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_7714335
_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
'C32.93 H22.79 Fe I1.07 N4 O2.93, C F3 O3 S, C H4 O'
_chemical_formula_sum            'C34.93 H26.79 F3 Fe I1.07 N4 O6.93 S'
_chemical_formula_weight         894.12
_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             2023-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-13 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                68.856(4)
_cell_angle_beta                 86.751(3)
_cell_angle_gamma                68.419(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2770(4)
_cell_length_b                   12.4031(5)
_cell_length_c                   12.7647(6)
_cell_measurement_reflns_used    14148
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      68.1910
_cell_measurement_theta_min      3.7060
_cell_volume                     1679.29(14)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -84.00   0.00   0.50    0.25    --  -40.91 117.00-129.00  168
  2  \w   -111.00 -26.00   0.50    0.25    --  -40.91 161.00  22.00  170
  3  \w   -105.00 -54.00   0.50    0.25    --  -40.91-161.00  -7.00  102
  4  \w     54.00 105.00   0.50    0.25    --   40.91 161.00  22.00  102
  5  \w      0.00  84.00   0.50    0.25    --   40.91-117.00 143.00  168
  6  \w     27.00 111.00   0.50    0.25    --   40.91-161.00  -7.00  168
  7  \w     32.00 109.00   0.50    1.00    --   96.59-117.00 143.00  154
  8  \w     32.00 136.00   0.50    1.00    --   96.59-161.00  -7.00  208
  9  \w     53.00 157.00   0.50    1.00    --   96.59 161.00  22.00  208
 10  \w     81.00 157.00   0.50    1.00    --   96.59 117.00-129.00  152
 11  \w   -105.00 -29.00   0.50    0.25    --  -40.91 -37.00-120.00  152
 12  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00  30.00  166
 13  \w    -53.00  23.00   0.50    0.25    --  -40.91  37.00 -90.00  152
 14  \w    -53.00  23.00   0.50    0.25    --  -40.91  37.00-150.00  152
 15  \w   -109.00 -32.00   0.50    0.25    --  -40.91 -25.00  90.00  154
 16  \w    -66.00  24.00   0.50    0.25    --  -40.91  77.00 -60.00  180
 17  \w    -23.00  53.00   0.50    0.25    --   40.91 -37.00 120.00  152
 18  \w    -22.00  57.00   0.50    0.25    --   40.91 -50.00 -30.00  158
 19  \w     25.00 104.00   0.50    0.25    --   40.91  50.00   0.00  158
 20  \w    -24.00  67.00   0.50    0.25    --   40.91 -77.00 -90.00  182
 21  \w    -22.00  57.00   0.50    0.25    --   40.91 -50.00  60.00  158
 22  \w     32.00 109.00   0.50    0.25    --   40.91  25.00 -90.00  154
 23  \w     33.00 126.00   0.50    1.00    --   96.59-144.00-120.00  186
 24  \w     81.00 157.00   0.50    1.00    --   96.59  50.00 -90.00  152
 25  \w     29.00 105.00   0.50    1.00    --   96.59 -25.00  90.00  152
 26  \w     34.00 113.00   0.50    1.00    --   96.59 -50.00-180.00  158
 27  \w     32.00 122.00   0.50    1.00    --   96.59 -77.00 120.00  180
 28  \w     67.00 157.00   0.50    1.00    --   96.59 144.00-180.00  180
 29  \w     83.00 157.00   0.50    1.00    --   96.59  77.00 -90.00  148
 30  \w     32.00 109.00   0.50    1.00    --   96.59-117.00 -30.00  154
 31  \w     33.00 126.00   0.50    1.00    --   96.59-144.00 150.00  186
 32  \w     81.00 157.00   0.50    1.00    --   96.59 117.00 -30.00  152
 33  \w     32.00 109.00   0.50    1.00    --   96.59-117.00-180.00  154
 34  \w     33.00 115.00   0.50    1.00    --   96.59 -59.00 -60.00  164
 35  \w     31.00 124.00   0.50    1.00    --   96.59 -86.00 -60.00  186
 36  \w     88.00 157.00   0.50    1.00    --   96.59  25.00-180.00  138
 37  \w     32.00 109.00   0.50    1.00    --   96.59-117.00  30.00  154
 38  \w     84.00 157.00   0.50    1.00    --   96.59  96.00  90.00  146
 39  \w     32.00 122.00   0.50    1.00    --   96.59 -77.00 150.00  180
 40  \w     81.00 157.00   0.50    1.00    --   96.59 117.00-150.00  152
 41  \w     83.00 157.00   0.50    1.00    --   96.59  77.00  30.00  148
 42  \w     87.00 157.00   0.50    1.00    --   96.59  33.00   0.00  140
 43  \w     84.00 157.00   0.50    1.00    --   96.59  96.00   0.00  146
 44  \w     88.00 157.00   0.50    1.00    --   96.59  25.00 -30.00  138
 45  \w     34.00 110.00   0.50    1.00    --   96.59 -42.00 -90.00  152
 46  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00  90.00  166
 47  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00 -30.00  166
 48  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00-120.00  166
 49  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00 150.00  166
 50  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00 120.00  166
 51  \w   -104.00 -21.00   0.50    0.25    --  -40.91 -63.00-180.00  166
;
_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  0.0848
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25194
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.620
_diffrn_reflns_theta_min         3.727
_exptl_absorpt_coefficient_mu    12.549
_exptl_absorpt_correction_T_max  0.508
_exptl_absorpt_correction_T_min  0.038
_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    1.768
_exptl_crystal_description       block
_exptl_crystal_F_000             891
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00111(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0451P)^2^+8.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5589
_reflns_number_total             6140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02503a2.cif
_cod_data_source_block           rdt135c-150k
_cod_original_cell_volume        1679.29(13)
_cod_database_code               7714335
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 O4-C34
 1.42 with sigma of 0.02
 O4-C30
 1.38 with sigma of 0.02
 C15-O3
 1.38 with sigma of 0.02
 O3-C17
 1.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O3) = Uiso(C17)
Uiso(O4) = Uiso(C34)
4. Others
 Fixed Sof: I1(0.48) I2(0.59) O3(0.52) C17(0.52) H17A(0.52) H17B(0.52)
 H17C(0.52) O4(0.41) C34(0.41) H34A(0.41) H34B(0.41) H34C(0.41)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14),
 C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C27(H27),
  C29(H29), C31(H31), C32(H32)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C)
5.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              69365
_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
;