Circularly Polarized Luminescence and Magneto-Optic Effect from Chiral Dy(III)-Single Molecule Magnet
Huang, Hong; Sun, Rong; Wu, Xiao-Fan; Liu, Youchao; Zhan, Jun-Zheng; Wang, Bingwu; Gao, Song; Dalton Transactions  (2023) –; doi:10.1039/D3DT00625E

data_7712950
_publ_section_title
;
 Circularly Polarized Luminescence and Magneto-Optic Effect from Chiral
 Dy(III)-Single Molecule Magnet
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00625E
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H28 Dy N5 O14 Zn'
_chemical_formula_sum            'C30 H28 Dy N5 O14 Zn'
_chemical_formula_weight         910.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.007(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0327(5)
_cell_length_b                   17.1436(7)
_cell_length_c                   22.4164(17)
_cell_measurement_reflns_used    5880
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7970
_cell_measurement_theta_min      2.2190
_cell_volume                     3445.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.847
_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  20.00   1.00    6.50    --   11.90 -57.00  90.00   60
  2  \w    -62.00  98.00   1.00    6.50    --   11.90   0.00 -60.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0732147000
_diffrn_orient_matrix_UB_12      0.0130854000
_diffrn_orient_matrix_UB_13      -0.0029922000
_diffrn_orient_matrix_UB_21      -0.0274749000
_diffrn_orient_matrix_UB_22      0.0203404000
_diffrn_orient_matrix_UB_23      -0.0266238000
_diffrn_orient_matrix_UB_31      -0.0117927000
_diffrn_orient_matrix_UB_32      0.0335815000
_diffrn_orient_matrix_UB_33      0.0172648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20354
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.666
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.520
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.008(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         12822
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0354P)^2^+5.8744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.523
_reflns_Friedel_fraction_full    0.666
_reflns_Friedel_fraction_max     0.472
_reflns_number_gt                11017
_reflns_number_total             12822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00625e2.cif
_cod_data_source_block           exp_2258
_cod_database_code               7712950
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.721
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.992(18)
 0.008(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid bond restraints
 C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
Uanis(O6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.2
Uanis(C45) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5.a Rotating group:
 O14(H14A,H14B), O4(H4A,H4B)
5.b Ternary CH refined with riding coordinates:
 C9(H9), C37(H37), C16(H16), C38(H38)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C8(H8), C7(H7), C27(H27), C47(H47), C49(H49), C6(H6), C48(H48),
 C55(H55), C45(H45), C29(H29), C28(H28), C57(H57), C15(H15), C20(H20), C18(H18),
  C56(H56), C41(H41), C36(H36), C40(H40), C44(H44), C5(H5), C21(H21), C11(H11),
 C53(H53), C43(H43), C12(H12), C42(H42), C19(H19), C34(H34), C33(H33), C13(H13),
  C32(H32), C22(H22), C14(H14), C35(H35)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30003
_shelx_hkl_checksum              37946
_shelx_fab_checksum              210
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.377
_oxdiff_exptl_absorpt_empirical_full_min 0.785