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_4133893
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.744(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0292(4)
_cell_length_b                   36.0119(9)
_cell_length_c                   16.3147(13)
_cell_measurement_reflns_used    5447
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      24.6570
_cell_measurement_theta_min      3.2550
_cell_volume                     7435.8(7)
_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_environment      air
_diffrn_ambient_temperature      300(1)
_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    -40.00  19.00   0.50   30.00    --  -26.22  55.00  56.84  118
  2  \w     -7.00  20.00   0.50   30.00    --  -26.22  77.00-150.00   54
  3  \w    -98.00   2.00   0.50   30.00    --  -26.22 -57.00-120.00  200
  4  \w    -42.00  67.00   0.50   30.00    --   28.10 -38.00  90.00  218
  5  \w     -3.00  49.00   0.50   30.00    --   28.10  77.00  90.00  104
;
_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      0.0480943000
_diffrn_orient_matrix_UB_12      0.0051819000
_diffrn_orient_matrix_UB_13      0.0282837000
_diffrn_orient_matrix_UB_21      0.0214958000
_diffrn_orient_matrix_UB_22      0.0046550000
_diffrn_orient_matrix_UB_23      -0.0347427000
_diffrn_orient_matrix_UB_31      -0.0190246000
_diffrn_orient_matrix_UB_32      0.0184145000
_diffrn_orient_matrix_UB_33      0.0008579000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.1121
_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       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.839
_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            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.155
_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) ...  2915 Ang^3
N: Electron Count Voids / Cell =    733 (i.e. around 180e- 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         0.935
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         13080
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0745P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6753
_reflns_number_total             13080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10584_si_001.cif
_cod_data_source_block           1c
_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               4133893
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C49 H35 B Dy F13 N11 P S2'
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 P1-F10 = P1-F10A = P1-F9 = P1-F12 = P1-F12A = P1-F8 = P1-F8A = P1-F11 = P1-
 F13 = P1-F13A
 1.5 with sigma of 0.01
 C9-C17
 1.4 with sigma of 0.01
 F4-C13 = F5A-C13
 1.3 with sigma of 0.01
 C17A-C10A = C18-C17 = C9-C10
 1.55 with sigma of 0.01
 C9A-C18A
 1.55 with sigma of 0.01
 C9A-C17A
 1.4 with sigma of 0.01
 F4A-C13
 1.4 with sigma of 0.01
 F13-F8
 2.2 with sigma of 0.01
 F12-F10
 2.2 with sigma of 0.01
 F8-F12
 2.2 with sigma of 0.01
 F9-F12
 2.2 with sigma of 0.01
 F13-F11
 2.2 with sigma of 0.01
 F13A-F8A
 2.2 with sigma of 0.01
 F13A-F10A
 2.2 with sigma of 0.01
 F13A-F11
 2.2 with sigma of 0.01
 F9-F12A
 2.2 with sigma of 0.01
 F2-F3
 2.2 with sigma of 0.01
 C13-F6
 2.2 with sigma of 0.01
 F4-F5
 2.2 with sigma of 0.01
 F7-F6
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F9) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq,
Uanis(F12A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F10A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C17A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C10) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F4A) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F8A) = Uanis(F10A) = Uanis(F12) = Uanis(F12A) = Uanis(F8) = Uanis(F13) =
Uanis(F13A) = Uanis(F10)
Uanis(F6A) = Uanis(F6)
Uanis(C17A) = Uanis(C9A)
Uanis(F5A) = Uanis(F4A)
Uanis(F4) = Uanis(F5)
Uanis(C18A) = Uanis(C18)
Uanis(C10) = Uanis(C10A)
4. Others
 Sof(F10)=Sof(F8)=Sof(F13)=Sof(F12)=1-FVAR(1)
 Sof(F13A)=Sof(F10A)=Sof(F12A)=Sof(F8A)=FVAR(1)
 Sof(F4A)=Sof(F7A)=Sof(F6A)=Sof(F5A)=1-FVAR(2)
 Sof(F5)=Sof(F7)=Sof(F4)=Sof(F6)=FVAR(2)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C9)=Sof(C17)=1-FVAR(3)
 Sof(C17A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C9A)=FVAR(3)
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:
 C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C10A(H10D,H10E,H10F), C18A(H18D,
 H18E,H18F)
;
_shelx_res_checksum              96690
_shelx_hkl_checksum              16991
_shelx_fab_checksum              3176
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.820