Photoinduced reversible spin-state switching of an Fe <sup>III</sup> complex assisted by a halogen-bonded supramolecular network
Jeon, Ie-Rang; Mathonière, Corine; Clérac, Rodolphe; Rouzières, Mathieu; Jeannin, Olivier; Trzop, Elzbieta; Collet, Eric; Fourmigué, Marc; Chemical Communications 53 (2017) 10283–10286; doi:10.1039/C7CC03797J

data_1546820
_publ_section_title
;
 Photoinduced reversible spin-state switching of an Fe <sup>III</sup>
 complex assisted by a halogen-bonded supramolecular network
;
_journal_issue                   74
_journal_name_full               'Chemical Communications'
_journal_page_first              10283
_journal_page_last               10286
_journal_paper_doi               10.1039/C7CC03797J
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 F3 I3, I, C32 H22 Fe N4 O2'
_chemical_formula_sum            'C38 H22 F3 Fe I4 N4 O2'
_chemical_formula_weight         1187.04
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-06-15 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7237(2)
_cell_length_b                   22.9833(2)
_cell_length_c                   19.4485(2)
_cell_measurement_reflns_used    13592
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.9350
_cell_measurement_theta_min      3.3200
_cell_volume                     7129.98(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury3.9 (2016)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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     10.00 101.00   1.00   25.00    --   32.27  57.00   0.00   91
  2  \w      9.00 103.00   1.00   25.00    --   32.27  57.00  90.00   94
  3  \w    -28.00   2.00   1.00   25.00    --   32.27 125.00-132.09   30
  4  \w     10.00 103.00   1.00   25.00    --   32.27  57.00 -60.00   93
  5  \w    -29.00   1.00   1.00   25.00    --   32.27 128.00  22.02   30
  6  \w      1.00  69.00   1.00   25.00    --   32.27  38.00 -90.00   68
  7  \w    -23.00  73.00   1.00   25.00    --   32.27 -99.00-180.00   96
  8  \w    -22.00  74.00   1.00   25.00    --   32.27 -99.00 -30.00   96
  9  \w    -39.00  48.00   1.00   25.00    --   32.27 -77.00  90.00   87
 10  \w    -38.00  53.00   1.00   25.00    --   32.27 -57.00   0.00   91
 11  \w      6.00 103.00   1.00   25.00    --   32.27  68.00 133.00   97
 12  \w    -36.00  45.00   1.00   25.00    --   32.27 -57.00-150.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046585000
_diffrn_orient_matrix_UB_12      0.0294013000
_diffrn_orient_matrix_UB_13      -0.0116056000
_diffrn_orient_matrix_UB_21      -0.0374579000
_diffrn_orient_matrix_UB_22      -0.0073279000
_diffrn_orient_matrix_UB_23      -0.0273167000
_diffrn_orient_matrix_UB_31      -0.0235101000
_diffrn_orient_matrix_UB_32      0.0058468000
_diffrn_orient_matrix_UB_33      0.0241055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60010
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.945
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            brown
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 5066 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         15538
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0330
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12446
_reflns_number_total             15538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03797j2.cif
_cod_data_source_block           Feqsal100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1546820
_chemical_oxdiff_formula         'C38 H22 F3 Fe I4 N4 O2'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44