Bidirectional photoswitchability in an iron(iii) spin crossover complex: symmetry-breaking and solvent effects.
Díaz-Torres, Raúl; Chastanet, Guillaume; Collet, Eric; Trzop, Elzbieta; Harding, Phimphaka; Harding, David J.; Chemical science 14 (2023) 7185–7191; doi:10.1039/d3sc01495a

data_1569262
_publ_section_title
;
 Bidirectional photoswitchability in an iron(iii) spin crossover complex:
 symmetry-breaking and solvent effects.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7185
_journal_page_last               7191
_journal_paper_doi               10.1039/d3sc01495a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C32 H20 Fe I2 N4 O2, N O3, 2(C H4 O)'
_chemical_formula_sum            'C34 H28 Fe I2 N5 O7'
_chemical_formula_weight         928.26
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_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             2020-04-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                80.540(5)
_cell_angle_beta                 69.855(5)
_cell_angle_gamma                69.795(7)
_cell_formula_units_Z            2
_cell_length_a                   12.0079(9)
_cell_length_b                   12.4717(10)
_cell_length_c                   12.8977(5)
_cell_measurement_reflns_used    17300
_cell_measurement_temperature    300.0(2)
_cell_measurement_theta_max      68.4160
_cell_measurement_theta_min      3.6160
_cell_volume                     1699.5(2)
_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 1.3-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      300.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_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   -110.00 -31.00   0.50    1.00    --  -40.91 -22.00  48.00  158
  2  \w    -28.00  51.00   0.50    1.00    --   40.91 -22.00  48.00  158
  3  \w     31.00 110.00   0.50    1.00    --   40.91  22.00-145.00  158
  4  \w     28.00 106.00   0.50    3.00    --   96.59 -22.00  48.00  156
  5  \w     87.00 157.00   0.50    3.00    --   96.59  22.00-145.00  140
  6  \w    -50.00  28.00   0.50    1.00    --  -40.91  22.00-145.00  156
  7  \w    -97.00 -14.00   0.50    1.00    --  -40.91 138.00-180.00  166
  8  \w    -66.00  24.00   0.50    1.00    --  -40.91  77.00  90.00  180
  9  \w    -77.00  14.00   0.50    1.00    --  -40.91 104.00 120.00  182
 10  \w    -50.00  27.00   0.50    1.00    --  -40.91  25.00  90.00  154
 11  \w    -57.00  22.00   0.50    1.00    --  -40.91  50.00 -30.00  158
 12  \w    -53.00  23.00   0.50    1.00    --  -40.91  37.00 -30.00  152
 13  \w     29.00 105.00   0.50    1.00    --   40.91  37.00 -90.00  152
 14  \w    -32.00  63.00   0.50    1.00    --   40.91 -12.00 -90.00  190
 15  \w     15.00  42.00   0.50    1.00    --   40.91  81.00  48.42   54
 16  \w     14.00  97.00   0.50    1.00    --   40.91-138.00-120.00  166
 17  \w     16.00  42.00   0.50    1.00    --   40.91  79.00   6.21   52
 18  \w     16.00  42.00   0.50    1.00    --   40.91  78.00 -36.29   52
 19  \w     34.00 113.00   0.50    3.00    --   96.59 -50.00-150.00  158
 20  \w     31.00 106.00   0.50    3.00    --   96.59 -33.00 -60.00  150
 21  \w     33.00 126.00   0.50    3.00    --   96.59-144.00  90.00  186
 22  \w     32.00 122.00   0.50    3.00    --   96.59 -77.00 -30.00  180
 23  \w     27.00 105.00   0.50    3.00    --   96.59 -96.00  90.00  156
 24  \w     33.00 126.00   0.50    3.00    --   96.59-144.00 -90.00  186
 25  \w     33.00 118.00   0.50    3.00    --   96.59 -68.00  90.00  170
 26  \w     31.00 124.00   0.50    3.00    --   96.59 -86.00-120.00  186
 27  \w     32.00 109.00   0.50    3.00    --   96.59-117.00  90.00  154
 28  \w     88.00 157.00   0.50    3.00    --   96.59  25.00  90.00  138
 29  \w     83.00 157.00   0.50    3.00    --   96.59  17.00 -30.00  148
 30  \w     78.00 157.00   0.50    3.00    --   96.59  59.00  60.00  158
 31  \w     34.00 110.00   0.50    3.00    --   96.59 -42.00 120.00  152
 32  \w     32.00 109.00   0.50    3.00    --   96.59-117.00-120.00  154
 33  \w     31.00 106.00   0.50    3.00    --   96.59 -33.00-150.00  150
 34  \w     33.00 126.00   0.50    3.00    --   96.59-144.00   0.00  186
 35  \w     81.00 157.00   0.50    3.00    --   96.59 117.00 120.00  152
 36  \w     84.00 157.00   0.50    3.00    --   96.59  42.00   0.00  146
 37  \w     32.00 109.00   0.50    3.00    --   96.59-117.00-180.00  154
 38  \w     32.00 109.00   0.50    3.00    --   96.59-117.00 -90.00  154
 39  \w     27.00 105.00   0.50    3.00    --   96.59 -96.00 120.00  156
 40  \w     34.00 110.00   0.50    3.00    --   96.59 -42.00  30.00  152
 41  \w     81.00 157.00   0.50    3.00    --   96.59  50.00-120.00  152
 42  \w   -105.00 -29.00   0.50    1.00    --  -40.91 -37.00 120.00  152
 43  \w   -104.00 -23.00   0.50    1.00    --  -40.91 -54.00  88.85  162
 44  \w   -104.00 -21.00   0.50    1.00    --  -40.91 -63.00   0.00  166
 45  \w   -104.00 -21.00   0.50    1.00    --  -40.91 -63.00 -90.00  166
 46  \w   -104.00 -21.00   0.50    1.00    --  -40.91 -63.00  30.00  166
 47  \w   -104.00 -21.00   0.50    1.00    --  -40.91 -63.00 -60.00  166
 48  \w   -104.00 -21.00   0.50    1.00    --  -40.91 -63.00-180.00  166
 49  \w     16.00  42.00   0.50    1.00    --   40.91  80.00-137.27   52
 50  \w     15.00  42.00   0.50    1.00    --   40.91  81.00  25.72   54
 51  \w     16.00  42.00   0.50    1.00    --   40.91  79.00 133.45   52
 52  \w     16.00  42.00   0.50    1.00    --   40.91  79.00-153.74   52
 53  \w     16.00  42.00   0.50    1.00    --   40.91  76.00 103.23   52
 54  \w     15.00  42.00   0.50    1.00    --   40.91  82.00 159.04   54
 55  \w     16.00  42.00   0.50    1.00    --   40.91  79.00 -73.73   52
 56  \w     16.00  42.00   0.50    1.00    --   40.91  79.00-101.35   52
 57  \w     79.00 157.00   0.50    3.00    --   96.59  57.00  28.20  156
 58  \w     78.00 157.00   0.50    3.00    --   96.59  59.00 120.00  158
;
_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      0.1159361000
_diffrn_orient_matrix_UB_12      -0.1043537000
_diffrn_orient_matrix_UB_13      -0.0401209000
_diffrn_orient_matrix_UB_21      -0.0850935000
_diffrn_orient_matrix_UB_22      -0.0718491000
_diffrn_orient_matrix_UB_23      0.0093800000
_diffrn_orient_matrix_UB_31      0.0020203000
_diffrn_orient_matrix_UB_32      0.0363203000
_diffrn_orient_matrix_UB_33      -0.1205506000
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25766
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.570
_diffrn_reflns_theta_min         3.655
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.295
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (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 black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             910
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.609
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0825P)^2^+5.5550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5491
_reflns_number_total             6209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01495a2.cif
_cod_data_source_block           rdt54b-300k
_cod_depositor_comments
'Adding full bibliography for 1569262--1569271.cif.'
_cod_database_code               1569262
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C34H28FeI2N5O7
_shelx_estimated_absorpt_t_max   0.427
_shelx_estimated_absorpt_t_min   0.032
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26),
  C28(H28), C30(H30), C31(H31)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O7(H7A)
;
_shelx_res_checksum              55385
_shelx_hkl_checksum              17161
_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 2.231
_oxdiff_exptl_absorpt_empirical_full_min 0.455