Identification of Complexes of Nd(III) with Dithiophosphinic Acids Verifying Difference in Complexation between Ln(III) and An(III)
Guo, Qiling; Fang, Tuo; Liu, Qian; Zhu, Liyang; Yang, Suliang; Tian, Guoxin; Dalton Transactions  (2022) –; doi:10.1039/D2DT00625A

data_7709920
_publ_section_title
;
 Identification of Complexes of Nd(III) with Dithiophosphinic Acids
 Verifying Difference in Complexation between Ln(III) and An(III)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00625A
_journal_year                    2022
_chemical_formula_moiety         '3(C8 H18 P S2), H18 Nd O9, 1.17(H2 O)'
_chemical_formula_sum            'C24 H74.34 Nd O10.17 P3 S6'
_chemical_formula_weight         955.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-03-12
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.03.10 svn.r54f81f84 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.040(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9097(4)
_cell_length_b                   25.6255(5)
_cell_length_c                   10.9443(3)
_cell_measurement_reflns_used    23945
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      31.1620
_cell_measurement_theta_min      3.3450
_cell_volume                     4695.76(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.787
_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     11.00  66.00   0.50    0.50    --    5.65  82.00  12.00  110
  2  \w    -54.00 -22.00   0.50    0.50    --    5.65 -82.00-109.00   64
  3  \w    -20.00  29.00   0.50    0.50    --   -4.71 -99.00  90.00   98
  4  \w    -20.00   6.00   0.50    0.50    --   -4.71 -99.00 120.00   52
  5  \w    -19.00   7.00   0.50    0.50    --   -4.71 -99.00-120.00   52
  6  \w    -66.00  17.00   0.50    0.50    --    5.65 -37.00-120.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44211
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.179
_diffrn_reflns_theta_min         3.272
_exptl_absorpt_coefficient_mu    1.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2003
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11970
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0462P)^2^+4.3286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10067
_reflns_number_total             11970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00625a2.cif
_cod_data_source_block           20200527a
_cod_database_code               7709920
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.752
_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. Restrained distances
 O7-H7D = O7-H7E
 0.85 with sigma of 0.02
 O1-H1C = O1-H1D
 0.85 with sigma of 0.02
 O6-H6A = O6-H6B
 0.85 with sigma of 0.02
 O4-H4D = O4-H4E
 0.85 with sigma of 0.02
 O8-H8D = O8-H8E
 0.85 with sigma of 0.02
 O2-H2A = O2-H2B
 0.85 with sigma of 0.02
 O9-H9C = O9-H9D
 0.85 with sigma of 0.02
 O5-H5C = O5-H5D
 0.85 with sigma of 0.02
 O3-H3D = O3-H3E
 0.85 with sigma of 0.02
 H5C-H5D
 1.34 with sigma of 0.04
 H8D-H8E
 1.34 with sigma of 0.04
 H7D-H7E
 1.34 with sigma of 0.04
 H4D-H4E
 1.34 with sigma of 0.04
 H2A-H2B
 1.34 with sigma of 0.04
 H6A-H6B
 1.34 with sigma of 0.04
 H9C-H9D
 1.34 with sigma of 0.04
 H3D-H3E
 1.34 with sigma of 0.04
 H1C-H1D
 1.34 with sigma of 0.04
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C9-P2 \\sim C9A-P2A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C10-C12 \\sim C10A-C12A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C13-P2 \\sim C13A-P2A
 with sigma of 0.02
 S3-S4 \\sim S3A-S4A
 with sigma of 0.04
 C13-S4 \\sim C13A-S4A
 with sigma of 0.04
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C14-C16 \\sim C14A-C16A
 with sigma of 0.02
 C13-S3 \\sim C13A-S3A
 with sigma of 0.04
 P2-S3 \\sim P2A-S3A
 with sigma of 0.02
 P2-S4 \\sim P2A-S4A
 with sigma of 0.02
 C14-P2 \\sim C14A-P2A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C9-C12 \\sim C9A-C12A
 with sigma of 0.04
 C9-C13 \\sim C9A-C13A
 with sigma of 0.04
 C9-S3 \\sim C9A-S3A
 with sigma of 0.04
 C9-S4 \\sim C9A-S4A
 with sigma of 0.04
 C15-C16 \\sim C15A-C16A
 with sigma of 0.04
 C10-P2 \\sim C10A-P2A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.04
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
 C13-C16 \\sim C13A-C16A
 with sigma of 0.04
 Nd1-H3D \\sim Nd1-H3E
 with sigma of 0.02
 Nd1-H2A \\sim Nd1-H2B
 with sigma of 0.02
 Nd1-H6A \\sim Nd1-H6B
 with sigma of 0.02
 Nd1-H9C \\sim Nd1-H9D
 with sigma of 0.02
 Nd1-H5C \\sim Nd1-H5D
 with sigma of 0.02
 Nd1-H7D \\sim Nd1-H7E
 with sigma of 0.02
 Nd1-H1C \\sim Nd1-H1D
 with sigma of 0.02
 Nd1-H4D \\sim Nd1-H4E
 with sigma of 0.02
 Nd1-H8D \\sim Nd1-H8E
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C13, C14, C16, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(P2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(S3A)=Sof(S4A)=
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(O11)=Sof(H11G)=
 Sof(H11H)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(P2)=Sof(S3)=Sof(S4)=FVAR(1)
 Fixed Uiso: C9A(0.04) C10A(0.04) C11A(0.04) C12A(0.04) C13A(0.04) C14A(0.04)
 C15A(0.04) C16A(0.04)
6.a Riding coordinates:
 C12A(H12D,H12E,H12F)
6.b Free rotating group:
 O10(H10B,H10C), O11(H11G,H11H)
6.c Ternary CH refined with riding coordinates:
 C2(H2), C6(H6), C10(H10), C14(H14), C18(H18), C22(H22), C10A(H10A), C14A(H14A)
6.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C13(H13A,H13B), C17(H17A,H17B),
 C21(H21A,H21B), C9A(H9AA,H9AB), C13A(H13C,H13D)
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C11A(H11D,H11E,H11F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              78013
_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
;