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_7713778
_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         'C19 H14 Br N3'
_chemical_formula_sum            'C19 H14 Br N3'
_chemical_formula_weight         364.24
_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_block_doi                 10.5517/ccdc.csd.cc2d2ts3
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                73.8612(10)
_cell_angle_beta                 85.8430(10)
_cell_angle_gamma                87.8508(10)
_cell_formula_units_Z            4
_cell_length_a                   10.67300(10)
_cell_length_b                   11.4988(2)
_cell_length_c                   12.9614(2)
_cell_measurement_reflns_used    17328
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6820
_cell_measurement_theta_min      3.5410
_cell_volume                     1523.75(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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   -119.00 -84.00   0.50    0.35    --  -47.79-125.00-150.00   70
  2  \w    -43.00  25.00   0.50    0.35    --  -47.79  38.00-180.00  136
  3  \w    -43.00  25.00   0.50    0.35    --  -47.79  38.00  60.00  136
  4  \w   -120.00 -78.00   0.50    0.35    --  -47.79-125.00  30.00   84
  5  \w    -25.00  27.00   0.50    0.35    --  -47.79  19.00 -60.00  104
  6  \w    -69.00  22.00   0.50    0.35    --  -47.79  77.00 -60.00  182
  7  \w     43.00  93.00   0.50    0.35    --   47.79-125.00-150.00  100
  8  \w   -112.00 -79.00   0.50    1.40    --  -91.75 -15.00 -30.00   66
  9  \w   -135.00 -94.00   0.50    1.40    --  -91.75 -15.00-120.00   82
 10  \w    -59.00 -33.00   0.50    1.40    --  -91.75  61.00 150.00   52
 11  \w    -49.00 -21.00   0.50    1.40    --  -91.75  45.00  90.00   56
 12  \w     81.00 111.00   0.50    1.40    --  113.25-125.00   0.00   60
 13  \w     43.00  70.00   0.50    1.40    --  113.25 -61.00  30.00   54
 14  \w     98.00 166.00   0.50    1.40    --  113.25  77.00  60.00  136
 15  \w    126.00 178.00   0.50    1.40    --  113.25  77.00 -60.00  104
 16  \w     44.00  70.00   0.50    1.40    --  113.25 -61.00  90.00   52
 17  \w     93.00 121.00   0.50    1.40    --  113.25  77.00 -60.00   56
 18  \w     42.00  69.00   0.50    1.40    --  113.25-116.00  46.24   54
 19  \w     44.00  69.00   0.50    1.40    --  113.25 -61.00   0.00   50
 20  \w     46.00  72.00   0.50    1.40    --  113.25 -77.00-150.00   52
 21  \w     42.00  71.00   0.50    1.40    --  113.25 -61.00 120.00   58
 22  \w    111.00 136.00   0.50    1.40    --  113.25  45.00 150.00   50
 23  \w     68.00 102.00   0.50    1.40    --  113.25 -77.00  30.00   68
 24  \w     78.00 111.00   0.50    1.40    --  113.25-125.00-150.00   66
 25  \w     46.00 111.00   0.50    1.40    --  113.25-125.00 -60.00  130
 26  \w     42.00  76.00   0.50    1.40    --  113.25-125.00   0.00   68
 27  \w    143.00 168.00   0.50    1.40    --  113.25  30.00-120.00   50
 28  \w    104.00 174.00   0.50    1.40    --  113.25  15.00-150.00  140
 29  \w    119.00 159.00   0.50    1.40    --  113.25  15.00 120.00   80
 30  \w    103.00 177.00   0.50    1.40    --  113.25  30.00   0.00  148
 31  \w     44.00  71.00   0.50    1.40    --  113.25 -95.00   0.00   54
 32  \w     46.00 105.00   0.50    1.40    --  113.25 -95.00 104.00  118
 33  \w     61.00  93.00   0.50    1.40    --  113.25 -95.00 150.00   64
 34  \w     46.00 111.00   0.50    1.40    --  113.25-125.00  90.00  130
 35  \w     42.00  94.00   0.50    1.40    --  113.25 -77.00 -90.00  104
 36  \w     81.00 106.00   0.50    1.40    --  113.25 -95.00   0.00   50
 37  \w     43.00  68.00   0.50    1.40    --  113.25 -61.00 150.00   50
 38  \w    107.00 135.00   0.50    1.40    --  113.25  30.00-120.00   56
 39  \w    105.00 147.00   0.50    1.40    --  113.25  15.00 150.00   84
 40  \w     97.00 174.00   0.50    1.40    --  113.25 125.00   0.00  154
 41  \w     71.00 108.00   0.50    1.40    --  113.25-125.00 -30.00   74
 42  \w     80.00 105.00   0.50    1.40    --  113.25 -95.00  90.00   50
 43  \w    112.00 138.00   0.50    1.40    --  113.25  61.00  30.00   52
 44  \w     79.00 105.00   0.50    1.40    --  113.25 -95.00-150.00   52
 45  \w     76.00 108.00   0.50    1.40    --  113.25-116.00  46.24   64
 46  \w    101.00 127.00   0.50    1.40    --  113.25  30.00 -30.00   52
 47  \w     51.00 109.00   0.50    1.40    --  113.25-113.00  27.54  116
 48  \w     50.00 110.00   0.50    1.40    --  113.25-118.00-131.25  120
;
_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      0.0395171000
_diffrn_orient_matrix_UB_12      -0.0262799000
_diffrn_orient_matrix_UB_13      -0.1081215000
_diffrn_orient_matrix_UB_21      -0.0621356000
_diffrn_orient_matrix_UB_22      -0.1246819000
_diffrn_orient_matrix_UB_23      0.0405284000
_diffrn_orient_matrix_UB_31      -0.1246165000
_diffrn_orient_matrix_UB_32      0.0567693000
_diffrn_orient_matrix_UB_33      -0.0451824000
_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  0.0169
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.957
_diffrn_reflns_theta_min         3.557
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00052(9)
_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   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0414P)^2^+1.1904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6385
_reflns_number_total             6503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01569f2.cif
_cod_data_source_block           mcconnell29
_cod_database_code               7713778
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C19H14BrN3
_chemical_oxdiff_usercomment     'T Paschelke  TP041'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
  C29(H29), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
;
_shelx_res_checksum              44682
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.822