Observation of Proton Transfer Coupled Spin Transition and Trapping of Photoinduced Metastable Proton Transfer State in an Fe(II) Complex.
Nakanishi, Takumi; Hori, Yuta; Sato, Hiroyasu; Wu, Shu-Qi; Okazawa, Atsushi; Kojima, Norimichi; Yamamoto, Takashi; Einaga, Yasuaki; Hayami, Shinya; Horie, Yusuke; Okajima, Hajime; Sakamoto, Akira; Shiota, Yoshihito; Yoshizawa, Kazunari; Sato, Osamu; Journal of the American Chemical Society 141 (2019) 14384–14393; doi:10.1021/jacs.9b07204

data_4128804
_publ_section_title
;
 Observation of Proton Transfer Coupled Spin Transition and Trapping of
 Photoinduced Metastable Proton Transfer State in an Fe(II) Complex.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14384
_journal_page_last               14393
_journal_paper_doi               10.1021/jacs.9b07204
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '2(As F6), C36 H26 Cl2 Fe N8 O2'
_chemical_formula_sum            'C36 H26 As2 Cl2 F12 Fe N8 O2'
_chemical_formula_weight         1107.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.615(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4896(6)
_cell_length_b                   16.0053(4)
_cell_length_c                   16.6301(6)
_cell_measurement_reflns_used    11266
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.7490
_cell_measurement_theta_min      2.5380
_cell_volume                     3924.0(3)
_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    '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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_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    -80.00 100.00   0.50   12.00    --   10.00  45.00   0.00  360
  2  \w    -80.00 100.00   0.50   12.00    --   10.00  45.00  90.00  360
  3  \w      0.00   0.50   0.50   12.00    --   10.00  45.00  90.00    1
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0450018000
_diffrn_orient_matrix_UB_12      -0.0156861000
_diffrn_orient_matrix_UB_13      0.0212910000
_diffrn_orient_matrix_UB_21      -0.0023922000
_diffrn_orient_matrix_UB_22      -0.0020559000
_diffrn_orient_matrix_UB_23      0.0414677000
_diffrn_orient_matrix_UB_31      -0.0168841000
_diffrn_orient_matrix_UB_32      -0.0414128000
_diffrn_orient_matrix_UB_33      -0.0100559000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38574
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.341
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.299
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.874
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0375P)^2^+9.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6615
_reflns_number_total             8021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07204_si_004.cif
_cod_data_source_block           '[1Cl](As)_25K'
_cod_database_code               4128804
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Fe C H N O F Cl As'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H2), N4(H1), C26(H00W), C28(H010), C8(H014), C35(H016), C22(H017),
 C33(H018), C27(H019), C34(H01B), C32(H01C), C9(H01D), C29(H01E), C11(H01F),
 C19(H01G), C21(H01H), C14(H01I), C1(H01J), C17(H01K), C15(H01L), C2(H01M),
 C10(H01N), C3(H01O), C4(H01P), C20(H01Q), C16(H01R)
;
_shelx_res_checksum              69520
_shelx_hkl_checksum              11406
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.150
_oxdiff_exptl_absorpt_empirical_full_min 0.613