Hysteresis Photomodulation via Single-Crystal-to-Single-Crystal Isomerization of a Photochromic Chain of Dysprosium Single-Molecule Magnets.
Hojorat, Maher; Al Sabea, Hassan; Norel, Lucie; Bernot, Kevin; Roisnel, Thierry; Gendron, Frederic; Le Guennic, Boris; Trzop, Elzbieta; Collet, Eric; Long, Jeffrey R.; Rigaut, Stéphane; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10584

data_4133892
_publ_section_title
;
 Hysteresis Photomodulation via Single-Crystal-to-Single-Crystal
 Isomerization of a Photochromic Chain of Dysprosium Single-Molecule
 Magnets.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10584
_journal_year                    2019
_chemical_formula_moiety         'C49 H35 B Dy F7 N11 S2, F6 P'
_chemical_formula_sum            'C49 H35 B Dy F13 N11 P S2'
_chemical_formula_weight         1293.28
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.660(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8317(4)
_cell_length_b                   36.4980(9)
_cell_length_c                   16.7295(5)
_cell_measurement_reflns_used    10039
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.4910
_cell_measurement_theta_min      3.2290
_cell_volume                     7544.1(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.0
_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 0.998
_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    -78.00 -52.50   0.75   45.00    --    0.94   0.00-180.00   34
  2  \w    -60.00 -33.00   0.75   60.00    --  -32.81 178.00 150.00   36
  3  \w     48.00 120.00   0.75   60.00    --   34.68 178.00  90.00   96
  4  \w     34.00 109.00   0.75   60.00    --   34.68  77.00  30.00  100
  5  \w    -24.00 112.50   0.75   60.00    --   34.68  19.00-150.00  182
  6  \w    -78.00 -52.50   0.75   45.00    --    0.94   0.00-180.00   34
  7  \w    -60.00 -33.00   0.75   60.00    --  -32.81 178.00 150.00   36
  8  \w     48.00 120.00   0.75   60.00    --   34.68 178.00  90.00   96
  9  \w     34.00 109.00   0.75   60.00    --   34.68  77.00  30.00  100
 10  \w    -24.00 112.50   0.75   60.00    --   34.68  19.00-150.00  182
 
This is a product of crystal irradiation for ~32h with 532nm cw-laser. 
Single-crystal-to-single-crystal transformation. 
;
_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      0.0501750000
_diffrn_orient_matrix_UB_12      0.0046842000
_diffrn_orient_matrix_UB_13      0.0282833000
_diffrn_orient_matrix_UB_21      0.0213485000
_diffrn_orient_matrix_UB_22      0.0044579000
_diffrn_orient_matrix_UB_23      -0.0337193000
_diffrn_orient_matrix_UB_31      -0.0179918000
_diffrn_orient_matrix_UB_32      0.0183257000
_diffrn_orient_matrix_UB_33      0.0009880000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            69078
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.109
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82902
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
N: Total Potential Solvent Accessible Void Vol  (SOLV-Map Value) ...  3019 Ang^3
N: Electron Count Voids / Cell =    688 (i.e. around 170e- per assymetric unit)
Distribution of electron density as well knowledge about the reaction process
do not allow for accurate determination of the voids content: it may concern 
used solvents, reaction side products or products of complex decomposition. 
;
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         13253
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7127
_reflns_number_total             13253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10584_si_002.cif
_cod_data_source_block           1o
_cod_depositor_comments
;
The following automatic conversions were performed:

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

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

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4133892
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.763
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C33 = C31-C32
 1.4 with sigma of 0.01
 C41-C40 = C40-C39
 1.4 with sigma of 0.01
 F4-C13 = F4A-C13 = F5-C13 = F5A-C13
 1.35 with sigma of 0.01
 C14-C13 \\sim C13-C12
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F12) \\sim
Ueq, Uanis(F5A) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(F3) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(F4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F13)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(F5)=Sof(F4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C2(H2), C22(H22), C1(H1), C19(H19), C21(H21), C41(H41), C34(H34),
 C40(H40), C25(H25), C4(H4), C5(H5), C35(H35), C49(H49), C37(H37), C33(H33),
 C45(H45), C29(H29), C36(H36), C24(H24), C26(H26), C32(H32), C43(H43), C48(H48),
  C44(H44), C42(H42), C28(H28), C27(H27)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              16030
_shelx_hkl_checksum              52702
_shelx_fab_checksum              64338
_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 1.162
_oxdiff_exptl_absorpt_empirical_full_min 0.842