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_7714332
_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         'C33 H23 Fe I N4 O3, N O3, 2(C H4 O)'
_chemical_formula_sum            'C35 H31 Fe I N5 O8'
_chemical_formula_weight         832.40
_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                80.399(2)
_cell_angle_beta                 69.404(2)
_cell_angle_gamma                69.419(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0122(3)
_cell_length_b                   12.2552(2)
_cell_length_c                   12.7554(2)
_cell_measurement_reflns_used    13441
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.3280
_cell_measurement_theta_min      3.6840
_cell_volume                     1643.55(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.76a (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      150(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_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    -52.00  24.00   0.50    0.75    --  -40.91  36.00  78.00  152
  2  \w   -105.00 -30.00   0.50    0.75    --  -40.91 -36.00 -77.00  150
  3  \w     86.00 157.00   0.50    3.00    --   96.59  36.00  78.00  142
  4  \w     32.00 108.00   0.50    3.00    --   96.59 -36.00 -77.00  152
  5  \w   -104.00 -21.00   0.50    0.75    --  -40.91 -63.00 -90.00  166
  6  \w   -109.00 -32.00   0.50    0.75    --  -40.91 -25.00 -60.00  154
  7  \w    -41.00 -15.00   0.50    0.75    --  -40.91 -78.00  94.27   52
  8  \w    -77.00  14.00   0.50    0.75    --  -40.91 104.00-180.00  182
  9  \w    -57.00  22.00   0.50    0.75    --  -40.91  50.00 120.00  158
 10  \w    -66.00  24.00   0.50    0.75    --  -40.91  77.00 120.00  180
 11  \w    -23.00  53.00   0.50    0.75    --   40.91 -37.00 120.00  152
 12  \w     14.00  97.00   0.50    0.75    --   40.91-138.00  30.00  166
 13  \w     16.00  42.00   0.50    0.75    --   40.91  79.00 171.40   52
 14  \w     19.00 114.00   0.50    0.75    --   40.91  12.00  60.00  190
 15  \w     15.00  42.00   0.50    0.75    --   40.91  82.00 -53.02   54
 16  \w    -23.00  52.00   0.50    0.75    --   40.91 -36.00 -77.00  150
 17  \w     16.00  42.00   0.50    0.75    --   40.91  79.00 -30.49   52
 18  \w     16.00  42.00   0.50    0.75    --   40.91  78.00-146.47   52
 19  \w     30.00 105.00   0.50    0.75    --   40.91  36.00  78.00  150
 20  \w     15.00  42.00   0.50    0.75    --   40.91  81.00 -92.81   54
 21  \w     29.00 105.00   0.50    0.75    --   40.91  37.00 120.00  152
 22  \w     15.00  42.00   0.50    0.75    --   40.91  81.00-162.45   54
 23  \w     83.00 157.00   0.50    3.00    --   96.59  17.00   0.00  148
 24  \w     87.00 157.00   0.50    3.00    --   96.59  33.00  30.00  140
 25  \w     32.00 109.00   0.50    3.00    --   96.59-117.00 120.00  154
 26  \w     32.00 109.00   0.50    3.00    --   96.59-117.00  90.00  154
 27  \w     33.00 126.00   0.50    3.00    --   96.59-144.00 -60.00  186
 28  \w     88.00 157.00   0.50    3.00    --   96.59  25.00-180.00  138
 29  \w     33.00 126.00   0.50    3.00    --   96.59-144.00 -30.00  186
 30  \w     26.00 110.00   0.50    3.00    --   96.59 -17.00  60.00  168
 31  \w     81.00 157.00   0.50    3.00    --   96.59 117.00  30.00  152
 32  \w     33.00 118.00   0.50    3.00    --   96.59 -68.00 -60.00  170
 33  \w     32.00 109.00   0.50    3.00    --   96.59-117.00  30.00  154
 34  \w     27.00 105.00   0.50    3.00    --   96.59 -96.00 150.00  156
 35  \w     26.00 110.00   0.50    3.00    --   96.59 -17.00-120.00  168
 36  \w     27.00 105.00   0.50    3.00    --   96.59 -96.00 -60.00  156
 37  \w     83.00 157.00   0.50    3.00    --   96.59  77.00  90.00  148
 38  \w     27.00 105.00   0.50    3.00    --   96.59 -96.00 120.00  156
 39  \w     34.00 113.00   0.50    3.00    --   96.59 -50.00   0.00  158
 40  \w     76.00 157.00   0.50    3.00    --   96.59  66.00-137.72  162
 41  \w     34.00 110.00   0.50    3.00    --   96.59 -42.00  90.00  152
 42  \w     84.00 157.00   0.50    3.00    --   96.59  96.00  60.00  146
 43  \w     29.00 105.00   0.50    3.00    --   96.59 -25.00 150.00  152
 44  \w     32.00 109.00   0.50    3.00    --   96.59-117.00-180.00  154
 45  \w     33.00 118.00   0.50    3.00    --   96.59 -68.00 120.00  170
 46  \w   -104.00 -25.00   0.50    0.75    --  -40.91 -50.00 150.00  158
 47  \w    -61.00  23.00   0.50    0.75    --  -40.91  63.00-120.00  168
 48  \w   -114.00 -19.00   0.50    0.75    --  -40.91 -12.00-180.00  190
 49  \w   -104.00 -25.00   0.50    0.75    --  -40.91 -50.00   0.00  158
 50  \w   -104.00 -21.00   0.50    0.75    --  -40.91 -63.00 120.00  166
 51  \w   -104.00 -25.00   0.50    0.75    --  -40.91 -50.00-150.00  158
 52  \w   -104.00 -25.00   0.50    0.75    --  -40.91 -50.00  60.00  158
 53  \w     21.00 105.00   0.50    0.75    --   40.91  63.00 120.00  168
 54  \w    -22.00  57.00   0.50    0.75    --   40.91 -50.00-120.00  158
 55  \w     15.00  42.00   0.50    0.75    --   40.91  82.00 107.52   54
 56  \w     16.00  42.00   0.50    0.75    --   40.91  78.00 153.87   52
 57  \w     16.00  42.00   0.50    0.75    --   40.91  79.00-113.53   52
 58  \w     15.00  42.00   0.50    0.75    --   40.91  81.00  28.63   54
 59  \w     16.00  42.00   0.50    0.75    --   40.91  76.00-123.50   52
 60  \w     16.00  42.00   0.50    0.75    --   40.91  79.00 -53.15   52
 61  \w     16.00  42.00   0.50    0.75    --   40.91  80.00  -8.87   52
 62  \w     16.00  42.00   0.50    0.75    --   40.91  79.00  66.12   52
 63  \w     21.00 105.00   0.50    0.75    --   40.91  63.00 -90.00  168
 64  \w     16.00  42.00   0.50    0.75    --   40.91  76.00 100.13   52
 65  \w     16.00  42.00   0.50    0.75    --   40.91  79.00  26.78   52
;
_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  0.0966
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25178
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.490
_diffrn_reflns_theta_min         3.706
_exptl_absorpt_coefficient_mu    11.580
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.76a (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    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+2.7434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.1874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5312
_reflns_number_total             6004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02503a2.cif
_cod_data_source_block           rdt82-150k
_cod_database_code               7714332
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 C29B-O4
 1.38 with sigma of 0.02
 C13A-O3
 1.38 with sigma of 0.02
 O3-C33
 1.42 with sigma of 0.02
 O4-C34
 1.42 with sigma of 0.02
 O1-C16 \\sim O1-C16A
 with sigma of 0.02
 C10-C11 \\sim C10-C11A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C11-C16 \\sim C11A-C16A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C13-I1 \\sim C13A-I1
 with sigma of 0.02
 C13-O3 \\sim C13A-O3
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 O1-C11 \\sim O1-C11A
 with sigma of 0.04
 O1-C15 \\sim O1-C15A
 with sigma of 0.04
 C10-C12 \\sim C10-C12A
 with sigma of 0.04
 C10-C16 \\sim C10-C16A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C11-C15 \\sim C11A-C15A
 with sigma of 0.04
 C12-C14 \\sim C12A-C14A
 with sigma of 0.04
 C12-C16 \\sim C12A-C16A
 with sigma of 0.04
 C12-I1 \\sim C12A-I1
 with sigma of 0.04
 C12-O3 \\sim C12A-O3
 with sigma of 0.04
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 C14-I1 \\sim C14A-I1
 with sigma of 0.04
 C14-O3 \\sim C14A-O3
 with sigma of 0.04
 C32-C31 \\sim C32-C31A
 with sigma of 0.02
 C31-C30A \\sim C31A-C30B
 with sigma of 0.02
 C29A-C28A \\sim C29B-C28B
 with sigma of 0.02
 C29A-O4 \\sim C29B-O4
 with sigma of 0.02
 C29A-I2 \\sim C29B-I2
 with sigma of 0.02
 C29A-C30A \\sim C29B-C30B
 with sigma of 0.02
 C28A-C27A \\sim C28B-C27A
 with sigma of 0.02
 C32-C30A \\sim C32-C30B
 with sigma of 0.04
 C31-C29A \\sim C31A-C29B
 with sigma of 0.04
 C29A-C27A \\sim C29B-C27A
 with sigma of 0.04
 C28A-O4 \\sim C28B-O4
 with sigma of 0.04
 C28A-I2 \\sim C28B-I2
 with sigma of 0.04
 C28A-C30A \\sim C28B-C30B
 with sigma of 0.04
 O4-C30A \\sim O4-C30B
 with sigma of 0.04
 I2-C30A \\sim I2-C30B
 with sigma of 0.04
3. Others
 Fixed Sof: H10(0.5) H10A(0.5) C31(0.5) H31(0.5) C30A(0.5) H30A(0.5) C29A(0.5)
 C28A(0.5) H28A(0.5) C31A(0.5) H31A(0.5) C30B(0.5) H30B(0.5) C29B(0.5)
 C28B(0.5) H28B(0.5) I1(0.5) O4(0.5) C16(0.5) C11(0.5) C12(0.5) H12(0.5)
 C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) I2(0.5) O3(0.5) C16A(0.5) C11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5)
 C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C10(H10A), C17(H17),
  C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26), C31(H31),
 C30A(H30A), C28A(H28A), C31A(H31A), C30B(H30B), C28B(H28B), C12(H12), C14(H14),
  C15(H15), C12A(H12A), C14A(H14A), C15A(H15A)
4.b Fitted hexagon refined as free rotating group:
 C27A(C32,C31,C30A,C29A,C28A), C16(C11,C12,C13,C14,C15), C16A(C11A,C12A,C13A,
 C14A,C15A)
4.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
4.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9)
;
_shelx_res_checksum              17349
_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
;