Improving Spin Crossover Characteristics in Heteroleptic [FeIII(qsal-5-I)(qsal-5-OMe)]A Complexes
Díaz-Torres, Raúl; Gómez-Coca, Silvia; Ruiz, Eliseo; Harding, Phimphaka; Harding, David J.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02503A

data_7714336
_publ_section_title
;
 Improving Spin Crossover Characteristics in Heteroleptic
 [FeIII(qsal-5-I)(qsal-5-OMe)]A Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02503A
_journal_year                    2023
_chemical_formula_moiety         'C34 H26 Fe N4 O4, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C36 H28 Cl2 F3 Fe N4 O7 S'
_chemical_formula_weight         844.43
_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_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.960(2)
_cell_angle_beta                 74.257(2)
_cell_angle_gamma                63.718(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3329(3)
_cell_length_b                   12.3551(2)
_cell_length_c                   12.8195(3)
_cell_measurement_reflns_used    15773
_cell_measurement_temperature    151(3)
_cell_measurement_theta_max      68.3190
_cell_measurement_theta_min      3.5650
_cell_volume                     1682.41(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      151(3)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -91.00  -9.00   0.50    0.60    --  -40.91 128.00-108.00  164
  2  \w     15.00  99.00   0.50    0.60    --   40.91-141.00   5.00  168
  3  \w      9.00  91.00   0.50    0.60    --   40.91-128.00 177.00  164
  4  \w     75.00 157.00   0.50    2.39    --   96.90 128.00-108.00  164
  5  \w     34.00 124.00   0.50    2.39    --   96.90-141.00   5.00  180
  6  \w     67.00 157.00   0.50    2.39    --   96.90 141.00  63.00  180
  7  \w     35.00 114.00   0.50    2.39    --   96.90-128.00 177.00  158
  8  \w   -114.00 -19.00   0.50    0.60    --  -40.91 -12.00   0.00  190
  9  \w    -99.00 -15.00   0.50    0.60    --  -40.91 141.00  63.00  168
 10  \w    -57.00  22.00   0.50    0.60    --  -40.91  50.00  30.00  158
 11  \w    -22.00  57.00   0.50    0.60    --   40.91 -50.00   0.00  158
 12  \w     32.00 109.00   0.50    0.60    --   40.91  25.00 -30.00  154
 13  \w    -23.00  71.00   0.50    0.60    --   40.91 -91.00 150.00  188
 14  \w     25.00 104.00   0.50    0.60    --   40.91  50.00 -90.00  158
 15  \w     21.00 105.00   0.50    0.60    --   40.91  63.00  30.00  168
 16  \w     29.00 105.00   0.50    0.60    --   40.91  37.00-150.00  152
 17  \w     32.00 109.00   0.50    0.60    --   40.91  25.00 120.00  154
 18  \w    -23.00  61.00   0.50    0.60    --   40.91 -63.00-180.00  168
 19  \w    -22.00  57.00   0.50    0.60    --   40.91 -50.00 120.00  158
 20  \w     34.00 110.00   0.50    2.39    --   96.90 -42.00  30.00  152
 21  \w     27.00 105.00   0.50    2.39    --   96.90 -96.00-180.00  156
 22  \w     32.00 123.00   0.50    2.39    --   96.90 -77.00 150.00  182
 23  \w     76.00 157.00   0.50    2.39    --   96.90  68.00  30.00  162
 24  \w     32.00 109.00   0.50    2.39    --   96.90-117.00   0.00  154
 25  \w     32.00 123.00   0.50    2.39    --   96.90 -77.00   0.00  182
 26  \w     34.00 113.00   0.50    2.39    --   96.90 -50.00-150.00  158
 27  \w     78.00 157.00   0.50    2.39    --   96.90  59.00  60.00  158
 28  \w     26.00 111.00   0.50    2.39    --   96.90 -17.00 -90.00  170
 29  \w     32.00 123.00   0.50    2.39    --   96.90 -77.00-150.00  182
 30  \w     88.00 157.00   0.50    2.39    --   96.90  25.00-180.00  138
 31  \w     34.00 126.00   0.50    2.39    --   96.90-144.00   0.00  184
 32  \w     29.00 106.00   0.50    2.39    --   96.90 -25.00-180.00  154
 33  \w     88.00 157.00   0.50    2.39    --   96.90  25.00 150.00  138
 34  \w     27.00 105.00   0.50    2.39    --   96.90 -96.00   0.00  156
 35  \w     33.00 118.00   0.50    2.39    --   96.90 -68.00 -30.00  170
 36  \w     88.00 157.00   0.50    2.39    --   96.90  25.00 120.00  138
 37  \w     32.00 109.00   0.50    2.39    --   96.90-117.00 120.00  154
 38  \w     34.00 110.00   0.50    2.39    --   96.90 -42.00 -30.00  152
 39  \w     81.00 157.00   0.50    2.39    --   96.90 117.00 -30.00  152
 40  \w     32.00 109.00   0.50    2.39    --   96.90-117.00-180.00  154
 41  \w     26.00 111.00   0.50    2.39    --   96.90 -17.00  90.00  170
 42  \w     84.00 157.00   0.50    2.39    --   96.90  96.00 120.00  146
 43  \w     34.00 110.00   0.50    2.39    --   96.90 -42.00 120.00  152
 44  \w   -104.00 -21.00   0.50    0.60    --  -40.91 -63.00 120.00  166
 45  \w   -104.00 -21.00   0.50    0.60    --  -40.91 -63.00  60.00  166
 46  \w   -104.00 -21.00   0.50    0.60    --  -40.91 -63.00-150.00  166
 47  \w   -104.00 -21.00   0.50    0.60    --  -40.91 -63.00 150.00  166
 48  \w   -104.00 -21.00   0.50    0.60    --  -40.91 -63.00   0.00  166
 49  \w     21.00 105.00   0.50    0.60    --   40.91  63.00 -30.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26061
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.551
_diffrn_reflns_theta_min         3.589
_exptl_absorpt_coefficient_mu    6.303
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       needle
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.8157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5685
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02503a2.cif
_cod_data_source_block           rdt285-150k
_cod_database_code               7714336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.177
_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.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C26(H26),
  C28(H28), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              90004
_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
- Detector area scaling
;