Six-coordinate lanthanide complexes based on bidentate phosphine oxide ligands: synthesis, structure and magnetic properties
Wu, Xiao-Jun; Guo, Hong-Yao; Lin, Wei-Quan; Meng, Yan; Leng, Ji-Dong; Dalton Transactions 54 (2025) 7819–7827; doi:10.1039/D5DT00422E

data_7719002
_publ_section_title
;
 Six-coordinate lanthanide complexes based on bidentate phosphine oxide
 ligands: synthesis, structure and magnetic properties
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              7819
_journal_page_last               7827
_journal_paper_doi               10.1039/D5DT00422E
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C50 H44 Cl2 O4 P4 Yb, C4 H8 O, Cl'
_chemical_formula_sum            'C54 H52 Cl3 O5 P4 Yb'
_chemical_formula_weight         1184.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-09 deposited with the CCDC.	2025-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9276(3)
_cell_length_b                   21.7519(3)
_cell_length_c                   22.4546(3)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      69.9810
_cell_measurement_theta_min      3.5300
_cell_volume                     10221.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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     73.00 118.00   0.50    2.50    --   40.39-158.00  36.00   90
  2  \w     35.00  62.00   0.50    2.50    --   40.39-158.00  36.00   54
  3  \w   -146.00 -99.00   0.50   12.50    --  -95.00 -57.00  63.00   94
  4  \w    -55.00 -23.00   0.50   12.50    --  -95.00  64.00  38.00   64
  5  \w     25.00  65.00   0.50   12.50    --   99.00 -57.00  63.00   80
  6  \w     29.00  55.00   0.50   12.50    --   99.00 -64.00 -97.00   52
  7  \w     92.00 154.00   0.50   12.50    --   99.00 118.00 -83.00  124
  8  \w    -13.00  42.00   0.50    2.50    --  -40.39  19.00 -90.00  110
  9  \w   -105.00 -56.00   0.50    2.50    --  -40.39-158.00  36.00   98
 10  \w     45.00 106.00   0.50   12.50    --   99.00 -94.00-180.00  122
 11  \w     58.00 100.00   0.50   12.50    --   99.00-125.00  90.00   84
 12  \w     20.00  99.00   0.50   12.50    --   99.00 -94.00-150.00  158
 13  \w     21.00  53.00   0.50   12.50    --   99.00 -45.00 -30.00   64
 14  \w     28.00  53.00   0.50   12.50    --   99.00-125.00  90.00   50
 15  \w     22.00  47.00   0.50   12.50    --   99.00 -45.00  60.00   50
 16  \w     29.00  71.00   0.50   12.50    --   99.00 -61.00 -60.00   84
 17  \w     28.00  53.00   0.50   12.50    --   99.00 -45.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0351009000
_diffrn_orient_matrix_UB_12      0.0461630000
_diffrn_orient_matrix_UB_13      -0.0405187000
_diffrn_orient_matrix_UB_21      0.0358559000
_diffrn_orient_matrix_UB_22      -0.0257609000
_diffrn_orient_matrix_UB_23      -0.0544815000
_diffrn_orient_matrix_UB_31      -0.0538699000
_diffrn_orient_matrix_UB_32      -0.0471262000
_diffrn_orient_matrix_UB_33      -0.0098502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.525
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             4776
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0872P)^2^+3.0514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7605
_reflns_number_total             9639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00422e2.cif
_cod_data_source_block           yb
_cod_original_cell_volume        10221.7(3)
_cod_database_code               7719002
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         YbCl3P4O5C54H52
_chemical_oxdiff_usercomment     'Yb Cl P O C H'
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C63-C67 = C66-C65
 1.54 with sigma of 0.01
 C63A-C67A = C66A-C65A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C63A) \\sim Ueq, Uanis(C66A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C65A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(O64A)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C65A)=Sof(H65C)=Sof(H65D)=
 Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=Sof(H67C)=Sof(H67D)=1-FVAR(1)
 Sof(O64)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=
 Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C45(H45A,H45B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C63A(H63C,H63D), C65A(H65C,H65D), C66A(H66C,H66D), C67A(H67C,
 H67D)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59)
;
_shelx_res_checksum              7444
_shelx_hkl_checksum              41483
_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 2.645
_oxdiff_exptl_absorpt_empirical_full_min 0.396