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_7246867
_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         812.810
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2020-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0092(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.54644(13)
_cell_length_b                   13.04848(16)
_cell_length_c                   23.9438(3)
_cell_measurement_reflns_used    14513
_cell_measurement_temperature    295.9
_cell_measurement_theta_max      68.3500
_cell_measurement_theta_min      1.8880
_cell_volume                     3602.48(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      295.9
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9892
_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    -58.00  22.00   0.50    0.45    --  -40.91  51.00 169.00  160
  2  \w   -104.00 -24.00   0.50    0.45    --  -40.91 -51.00  23.00  160
  3  \w     24.00 104.00   0.50    0.45    --   40.91  51.00 169.00  160
  4  \w     34.00 113.00   0.50    1.80    --   96.59 -51.00  23.00  158
  5  \w     80.00 157.00   0.50    1.80    --   96.59  51.00 169.00  154
  6  \w   -109.00 -32.00   0.50    0.45    --  -40.91 -25.00  30.00  154
  7  \w    -27.00  50.00   0.50    0.45    --   40.91 -25.00-150.00  154
  8  \w    -22.00  57.00   0.50    0.45    --   40.91 -50.00-120.00  158
  9  \w     29.00 105.00   0.50    0.45    --   40.91  37.00 -90.00  152
 10  \w     19.00 114.00   0.50    0.45    --   40.91  12.00   0.00  190
 11  \w    -22.00  58.00   0.50    0.45    --   40.91 -51.00  23.00  160
 12  \w    -22.00  57.00   0.50    0.45    --   40.91 -50.00 -90.00  158
 13  \w     29.00 105.00   0.50    0.45    --   40.91  37.00 150.00  152
 14  \w    -27.00  50.00   0.50    0.45    --   40.91 -25.00 -60.00  154
 15  \w     26.00 110.00   0.50    1.80    --   96.59 -17.00 150.00  168
 16  \w     81.00 157.00   0.50    1.80    --   96.59  50.00 150.00  152
 17  \w     33.00 126.00   0.50    1.80    --   96.59-144.00 -90.00  186
 18  \w     88.00 157.00   0.50    1.80    --   96.59  25.00  30.00  138
 19  \w     81.00 157.00   0.50    1.80    --   96.59  50.00 120.00  152
 20  \w     34.00 110.00   0.50    1.80    --   96.59 -42.00 150.00  152
 21  \w     32.00 109.00   0.50    1.80    --   96.59-117.00 -30.00  154
 22  \w     87.00 157.00   0.50    1.80    --   96.59  33.00 120.00  140
 23  \w     31.00 106.00   0.50    1.80    --   96.59 -33.00 -30.00  150
 24  \w     81.00 157.00   0.50    1.80    --   96.59 117.00   0.00  152
 25  \w     34.00 113.00   0.50    1.80    --   96.59 -50.00-120.00  158
 26  \w     67.00 157.00   0.50    1.80    --   96.59   8.00 120.00  180
 27  \w   -104.00 -36.00   0.50    0.45    --  -40.91 -63.00-120.00  136
 28  \w   -104.00 -21.00   0.50    0.45    --  -40.91 -63.00 -30.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0159255000
_diffrn_orient_matrix_UB_12      -0.0078625000
_diffrn_orient_matrix_UB_13      -0.0640792000
_diffrn_orient_matrix_UB_21      0.1033835000
_diffrn_orient_matrix_UB_22      0.0732264000
_diffrn_orient_matrix_UB_23      -0.0060173000
_diffrn_orient_matrix_UB_31      0.0831217000
_diffrn_orient_matrix_UB_32      -0.0924345000
_diffrn_orient_matrix_UB_33      0.0006924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9892
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29102
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9892
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.78
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.405
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.159
_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    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1649.094
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.1327
_refine_diff_density_min         -1.1569
_refine_diff_density_rms         0.1045
_refine_ls_d_res_high            0.8270
_refine_ls_d_res_low             11.9554
_refine_ls_goodness_of_fit_ref   1.0275
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     544
_refine_ls_number_reflns         6587
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.0266
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+4.2341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                5459
_reflns_number_total             6587
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ce00425b2.cif
_cod_data_source_block           UH109-RT
_cod_depositor_comments
'Adding full bibliography for 7246861--7246867.cif.'
_cod_original_cell_volume        3602.48(7)
_cod_database_code               7246867
_chemical_oxdiff_formula         C33H39Cl3FeIN4O2
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C15B-C14
 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
 C14-C15A
 1.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C15B, C16B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15A, C16A
 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(C15B)=Sof(H15c)=Sof(H15d)=Sof(C16B)=Sof(H16d)=
 Sof(H16e)=Sof(H16f)=1-FVAR(1)
 Sof(H14a)=Sof(H14b)=Sof(C15A)=Sof(H15a)=Sof(H15b)=Sof(C16A)=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), C15A(H15a,H15b),
 C15B(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), C16A(H16a,H16b,H16c), C16B(H16d,H16e,H16f)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.176
_oxdiff_exptl_absorpt_empirical_full_min 0.489