Crystal structure of tetra-phenyl phosphate tetra-kis-[dimethyl (2,2,2-tri-chloro-acet-yl)phos-pho-ramidato]lutetium(III), PPh<sub>4</sub>[Lu<i>L</i><sub>4</sub>].
Struhatska, Mariia B.; Ovchynnikov, Vladimir A.; Kariaka, Nataliia S.; Gawryszewska, Paula; Amirkhanov, Volodymyr M.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 370–374; doi:10.1107/S205698902400210X

data_2023049
_publ_section_title
;
 Crystal structure of tetra-phenyl phosphate tetra-kis-[dimethyl
 (2,2,2-tri-chloro-acet-yl)phos-pho-ramidato]lutetium(III),
 PPh<sub>4</sub>[Lu<i>L</i><sub>4</sub>].
;
_journal_coeditor_code           DJ2075
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              370
_journal_page_last               374
_journal_paper_doi               10.1107/S205698902400210X
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '(C24 H20 P) [Lu (C4 H6 Cl3 N O4 P)4]'
_chemical_formula_moiety         'C24 H20 P +, C16 H24 Cl12 Lu N4 O16 P4 -'
_chemical_formula_sum            'C40 H44 Cl12 Lu N4 O16 P5'
_chemical_formula_weight         1592.01
_chemical_name_systematic
;
Tetraphenyl phosphate
tetrakis[dimethyl (2,2,2-trichloroacetyl)phosphoramidato]lutetium(III)
;
_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
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 110.8107(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6882(3)
_cell_length_b                   18.9452(10)
_cell_length_c                   17.2139(3)
_cell_measurement_reflns_used    36128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7900
_cell_measurement_theta_min      2.3890
_cell_volume                     6001.8(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
ORTEPIII  for Windows(1.0.3) (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS Version 2013/1 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy R with HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            68030
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.914
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    9.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         11789
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0532P)^2^+11.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                10535
_reflns_number_total             11789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2075.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023049.cif.'
_cod_original_cell_volume        6001.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023049
_shelx_hkl_checksum              87790
_shelx_res_checksum              71630