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_7063242
_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 Gd N4 O16 P4, C24 H20 P'
_chemical_formula_sum            'C40 H44 Cl12 Gd N4 O16 P5'
_chemical_formula_weight         1574.29
_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     iterative
_audit_creation_date             2024-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.925(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8828(8)
_cell_length_b                   19.1092(8)
_cell_length_c                   17.3678(6)
_cell_measurement_reflns_used    6685
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      20.51
_cell_measurement_theta_min      2.19
_cell_volume                     6163.6(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83638
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.529
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1029 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.7214.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.407
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         10860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0357P)^2^+41.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7955
_reflns_number_total             10860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01700e2.cif
_cod_data_source_block           k366
_cod_depositor_comments
'Adding full bibliography for 7063240--7063242.cif.'
_cod_database_code               7063242
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
2.b 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), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              71212
_olex2_submission_special_instructions 'No special instructions were received'