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_1569264
_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             2018-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                80.7420(11)
_cell_angle_beta                 69.6815(13)
_cell_angle_gamma                69.7944(13)
_cell_formula_units_Z            2
_cell_length_a                   11.96519(17)
_cell_length_b                   12.45379(18)
_cell_length_c                   12.83894(17)
_cell_measurement_reflns_used    14368
_cell_measurement_temperature    240.00(10)
_cell_measurement_theta_max      68.8440
_cell_measurement_theta_min      3.6630
_cell_volume                     1681.88(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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    -81.00   9.00   0.50    2.00    --  -40.91 111.00 -59.00  180
  2  \w     80.00 157.00   0.50    8.00    --   98.15 111.00 -59.00  154
  3  \w     32.00 111.00   0.50    8.00    --   98.15-111.00-153.00  158
  4  \w   -104.00 -21.00   0.50    2.00    --  -40.91 -63.00  60.00  166
  5  \w   -104.00 -21.00   0.50    2.00    --  -40.91 -63.00-150.00  166
  6  \w    -77.00  17.00   0.50    2.00    --  -40.91 104.00  60.00  188
  7  \w     15.00 106.00   0.50    2.00    --   40.91  77.00 150.00  182
  8  \w    -16.00  77.00   0.50    2.00    --   40.91-104.00 -60.00  186
  9  \w     -9.00  81.00   0.50    2.00    --   40.91-111.00-153.00  180
 10  \w    -23.00  53.00   0.50    2.00    --   40.91 -37.00-120.00  152
 11  \w     11.00  97.00   0.50    2.00    --   40.91-138.00  60.00  172
 12  \w     29.00 105.00   0.50    2.00    --   40.91  37.00 -90.00  152
 13  \w     21.00 105.00   0.50    2.00    --   40.91  63.00 120.00  168
 14  \w     15.00 106.00   0.50    2.00    --   40.91  77.00 -60.00  182
 15  \w     29.00 105.00   0.50    2.00    --   40.91  37.00  60.00  152
 16  \w    -23.00  61.00   0.50    2.00    --   40.91 -63.00 120.00  168
 17  \w    -23.00  53.00   0.50    2.00    --   40.91 -37.00 -30.00  152
 18  \w     33.00 107.00   0.50    8.00    --   98.15 -33.00   0.00  148
 19  \w     80.00 157.00   0.50    8.00    --   98.15  59.00-180.00  154
 20  \w     33.00 107.00   0.50    8.00    --   98.15 -33.00 -90.00  148
 21  \w     80.00 157.00   0.50    8.00    --   98.15  59.00-120.00  154
 22  \w     80.00 157.00   0.50    8.00    --   98.15  59.00 -60.00  154
 23  \w     28.00 109.00   0.50    8.00    --   98.15 -96.00-150.00  162
 24  \w     34.00 113.00   0.50    8.00    --   98.15-117.00  30.00  158
 25  \w     28.00 109.00   0.50    8.00    --   98.15 -96.00  60.00  162
 26  \w     35.00 117.00   0.50    8.00    --   98.15 -59.00-180.00  164
 27  \w     80.00 157.00   0.50    8.00    --   98.15  59.00-150.00  154
 28  \w     28.00 109.00   0.50    8.00    --   98.15 -96.00  90.00  162
 29  \w     34.00 120.00   0.50    8.00    --   98.15 -68.00-150.00  172
 30  \w     34.00 113.00   0.50    8.00    --   98.15-117.00  60.00  158
 31  \w     63.00 157.00   0.50    8.00    --   98.15 144.00  60.00  188
 32  \w     34.00 113.00   0.50    8.00    --   98.15-117.00   0.00  158
 33  \w     82.00 157.00   0.50    8.00    --   98.15  50.00 -90.00  150
 34  \w     33.00 107.00   0.50    8.00    --   98.15 -33.00-180.00  148
 35  \w     34.00 120.00   0.50    8.00    --   98.15 -68.00  90.00  172
 36  \w     89.00 157.00   0.50    8.00    --   98.15  33.00-120.00  136
 37  \w     35.00 111.00   0.50    8.00    --   98.15 -42.00  30.00  152
 38  \w     77.00 157.00   0.50    8.00    --   98.15  68.00 150.00  160
 39  \w     34.00 113.00   0.50    8.00    --   98.15-117.00-180.00  158
 40  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00 -30.00  180
 41  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00 -90.00  180
 42  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00   0.00  180
 43  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00  30.00  180
 44  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00 -60.00  180
 45  \w   -105.00 -15.00   0.50    2.00    --  -40.91 -77.00-150.00  180
 46  \w   -104.00 -21.00   0.50    2.00    --  -40.91 -63.00 150.00  166
 47  \w    -63.00  32.00   0.50    2.00    --  -40.91  12.00 -60.00  190
;
_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      -0.1187553000
_diffrn_orient_matrix_UB_12      0.0304877000
_diffrn_orient_matrix_UB_13      -0.0346612000
_diffrn_orient_matrix_UB_21      0.0753703000
_diffrn_orient_matrix_UB_22      0.0246085000
_diffrn_orient_matrix_UB_23      -0.1206055000
_diffrn_orient_matrix_UB_31      0.0333389000
_diffrn_orient_matrix_UB_32      -0.1260064000
_diffrn_orient_matrix_UB_33      -0.0256989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.267
_diffrn_reflns_theta_min         3.675
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.487
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.833
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.085
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0619P)^2^+1.4214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5405
_reflns_number_total             6223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01495a2.cif
_cod_data_source_block           nut10_240k
_cod_depositor_comments
'Adding full bibliography for 1569262--1569271.cif.'
_cod_database_code               1569264
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C34H28FeI2N5O7
_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
 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:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O7(H7A)
;
_shelx_res_checksum              77225
_shelx_hkl_checksum              21412
_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 2.850
_oxdiff_exptl_absorpt_empirical_full_min 0.430