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_7246863
_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 H Cl3'
_chemical_formula_sum            'C33 H39 Cl3 Fe I N4 O2'
_chemical_formula_weight         812.78
_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             2023-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-18 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.8489(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.47081(14)
_cell_length_b                   12.93413(16)
_cell_length_c                   23.8498(3)
_cell_measurement_reflns_used    15999
_cell_measurement_temperature    200.0(5)
_cell_measurement_theta_max      68.4540
_cell_measurement_theta_min      1.9000
_cell_volume                     3534.10(8)
_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      200.0(5)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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    -57.00  22.00   0.50    0.30    --  -40.91  50.00 169.00  158
  2  \w   -104.00 -25.00   0.50    0.30    --  -40.91 -50.00  22.00  158
  3  \w     25.00 104.00   0.50    0.30    --   40.91  50.00 169.00  158
  4  \w     34.00 113.00   0.50    1.20    --   96.59 -50.00  22.00  158
  5  \w     81.00 157.00   0.50    1.20    --   96.59  50.00 169.00  152
  6  \w   -104.00 -21.00   0.50    0.30    --  -40.91 -63.00 -30.00  166
  7  \w    -57.00  22.00   0.50    0.30    --  -40.91  50.00  60.00  158
  8  \w   -105.00 -29.00   0.50    0.30    --  -40.91 -37.00-120.00  152
  9  \w    -22.00  57.00   0.50    0.30    --   40.91 -50.00-150.00  158
 10  \w    -27.00  50.00   0.50    0.30    --   40.91 -25.00-120.00  154
 11  \w    -23.00  53.00   0.50    0.30    --   40.91 -37.00  30.00  152
 12  \w    -22.00  57.00   0.50    0.30    --   40.91 -50.00 120.00  158
 13  \w    -22.00  57.00   0.50    0.30    --   40.91 -50.00  22.00  158
 14  \w     33.00 115.00   0.50    1.20    --   96.59 -59.00-120.00  164
 15  \w     67.00 157.00   0.50    1.20    --   96.59 144.00  60.00  180
 16  \w     88.00 157.00   0.50    1.20    --   96.59  25.00 -90.00  138
 17  \w     84.00 157.00   0.50    1.20    --   96.59  96.00-120.00  146
 18  \w     31.00 106.00   0.50    1.20    --   96.59 -33.00-180.00  150
 19  \w     78.00 157.00   0.50    1.20    --   96.59  59.00  90.00  158
 20  \w     31.00 106.00   0.50    1.20    --   96.59 -33.00 -90.00  150
 21  \w     83.00 157.00   0.50    1.20    --   96.59  77.00 120.00  148
 22  \w     88.00 157.00   0.50    1.20    --   96.59  25.00 -30.00  138
 23  \w     83.00 157.00   0.50    1.20    --   96.59  77.00-180.00  148
 24  \w     32.00 109.00   0.50    1.20    --   96.59-117.00 -60.00  154
 25  \w     88.00 157.00   0.50    1.20    --   96.59  25.00-180.00  138
 26  \w     97.00 149.00   0.50    1.20    --   96.59  25.00  30.00  104
 27  \w     38.00 103.00   0.50    1.20    --   96.59 -96.00  60.00  130
 28  \w     36.00  87.00   0.50    1.20    --   96.59 -96.00  30.00  102
;
_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  0.0919
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27434
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.686
_diffrn_reflns_theta_min         3.711
_exptl_absorpt_coefficient_mu    12.644
_exptl_absorpt_correction_T_max  0.442
_exptl_absorpt_correction_T_min  0.134
_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    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6473
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1008P)^2^+0.0913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             6473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00425b2.cif
_cod_data_source_block           uh109-200k
_cod_depositor_comments
'Adding full bibliography for 7246861--7246867.cif.'
_cod_original_cell_volume        3534.10(7)
_cod_database_code               7246863
_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, 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-C15 \\sim C14-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C14-C16 \\sim C14-C16A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C15A, C16A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C14(H14C,H14D), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C15(H15A,H15B),
 C15A(H15C,H15D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C18(H18), C19(H19),
  C21(H21), C22(H22), C23(H23), C24(H24), C27(H27)
5.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              89338
_shelx_hkl_checksum              21501
_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
;