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_7062069
_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         'C56 H70 Gd2 O16 P2'
_chemical_formula_sum            'C56 H70 Gd2 O16 P2'
_chemical_formula_weight         1375.56
_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             2022-08-21
_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                116.703(6)
_cell_angle_beta                 94.714(4)
_cell_angle_gamma                90.564(4)
_cell_formula_units_Z            1
_cell_length_a                   11.0947(6)
_cell_length_b                   12.2688(7)
_cell_length_c                   12.3032(7)
_cell_measurement_reflns_used    4811
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.0610
_cell_measurement_theta_min      3.6670
_cell_volume                     1488.97(17)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  86.00   1.00   18.50    --   16.76  38.00-150.00   87
  2  \w    -10.00  37.00   1.00   18.50    --   16.76  77.00 -60.00   47
  3  \w     -7.00  39.00   1.00   18.50    --   16.76  77.00  60.00   46
  4  \w     39.00  88.00   1.00   18.50    --   16.76 178.00  60.00   49
  5  \w    -55.00  39.00   1.00   18.50    --   16.76 -19.00  30.00   94
;
_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      -0.0352153000
_diffrn_orient_matrix_UB_12      -0.0550653000
_diffrn_orient_matrix_UB_13      -0.0184086000
_diffrn_orient_matrix_UB_21      0.0529562000
_diffrn_orient_matrix_UB_22      -0.0335730000
_diffrn_orient_matrix_UB_23      -0.0149268000
_diffrn_orient_matrix_UB_31      0.0090458000
_diffrn_orient_matrix_UB_32      0.0063517000
_diffrn_orient_matrix_UB_33      0.0603537000
_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  0.0685
_diffrn_reflns_av_unetI/netI     0.1233
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9066
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.172
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33600
_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    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3721
_reflns_number_total             5192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03544h2.cif
_cod_data_source_block           czw-253_auto
_cod_depositor_comments
'Adding full bibliography for 7062065--7062070.cif.'
_cod_original_cell_volume        1488.97(16)
_cod_database_code               7062069
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.542
_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, All O(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C13(H13), C26(H26), C16(H16), C9(H9),
 C12(H12), C21(H21), C11(H11), C10(H10)
2.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
2.d X=CH2 refined with riding coordinates:
 O2(H2A,H2B)
2.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C20(H20A,H20B,
 H20C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              34648
_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 2.330
_oxdiff_exptl_absorpt_empirical_full_min 0.677