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_7246864
_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, C3 H6 O'
_chemical_formula_sum            'C35 H44 Fe I N4 O3'
_chemical_formula_weight         751.49
_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             2020-05-12
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2023-04-27 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.22140(10)
_cell_length_b                   12.68900(10)
_cell_length_c                   23.7424(2)
_cell_measurement_reflns_used    24927
_cell_measurement_temperature    150.0(5)
_cell_measurement_theta_max      68.3730
_cell_measurement_theta_min      3.4680
_cell_volume                     3380.64(5)
_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-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_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   -114.00 -17.00   0.50    0.50    --  -40.91 -11.00  91.00  194
  2  \w    -87.00  -3.00   0.50    0.50    --  -40.91 121.00  82.00  168
  3  \w    -64.00  33.00   0.50    0.50    --  -40.91  11.00 -96.00  194
  4  \w    -40.00  -8.00   0.50    0.50    --  -40.91 122.00  -9.00   64
  5  \w    -21.00  32.00   0.50    0.50    --   40.91 -11.00  91.00  106
  6  \w     16.00  86.00   0.50    0.50    --   40.91-122.00 -91.00  140
  7  \w     57.00  82.00   0.50    0.50    --   40.91-121.00  -1.00   50
  8  \w     49.00  81.00   0.50    0.50    --   40.91  11.00 -96.00   64
  9  \w     40.00  65.00   0.50    0.50    --   40.91 -11.00  91.00   50
 10  \w     55.00 109.00   0.50    1.60    --   96.59-121.00  -1.00  108
 11  \w     86.00 119.00   0.50    1.60    --   96.59 121.00  82.00   66
 12  \w     74.00 127.00   0.50    1.60    --   96.59-151.00 107.00  106
 13  \w     23.00 114.00   0.50    1.60    --   96.59 -11.00  91.00  182
 14  \w     82.00 116.00   0.50    1.60    --   96.59  11.00 -96.00   68
 15  \w     79.00 110.00   0.50    1.60    --   96.59 151.00 151.00   62
 16  \w    -46.00 -21.00   0.50    0.50    --  -40.91 153.00-118.00   50
 17  \w    -89.00 -64.00   0.50    0.50    --  -40.91 153.00-118.00   50
 18  \w     29.00 105.00   0.50    0.50    --   40.91  37.00   0.00  152
 19  \w     57.00  82.00   0.50    1.60    --   96.59-153.00-160.00   50
 20  \w     30.00 105.00   0.50    1.60    --   96.59 -25.00   0.00  150
 21  \w     33.00 117.00   0.50    1.60    --   96.59 -68.00-150.00  168
 22  \w     77.00 107.00   0.50    1.60    --   96.59-117.00-150.00   60
 23  \w     31.00 106.00   0.50    1.60    --   96.59 -33.00 -90.00  150
 24  \w     68.00 118.00   0.50    1.60    --   96.59 151.00 151.00  100
 25  \w     52.00  77.00   0.50    0.50    --   40.91-104.00 -30.00   50
 26  \w    -12.00  14.00   0.50    0.50    --   40.91-104.00 -30.00   52
 27  \w     62.00 111.00   0.50    1.60    --   96.59 -59.00 -90.00   98
 28  \w     83.00 122.00   0.50    1.60    --   96.59-145.00 -60.00   78
 29  \w     36.00  61.00   0.50    1.60    --   96.59 -86.00 -90.00   50
 30  \w     92.00 118.00   0.50    1.60    --   96.59 -86.00 -90.00   52
 31  \w    132.00 157.00   0.50    1.60    --   96.59 117.00 150.00   50
 32  \w     87.00 113.00   0.50    1.60    --   96.59 117.00 150.00   52
 33  \w    113.00 139.00   0.50    1.60    --   96.59  25.00 -60.00   52
 34  \w     46.00  76.00   0.50    1.60    --   96.59-145.00 -60.00   60
 35  \w     33.00  59.00   0.50    1.60    --   96.59 -59.00 -90.00   52
 36  \w     83.00 109.00   0.50    1.60    --   96.59-117.00 -30.00   52
 37  \w     35.00 108.00   0.50    1.60    --   96.59 -42.00  90.00  146
 38  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00-180.00  166
 39  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00  30.00  166
 40  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00-150.00  166
 41  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00 -90.00  166
 42  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00 -30.00  166
 43  \w    -53.00  23.00   0.50    0.50    --  -40.91  37.00 -60.00  152
 44  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00  90.00  166
 45  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00 120.00  166
 46  \w    -61.00  23.00   0.50    0.50    --  -40.91  63.00 120.00  168
 47  \w    -97.00 -14.00   0.50    0.50    --  -40.91 138.00 120.00  166
 48  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00  60.00  166
 49  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00 -60.00  166
 50  \w   -104.00 -21.00   0.50    0.50    --  -40.91 -63.00   0.00  166
 51  \w     21.00 105.00   0.50    0.50    --   40.91  63.00-150.00  168
 52  \w     21.00 105.00   0.50    0.50    --   40.91  63.00 -90.00  168
 53  \w     78.00 107.00   0.50    1.60    --   96.59  59.00  60.00   58
;
_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      -0.1043854000
_diffrn_orient_matrix_UB_12      0.0767690000
_diffrn_orient_matrix_UB_13      0.0096947000
_diffrn_orient_matrix_UB_21      -0.0878577000
_diffrn_orient_matrix_UB_22      -0.0931826000
_diffrn_orient_matrix_UB_23      -0.0005525000
_diffrn_orient_matrix_UB_31      0.0150934000
_diffrn_orient_matrix_UB_32      -0.0123770000
_diffrn_orient_matrix_UB_33      0.0641878000
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0500
_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       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34357
_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         68.487
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.061
_exptl_absorpt_correction_T_max  0.534
_exptl_absorpt_correction_T_min  0.187
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6186
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+1.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             6186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00425b2.cif
_cod_data_source_block           uh114-150k
_cod_depositor_comments
'Adding full bibliography for 7246861--7246867.cif.'
_cod_database_code               7246864
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C35H44FeIN4O3
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O3, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C35, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
3.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)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              37259
_shelx_hkl_checksum              53230
_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 2.932
_oxdiff_exptl_absorpt_empirical_full_min 0.370