52, F53
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C2A(H2A), C3A(H3A),
  C4A(H4A), C5A(H5A), C10A(H10A), C12A(H12A), C13A(H13A), C15A(H15A),
 C17A(H17A), C18A(H18A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C10B(H10B), C12B(H12B), C13B(H13B),
 C15B(H15B), C17B(H17B), C18B(H18B), C21B(H21B), C22B(H22B), C23B(H23B),
 C24B(H24B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C10C(H10C), C12C(H12C),
 C13C(H13C), C15C(H15C), C17C(H17C), C18C(H18C), C21C(H21C), C22C(H22C),
 C23C(H23C), C24C(H24C), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C10D(H10D),
 C12D(H12D), C13D(H13D), C15D(H15D), C17D(H17D), C18D(H18D), C21D(H21D),
 C22D(H22D), C23D(H23D), C24D(H24D), C2E(H2E), C3E(H3E), C4E(H4E), C5E(H5E),
 C10E(H10E), C12E(H12E), C13E(H13E), C15E(H15E), C17E(H17E), C18E(H18E),
 C21E(H21E), C22E(H22E), C23E(H23E), C24E(H24E)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C8A(H8AA,H8AB,H8AC), C26A(H26D,H26E,
 H26F), C8B(H8BA,H8BB,H8BC), C26B(H26G,H26H,H26I), C8C(H8CA,H8CB,H8CC),
 C26C(H26J,H26K,H26L), C8D(H8DA,H8DB,H8DC), C26D(H26M,H26N,H26O), C8E(H8EA,H8EB,
 H8EC), C26E(H26P,H26Q,H26R)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56245
_shelx_fab_checksum              97325
_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 2.293
_oxdiff_exptl_absorpt_empirical_full_min 0.467