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_7063240
_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, C4 H12 N'
_chemical_formula_sum            'C20 H36 Cl12 Eu N5 O16 P4'
_chemical_formula_weight         1303.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                 94.501(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0428(8)
_cell_length_b                   10.2128(6)
_cell_length_c                   21.0833(11)
_cell_measurement_reflns_used    2656
_cell_measurement_temperature    294
_cell_measurement_theta_max      23.9920
_cell_measurement_theta_min      3.3260
_cell_volume                     2585.1(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    'SHELXT  (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    -38.00 -11.00   1.00   15.00    --  -25.36  19.00 -60.00   27
  2  \w    -85.00 -39.00   1.00   15.00    --  -25.36 131.00 -49.00   46
  3  \w    -89.00 -16.00   1.00   15.00    --  -25.36 137.00 126.00   73
  4  \w    -37.00  47.00   1.00   15.00    --   26.76 -57.00-120.00   84
  5  \w     10.00  96.00   1.00   15.00    --   26.76  57.00 120.00   86
  6  \w    -10.00  96.00   1.00   15.00    --   26.76  19.00  60.00  106
;
_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      0.0576108000
_diffrn_orient_matrix_UB_12      -0.0100584000
_diffrn_orient_matrix_UB_13      -0.0030771000
_diffrn_orient_matrix_UB_21      0.0101720000
_diffrn_orient_matrix_UB_22      0.0010637000
_diffrn_orient_matrix_UB_23      0.0335950000
_diffrn_orient_matrix_UB_31      -0.0082776000
_diffrn_orient_matrix_UB_32      -0.0687030000
_diffrn_orient_matrix_UB_33      0.0009536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5084
_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         26.000
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.015
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72240
_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    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5084
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0835P)^2^+4.6143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4166
_reflns_number_total             5084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01700e2.cif
_cod_data_source_block           kiev353
_cod_depositor_comments
'Adding full bibliography for 7063240--7063242.cif.'
_cod_database_code               7063240
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.378
_reflns_odcompleteness_completeness 90.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.27
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.78891
 0.21109
2. Restrained distances
 Cl6B-C8 = Cl6A-C8 = Cl4B-C8 = Cl4A-C8 = Cl5B-C8 = Cl5A-C8
 1.76 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(Cl4B) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl5B) \\sim Ueq,
Uanis(Cl5A) \\sim Ueq, Uanis(Cl6B) \\sim Ueq, Uanis(Cl6A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl4A(0.5) Cl4B(0.5) Cl5A(0.5) Cl5B(0.5) Cl6A(0.5) Cl6B(0.5)
5.a 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), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              70031
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.781
_oxdiff_exptl_absorpt_empirical_full_min 0.743