Light and thermally activated spin crossover coupled to an order–disorder transition of a propyl chain in an iron(iii) complex
Boonprab, Theerapoom; Habarakada, Upeksha; Chastanet, Guillaume; Harding, Phimphaka; Harding, David J.; CrystEngComm 25 (2023) 4126–4132; doi:10.1039/D3CE00425B

data_7246862
_publ_section_title
;
 Light and thermally activated spin crossover coupled to an
 order--disorder transition of a propyl chain in an iron(iii) complex
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4126
_journal_page_last               4132
_journal_paper_doi               10.1039/D3CE00425B
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'I, C32 H38 Fe N4 O2, C H2 Cl2'
_chemical_formula_sum            'C33 H40 Cl2 Fe I N4 O2'
_chemical_formula_weight         778.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.38700(10)
_cell_length_b                   12.60600(10)
_cell_length_c                   23.8251(2)
_cell_measurement_reflns_used    16471
_cell_measurement_temperature    200.0(5)
_cell_measurement_theta_max      68.3280
_cell_measurement_theta_min      1.8460
_cell_volume                     3419.95(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (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      200.0(5)
_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    -50.00  28.00   0.50    0.30    --  -40.91  22.00 156.00  156
  2  \w   -110.00 -31.00   0.50    0.30    --  -40.91 -22.00  -8.00  158
  3  \w    -95.00 -13.00   0.50    0.30    --  -40.91 136.00  18.00  164
  4  \w    -94.00 -12.00   0.50    0.30    --  -40.91 133.00-159.00  164
  5  \w    -76.00  13.00   0.50    0.30    --  -40.91 102.00 -51.00  178
  6  \w     31.00 110.00   0.50    0.30    --   40.91  22.00 156.00  158
  7  \w     13.00  95.00   0.50    0.30    --   40.91-136.00 -46.00  164
  8  \w    -13.00  76.00   0.50    0.30    --   40.91-102.00-155.00  178
  9  \w     12.00  94.00   0.50    0.30    --   40.91-133.00 131.00  164
 10  \w    -28.00  51.00   0.50    0.30    --   40.91 -22.00  -8.00  158
 11  \w     36.00 106.00   0.50    1.20    --   96.59-102.00-155.00  140
 12  \w    102.00 148.00   0.50    1.20    --   96.59 102.00 -51.00   92
 13  \w     71.00 157.00   0.50    1.20    --   96.59 136.00  18.00  172
 14  \w     98.00 150.00   0.50    1.20    --   96.59  22.00 156.00  104
 15  \w     36.00  67.00   0.50    1.20    --   96.59 -22.00  -8.00   62
 16  \w     51.00  76.00   0.50    1.20    --   96.59-133.00 131.00   50
 17  \w    -83.00 -21.00   0.50    0.30    --  -40.91 -63.00  30.00  124
 18  \w    -18.00   8.00   0.50    0.30    --   40.91   0.00-180.00   52
 19  \w    -22.00  52.00   0.50    0.30    --   40.91 -37.00 -30.00  148
 20  \w     44.00 106.00   0.50    0.30    --   40.91   0.00-180.00  124
 21  \w    111.00 137.00   0.50    1.20    --   96.59  25.00-150.00   52
 22  \w     91.00 157.00   0.50    1.20    --   96.59 117.00  90.00  132
 23  \w     84.00 150.00   0.50    1.20    --   96.59  96.00-180.00  132
 24  \w     27.00 105.00   0.50    1.20    --   96.59 -96.00 120.00  156
 25  \w     27.00  83.00   0.50    1.20    --   96.59 -96.00 150.00  112
 26  \w     66.00 102.00   0.50    1.20    --   96.59 -22.00  -8.00   72
 27  \w     89.00 130.00   0.50    1.20    --   96.59  33.00  30.00   82
 28  \w     33.00  59.00   0.50    1.20    --   96.59-145.00  60.00   52
 29  \w     88.00 121.00   0.50    1.20    --   96.59-145.00  60.00   66
 30  \w     89.00 116.00   0.50    1.20    --   96.59  25.00 -90.00   54
 31  \w     85.00 111.00   0.50    1.20    --   96.59  96.00  90.00   52
 32  \w    121.00 147.00   0.50    1.20    --   96.59  96.00  90.00   52
 33  \w    125.00 151.00   0.50    1.20    --   96.59  33.00-120.00   52
 34  \w    115.00 140.00   0.50    1.20    --   96.59  25.00-180.00   50
 35  \w    107.00 157.00   0.50    1.20    --   96.59 117.00   0.00  100
 36  \w     34.00  96.00   0.50    1.20    --   96.59 -42.00 150.00  124
;
_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  0.0708
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25119
_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         68.466
_diffrn_reflns_theta_min         3.711
_exptl_absorpt_coefficient_mu    12.336
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.923
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.110
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0878P)^2^+0.7349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5448
_reflns_number_total             6259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00425b2.cif
_cod_data_source_block           uh105-200k
_cod_depositor_comments
'Adding full bibliography for 7246861--7246867.cif.'
_cod_database_code               7246862
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.372
_shelx_estimated_absorpt_t_min   0.031
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C15A
 1.54 with sigma of 0.02
 C14-C15B
 1.54 with sigma of 0.02
 C15A-C16A
 1.54 with sigma of 0.02
 C15B-C16B
 1.54 with sigma of 0.02
 C33-Cl2B
 1.75 with sigma of 0.02
 Cl1A-C33
 1.75 with sigma of 0.02
 C33-Cl2A
 1.75 with sigma of 0.02
 Cl1B-C33
 1.75 with sigma of 0.02
 C14-C15B \\sim C14-C15A
 with sigma of 0.02
 C15B-C16B \\sim C15A-C16A
 with sigma of 0.02
 C33-Cl2A \\sim C33-Cl2B
 with sigma of 0.02
 C33-Cl1A \\sim C33-Cl1B
 with sigma of 0.02
3. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) C15B(0.5) H15A(0.5)
 H15B(0.5) C16B(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C15A(0.5) H15C(0.5)
 H15D(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) H33A(0.45) H33B(0.45)
 H33C(0.55) H33D(0.55) Cl1A(0.45) Cl2A(0.45) Cl1B(0.55) Cl2B(0.55)
4.a Ternary CH refined with riding coordinates:
 N4(H4), N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C14(H14C,H14D), C15B(H15A,H15B),
 C15A(H15C,H15D), C33(H33A,H33B), C33(H33C,H33D)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C2(H2A),
  C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11)
4.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C16B(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              94672
_shelx_hkl_checksum              48266
_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
;