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_4128802
_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                 117.852(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8192(11)
_cell_length_b                   15.8059(8)
_cell_length_c                   17.0759(11)
_cell_measurement_reflns_used    6430
_cell_measurement_temperature    25
_cell_measurement_theta_max      29.3160
_cell_measurement_theta_min      2.5580
_cell_volume                     4013.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30t (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30t (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30t (Rigaku OD, 2017)'
_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      25
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_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   14.00    --   10.00  45.00   0.00  360
  2  \w    -80.00 100.00   0.50   14.00    --   10.00  45.00  90.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-Custom'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0748
_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       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34920
_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         25.349
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30t (Rigaku Oxford Diffraction, 2017)
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    1.832
_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         2.591
_refine_diff_density_min         -2.216
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0349P)^2^+30.4060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5060
_reflns_number_total             7345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07204_si_005.cif
_cod_data_source_block           '[1Cl](As)_25K_Light'
_cod_database_code               4128802
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 As2-F8 \\sim As3-F9 \\sim As2-F10 \\sim As2-F12 \\sim As3-F13 \\sim As2-F14
\\sim As3-F15 \\sim As2-F16 ~
 As2-F17 \\sim As3-F11 \\sim As3-F7 \\sim As3-F18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F16 \\sim As2 \\sim F12 \\sim F14 \\sim F10 \\sim F17 \\sim F8: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
F15 \\sim As3 \\sim F18 \\sim F13 \\sim F11 \\sim F7 \\sim F9: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C28 \\sim C26 \\sim C25 \\sim N8 \\sim C29: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F16, As2, F17, F12, F8, F10, F14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F15, As3, F7, F13, F11, F18, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, N8, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F15)=Sof(F7)=Sof(As3)=Sof(F13)=Sof(F11)=Sof(F18)=Sof(F9)=1-FVAR(1)
 Sof(As2)=Sof(F17)=Sof(F16)=Sof(F12)=Sof(F8)=Sof(F10)=Sof(F14)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N7(H7), N3(H3), C32(H32), C8(H8), C3(H3a), C4(H4), C33(H33), C2(H2), C1(H1),
 C14(H14), C9(H9), C26(H26), C10(H10), C34(H34), C16(H16), C11(H11), C17(H17),
 C29(H29), C35(H35), C19(H19), C15(H15), C22(H22), C20(H20), C21(H21), C27(H27),
  C28(H28)
;
_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
;