Multifunctional LnIII complexes with SMM, luminescence and MCE properties constructed using selected phosphine oxide and diketonate
Yan, Han; Che, Zi-Wei; Sun, Wen-Bin; New Journal of Chemistry 47 (2023) 140–146; doi:10.1039/D2NJ03544H

data_7062065
_publ_section_title
;
 Multifunctional LnIII complexes with SMM, luminescence and MCE properties
 constructed using selected phosphine oxide and diketonate
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              140
_journal_page_last               146
_journal_paper_doi               10.1039/D2NJ03544H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C92 H138 Dy2 O14 P2'
_chemical_formula_sum            'C92 H138 Dy2 O14 P2'
_chemical_formula_weight         1854.96
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                85.183(3)
_cell_angle_beta                 86.395(3)
_cell_angle_gamma                62.322(5)
_cell_formula_units_Z            1
_cell_length_a                   13.1963(6)
_cell_length_b                   13.9250(7)
_cell_length_c                   15.1757(5)
_cell_measurement_reflns_used    9111
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.3760
_cell_measurement_theta_min      3.5300
_cell_volume                     2459.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.832
_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     -1.00  82.00   1.00   10.97    --   16.76  38.00  90.00   83
  2  \w    -10.00  29.00   1.00   10.97    --   16.76  77.00 -90.00   39
  3  \w    -10.00  39.00   1.00   10.97    --   16.76  77.00  30.00   49
  4  \w     -7.00  26.00   1.00   10.97    --   16.76  77.00 150.00   33
  5  \w    -44.00  33.00   1.00   10.97    --   16.76 -57.00 -90.00   77
  6  \w    -29.00  -3.00   1.00   10.97    --   16.76 -77.00-120.00   26
  7  \w    -46.00  33.00   1.00   10.97    --   16.76 -57.00 150.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283098000
_diffrn_orient_matrix_UB_12      -0.0326514000
_diffrn_orient_matrix_UB_13      0.0005654000
_diffrn_orient_matrix_UB_21      0.0535998000
_diffrn_orient_matrix_UB_22      -0.0469082000
_diffrn_orient_matrix_UB_23      -0.0041892000
_diffrn_orient_matrix_UB_31      0.0034986000
_diffrn_orient_matrix_UB_32      -0.0073958000
_diffrn_orient_matrix_UB_33      0.0467312000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21198
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.354
_diffrn_reflns_theta_min         3.074
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11255
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7274
_reflns_number_total             11255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03544h2.cif
_cod_data_source_block           292_auto
_cod_depositor_comments
'Adding full bibliography for 7062065--7062070.cif.'
_cod_database_code               7062065
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.646
_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
 C22A-C21 \\sim C22-C21 \\sim C24A-C21 \\sim C24-C21 \\sim C23A-C21 \\sim
C23-C21
 with sigma of 0.02
 C40-C37 \\sim C40A-C37 \\sim C38-C37 \\sim C38A-C37 \\sim C39-C37 \\sim
C39A-C37
 with sigma of 0.02
 C45-C43 \\sim C45A-C43 \\sim C46-C43 \\sim C46A-C43 \\sim C44-C43 \\sim
C44A-C43
 with sigma of 0.02
 C33-C32 \\sim C34A-C32 \\sim C34-C32 \\sim C35A-C32 \\sim C35-C32 \\sim
C33A-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C35 \\sim C33 \\sim C34 \\sim C33A \\sim C35A \\sim C34A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C40A \\sim C39A \\sim C38A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C43 \\sim C44A \\sim C44 \\sim C46A \\sim C46 \\sim C45A \\sim C45: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C21 \\sim C23 \\sim C22 \\sim C24 \\sim C23A \\sim C24A \\sim C22A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C34, C35, C32, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C35A, C34A, C33A, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C38A, C39A, C37, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C37, C39, C40, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C45A, C46A, C44A, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C45, C46, C43, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C23A, C21, C24A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C23, C24, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(2)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(3)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(3)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(4)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C3(H3), C4(H4), C5(H5),
 C6(H6), C7(H7), C30(H30), C19(H19), C41(H41)
6.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C2(C3,C4,C5,C6,C7)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C16(H16A,H16B,
 H16C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C23(H23A,
 H23B,H23C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C),
 C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C17(H17A,H17B,H17C), C35(H35A,H35B,
 H35C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F), C34A(H34D,H34E,H34F), C40A(H40D,
 H40E,H40F), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F), C46A(H46D,H46E,H46F),
 C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              47907
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.880