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_7062070
_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         'C51 H72 Dy O7 P'
_chemical_formula_sum            'C51 H72 Dy O7 P'
_chemical_formula_weight         990.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-12 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.401(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1425(7)
_cell_length_b                   19.2903(12)
_cell_length_c                   19.2838(9)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.3390
_cell_measurement_theta_min      3.3310
_cell_volume                     5607.9(5)
_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      298.00
_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 0.998
_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    -29.00  25.00   1.00   23.41    --  -16.68  38.00-180.00   54
  2  \w    -36.00   9.00   1.00   23.41    --  -16.68 -77.00-180.00   45
  3  \w    -38.00   9.00   1.00   23.41    --  -16.68 -77.00 -30.00   47
  4  \w     -3.00  87.00   1.00   23.41    --   16.76  19.00  60.00   90
;
_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      0.0226381000
_diffrn_orient_matrix_UB_12      -0.0211867000
_diffrn_orient_matrix_UB_13      0.0259529000
_diffrn_orient_matrix_UB_21      0.0143528000
_diffrn_orient_matrix_UB_22      0.0300193000
_diffrn_orient_matrix_UB_23      0.0191162000
_diffrn_orient_matrix_UB_31      -0.0386769000
_diffrn_orient_matrix_UB_32      -0.0012943000
_diffrn_orient_matrix_UB_33      0.0180536000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23229
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73038
_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    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         9862
_refine_ls_number_restraints     1438
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0854
_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^)+(0.1521P)^2^+14.3488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6462
_reflns_number_total             9862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03544h2.cif
_cod_data_source_block           czw-300-a_auto
_cod_depositor_comments
'Adding full bibliography for 7062065--7062070.cif.'
_cod_database_code               7062070
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H23D-C5A
 2.1 with sigma of 0.02
 C20A-C18A \\sim C19A-C18A \\sim C21A-C18A
 with sigma of 0.02
 C24A-C22A \\sim C25A-C22A \\sim C23A-C22A
 with sigma of 0.02
 C24A-C23A \\sim C25A-C23A \\sim C25A-C24A
 with sigma of 0.02
 C20A-C19A \\sim C21A-C19A \\sim C21A-C20A
 with sigma of 0.02
 C17-C15 \\sim C17-C16 \\sim C16-C15
 with sigma of 0.02
 Dy1-O4 \\sim Dy1-O5
 with sigma of 0.02
 C15A-C14A \\sim C17A-C14A \\sim C16A-C14A
 with sigma of 0.02
 C11A-C10A \\sim C13A-C10A \\sim C12A-C10A
 with sigma of 0.02
 C13A-C11A \\sim C12A-C11A \\sim C13A-C12A
 with sigma of 0.02
 C29-C26 \\sim C29A-C26 \\sim C28-C26 \\sim C28A-C26 \\sim C27-C26 \\sim
C27A-C26
 with sigma of 0.02
 C32-C30 \\sim C31A-C30 \\sim C31-C30 \\sim C32A-C30 \\sim C33-C30 \\sim
C33A-C30
 with sigma of 0.02
 P1-C46A \\sim P1-C46
 with sigma of 0.02
 P1-C40A \\sim P1-C40
 with sigma of 0.02
 P1-C34A \\sim P1-C34
 with sigma of 0.02
 P1-C35A \\sim P1-C36A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Dy1 \\sim O2A \\sim O3A \\sim C6A \\sim C5A \\sim C4A \\sim C22A \\sim C25A
\\sim C23A \\sim C24A \\sim C18A \\sim C20A \\sim C19A \\sim C21A: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
O5 \\sim O5A \\sim C1A \\sim C2A \\sim C3A \\sim C10A \\sim C11A \\sim C12A
\\sim C13A \\sim C14A \\sim C16A \\sim C15A \\sim C17A \\sim Dy1: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O2 \\sim O4 \\sim O3 \\sim O5 \\sim C18 \\sim C22 \\sim C4 \\sim C5 \\sim C6
\\sim C3 \\sim C16 \\sim C23 \\sim C2 \\sim C17 \\sim C20 \\sim C19 \\sim C25
\\sim C14 \\sim C15 \\sim C10 \\sim C1 \\sim C12 \\sim C11 \\sim C13 \\sim C24
\\sim C21: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
P1 \\sim C34 \\sim C36 \\sim C38 \\sim C35 \\sim C37 \\sim C39: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C26 \\sim C28 \\sim C29 \\sim C27:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C46 \\sim C48 \\sim C50 \\sim C51 \\sim C49 \\sim C47: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Dy1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C40 \\sim C42 \\sim C44 \\sim C45 \\sim C43 \\sim C41: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C26 \\sim C28 \\sim C29 \\sim C27 \\sim C29A \\sim C28A \\sim C27A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C31A \\sim C32A \\sim C33A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P1 \\sim C46A \\sim C48A \\sim C50A \\sim C51A \\sim C49A \\sim C47A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P1 \\sim C40A \\sim C41A \\sim C43A \\sim C45A \\sim C44A \\sim C42A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P1 \\sim C34A \\sim C35A \\sim C37A \\sim C39A \\sim C38A \\sim C36A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O2A, O3A, C6A, C5A, C4A, C18A, C20A, C19A, C21A, C22A, C24A, C25A, C23A, Dy1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O4A, C10A, C13A, O5A, C12A, C3A, C15A, C16A, C1A, C2A, C11A, C17A, C14A, Dy1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O2, O4, O3, O5, C18, C22, C4, C5, C6, C3, C16, C23, C2, C21, C17, C20, C19,
 C25, C14, C15, C10, C1, C12, C11, C13, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C34, C36, C38, C39, C37, C35, P1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C26, C28, C29, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C30, C31, C32, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C43, C41, C40, C42, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Dy1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C46, C48, C50, C51, C49, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C29A, C26, C28A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33A, C31A, C32A, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33, C31, C32, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C29, C28, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1, C46A, C48A, C50A, C51A, C49A, C47A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1, C40A, C41A, C43A, C45A, C44A, C42A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1, C34A, C35A, C37A, C39A, C38A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=
 Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(2)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(2)
 Sof(C46A)=Sof(C48A)=Sof(H48A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=
 Sof(C49A)=Sof(H49A)=Sof(C47A)=Sof(H47A)=1-FVAR(3)
 Sof(C46)=Sof(C48)=Sof(H48)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C49)=
 Sof(H49)=Sof(C47)=Sof(H47)=FVAR(3)
 Sof(C40A)=Sof(C41A)=Sof(H41A)=Sof(C43A)=Sof(H43A)=Sof(C45A)=Sof(H45A)=
 Sof(C44A)=Sof(H44A)=Sof(C42A)=Sof(H42A)=1-FVAR(4)
 Sof(C42)=Sof(H42)=Sof(C40)=Sof(C41)=Sof(H41)=Sof(C43)=Sof(H43)=Sof(C45)=
 Sof(H45)=Sof(C44)=Sof(H44)=FVAR(4)
 Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C37A)=Sof(H37A)=Sof(C39A)=Sof(H39A)=
 Sof(C38A)=Sof(H38A)=Sof(C36A)=Sof(H36A)=1-FVAR(5)
 Sof(C34)=Sof(C35)=Sof(H35)=Sof(C37)=Sof(H37)=Sof(C39)=Sof(H39)=Sof(C38)=
 Sof(H38)=Sof(C36)=Sof(H36)=FVAR(5)
 Fixed Sof: O2(0.5) O4(0.5) O3(0.5) O5(0.5) C18(0.5) C22(0.5) C4(0.5) C5(0.5)
 H5(0.5) C6(0.5) C3(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C2(0.5) H2(0.5) C21(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C14(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C10(0.5) C1(0.5)
 C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 O4A(0.5) O5A(0.5) C3A(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C2A(0.5)
 H2A(0.5) C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C14A(0.5) C15A(0.5) H15D(0.5)
 H15E(0.5) H15F(0.5) C10A(0.5) C1A(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C13A(0.5) H13D(0.5) H13E(0.5)
 H13F(0.5) O2A(0.5) O3A(0.5) C18A(0.5) C22A(0.5) C4A(0.5) C5A(0.5) H5A(0.5)
 C6A(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C21A(0.5) H21D(0.5) H21E(0.5)
 H21F(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C19A(0.5) H19D(0.5)
 H19E(0.5) H19F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C24A(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5)
 Fixed X: O4(0.666921) O3(0.52165)
 Fixed Y: O3(0.64281) O5A(0.75391) O3A(0.73835)
 Fixed Z: O5A(0.38566) O2A(0.313641) O3A(0.29056)
6.a Me refined with riding coordinates:
 C24A(H24D,H24E,H24F)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C35(H35), C37(H37), C39(H39), C38(H38), C36(H36), C48(H48), C50(H50),
 C51(H51), C49(H49), C47(H47), C42(H42), C41(H41), C43(H43), C45(H45), C44(H44),
  C5(H5), C2(H2), C2A(H2A), C5A(H5A), C48A(H48A), C50A(H50A), C51A(H51A),
 C49A(H49A), C47A(H47A), C41A(H41A), C43A(H43A), C45A(H45A), C44A(H44A),
 C42A(H42A), C35A(H35A), C37A(H37A), C39A(H39A), C38A(H38A), C36A(H36A)
6.c Fitted hexagon refined as free rotating group:
 C34(C35,C37,C39,C38,C36), C46(C48,C50,C51,C49,C47), C42(C40,C41,C43,C45,C44),
 C46A(C48A,C50A,C51A,C49A,C47A), C40A(C41A,C43A,C45A,C44A,C42A), C34A(C35A,C37A,
 C39A,C38A,C36A)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C29(H29A,H29B,
 H29C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C), C23(H23A,
 H23B,H23C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C),
 C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C),
 C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C15A(H15D,H15E,H15F), C12A(H12D,
 H12E,H12F), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F), C23A(H23D,H23E,H23F),
 C21A(H21D,H21E,H21F), C20A(H20D,H20E,H20F), C19A(H19D,H19E,H19F), C25A(H25D,
 H25E,H25F), C29A(H29D,H29E,H29F), C28A(H28D,H28E,H28F), C27A(H27D,H27E,H27F),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              97566
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.811