Very Long-Lived Photogenerated High-Spin Phase of a Multistable Spin-Crossover Molecular Material.
Delgado, Teresa; Tissot, Antoine; Guénée, Laure; Hauser, Andreas; Valverde-Muñoz, Francisco Javier; Seredyuk, Maksym; Real, José Antonio; Pillet, Sébastien; Bendeif, El-Eulmi; Besnard, Céline; Journal of the American Chemical Society 140 (2018) 12870–12876; doi:10.1021/jacs.8b06042

data_4132752
_publ_section_title
;
 Very Long-Lived Photogenerated High-Spin Phase of a Multistable
 Spin-Crossover Molecular Material.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12870
_journal_page_last               12876
_journal_paper_doi               10.1021/jacs.8b06042
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C30 H48 Fe N10, 2(F6 P)'
_chemical_formula_sum            'C30 H48 F12 Fe N10 P2'
_chemical_formula_weight         894.57
_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
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.390(6)
_cell_angle_beta                 101.321(7)
_cell_angle_gamma                98.577(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2022(7)
_cell_length_b                   10.1887(7)
_cell_length_c                   21.8917(18)
_cell_measurement_reflns_used    2721
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.0880
_cell_measurement_theta_min      2.2060
_cell_volume                     1987.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (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)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.499
_diffrn_measured_fraction_theta_max 0.484
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f      0.00 360.00   1.00    0.80   0.00   0.00   0.00    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0629844000
_diffrn_orient_matrix_UB_12      -0.0335065000
_diffrn_orient_matrix_UB_13      0.0010744000
_diffrn_orient_matrix_UB_21      -0.0056460000
_diffrn_orient_matrix_UB_22      0.0059910000
_diffrn_orient_matrix_UB_23      -0.0326917000
_diffrn_orient_matrix_UB_31      0.0488537000
_diffrn_orient_matrix_UB_32      0.0620689000
_diffrn_orient_matrix_UB_33      0.0058272000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.7121
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.499
_diffrn_reflns_Laue_measured_fraction_max 0.484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6961
_diffrn_reflns_point_group_measured_fraction_full 0.499
_diffrn_reflns_point_group_measured_fraction_max 0.484
_diffrn_reflns_theta_full        25.294
_diffrn_reflns_theta_max         25.586
_diffrn_reflns_theta_min         1.904
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2523
_reflns_number_total             3598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06042_si_002.cif
_cod_data_source_block           1848631_LIESST_90K
_cod_database_code               4132752
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 H48 F12 Fe N10 P2'
_reflns_odcompleteness_completeness 47.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.77
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C17B = N7-C17A = C18B-C17B = C18A-C17A = C19B-C18B = C19A-C18A = C20B-C19B
 = C20A-C19A
 1.495 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17B)
Uanis(C18A) = Uanis(C18B)
Uanis(C19B) = Uanis(C19A)
Uanis(C20B) = Uanis(C20A)
4. Rigid body (RIGU) restrains
 C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C19A)=
 Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C18B)=
 Sof(H18C)=Sof(H18D)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,
 H11B), C12(H12A,H12B), C17A(H17A,H17B), C18A(H18A,H18B), C18B(H18C,H18D),
 C17B(H17C,H17D), C19B(H19A,H19B), C19A(H19C,H19D), C21(H21A,H21B), C22(H22A,
 H22B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C13(H13), C15(H15), C16(H16), C23(H23), C25(H25),
 C26(H26)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              8731
_shelx_hkl_checksum              10252
_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 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.919