The influence of different cations on the structure and spectral properties of Ln3+ tetrakis-complexes with the CAPh-type ligand dimethyl-N-trichloroacetylamidophosphate
Struhatska, Mariia B.; Kariaka, Nataliia S.; Dyakonenko, Viktoriya V.; Shishkina, Svitlana V.; Smola, Sergii S.; Rusakova, Nataliia V.; Gawryszewska, Paula; Malta, Oscar L.; Carneiro Neto, Albano N.; Trush, Viktor O.; Amirkhanov, Volodymyr M.; New Journal of Chemistry 48 (2024) 11886–11898; doi:10.1039/D4NJ01700E

data_7063241
_publ_section_title
;
 The influence of different cations on the structure and spectral
 properties of Ln3+ tetrakis-complexes with the CAPh-type ligand
 dimethyl-N-trichloroacetylamidophosphate
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11886
_journal_page_last               11898
_journal_paper_doi               10.1039/D4NJ01700E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C16 H24 Cl12 Eu N4 O16 P4, C8 H20 N'
_chemical_formula_sum            'C24 H44 Cl12 Eu N5 O16 P4'
_chemical_formula_weight         1359.88
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-11 deposited with the CCDC.	2024-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.286(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4825(6)
_cell_length_b                   12.2546(3)
_cell_length_c                   21.3808(6)
_cell_measurement_reflns_used    6600
_cell_measurement_temperature    294
_cell_measurement_theta_max      24.3340
_cell_measurement_theta_min      3.2790
_cell_volume                     5362.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_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      6.00  74.00   1.00   10.00    --   26.76  77.00  30.00   68
  2  \w      0.00  90.00   1.00   10.00    --   26.76  77.00 -60.00   90
  3  \w     -7.00  65.00   1.00   10.00    --   26.76 -99.00 120.00   72
  4  \w     -4.00  98.00   1.00   10.00    --   26.76  19.00 -60.00  102
  5  \w    -43.00  56.00   1.00   10.00    --   26.76 -77.00-180.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0227714000
_diffrn_orient_matrix_UB_12      0.0297183000
_diffrn_orient_matrix_UB_13      -0.0174603000
_diffrn_orient_matrix_UB_21      -0.0183179000
_diffrn_orient_matrix_UB_22      0.0484017000
_diffrn_orient_matrix_UB_23      0.0041898000
_diffrn_orient_matrix_UB_31      0.0186135000
_diffrn_orient_matrix_UB_32      0.0112946000
_diffrn_orient_matrix_UB_33      0.0279154000
_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  0.1013
_diffrn_reflns_av_unetI/netI     0.0793
_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       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_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    1.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.827
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         10526
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1196P)^2^+5.6385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7499
_reflns_number_total             10526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01700e2.cif
_cod_data_source_block           kiev355
_cod_depositor_comments
'Adding full bibliography for 7063240--7063242.cif.'
_cod_original_cell_volume        5362.4(2)
_cod_database_code               7063241
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Restrained distances
 O3-C2 = O2-C1 = O7-C6 = O6-C5 = O10-C9 = O11-C10 = O15-C14 = O14-C13
 1.416 with sigma of 0.005
 Cl9-C16 = Cl12-C16 = Cl7-C16 = Cl8-C16 = Cl10-C16 = Cl11-C16 = Cl9A-C12 =
 Cl9B-C12 = Cl8B-C12 = Cl8A-C12 = Cl7B-C12 = Cl7A-C12
 1.76 with sigma of 0.002
2. Restrained angles
 Cl11-C16-Cl12
 fixed at 110 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl7 \\sim Cl8 \\sim Cl9 \\sim Cl10 \\sim Cl11 \\sim Cl12: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
P3 \\sim O10 \\sim O11 \\sim C9 \\sim C10: within 1.7A with sigma of 0.002 and
sigma for terminal atoms of 0.04 within 1.7A
Uanis(Cl8A) \\sim Ueq, Uanis(Cl8B) \\sim Ueq, Uanis(Cl9B) \\sim Ueq,
Uanis(Cl9A) \\sim Ueq, Uanis(Cl7A) \\sim Ueq, Uanis(Cl7B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl7(0.5) Cl7A(0.5) Cl7B(0.5) Cl8(0.5) Cl8A(0.5) Cl8B(0.5) Cl9(0.5)
 Cl9A(0.5) Cl9B(0.5) Cl10(0.5) Cl11(0.5) Cl12(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B)
5.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              72315
_platon_squeeze_void_probe_radius 1.20
_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 28.181
_oxdiff_exptl_absorpt_empirical_full_min 0.642