Lanthanide complexes with a new luminescent iminophosphonamide ligand bearing phenylbenzothiazole substituents.
Sinitsa, Dmitry K.; Pylova, Ekaterina K.; Mironova, Olga A.; Bashirov, Denis A.; Ryadun, Alexey A.; Sukhikh, Taisiya S.; Konchenko, Sergey N.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2181–2192; doi:10.1039/d3dt03511e

data_7714791
_publ_section_title
;
 Lanthanide complexes with a new luminescent iminophosphonamide ligand
 bearing phenylbenzothiazole substituents.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2181
_journal_page_last               2192
_journal_paper_doi               10.1039/d3dt03511e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C76 H52 Dy N8 P2 S4, C38 H26 N4 P S2, 4(C4 H8 O), 2(C7 H8)'
_chemical_formula_sum            'C144 H126 Dy N12 O4 P3 S6'
_chemical_formula_weight         2536.33
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2023-09-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-02 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.482(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7471(15)
_cell_length_b                   14.4532(10)
_cell_length_c                   37.979(3)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.28
_cell_volume                     12463.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            109716
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         1.441
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0737 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.9280.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             5252
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1398
_refine_ls_number_reflns         29622
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+23.1248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23274
_reflns_number_total             29622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03511e2.cif
_cod_data_source_block           sdk156
_cod_depositor_comments
'Adding full bibliography for 7714787--7714793.cif.'
_cod_database_code               7714791
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.844
_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
2. Restrained distances
 O20S-C21S = O20S-C24S
 1.45 with sigma of 0.02
 C22S-C21S = C22S-C23S = C24S-C23S
 1.5 with sigma of 0.02
 C21S-C24S = C22S-C24S = C23S-C21S = C22S-O20S = O20S-C23S
 2.5 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C16S(H16A,H16B), C17S(H17A,H17B), C18S(H18A,H18B), C19S(H19A,H19B), C21S(H21A,
 H21B), C22S(H22A,H22B), C23S(H23A,H23B), C24S(H24A,H24B), C25S(H25A,H25B),
 C26S(H26A,H26B), C27S(H27A,H27B), C28S(H28A,H28B), C31S(H31A,H31B), C32S(H32A,
 H32B), C33S(H33A,H33B), C34S(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C12(H12), C19(H19), C20(H20), C23(H23),
 C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
  C37(H37), C41(H41), C42(H42), C44(H44), C46(H46), C49(H49), C54(H54),
 C56(H56), C60(H60), C61(H61), C62(H62), C64(H64), C66(H66), C68(H68), C70(H70),
  C71(H71), C74(H74), C76(H76), C79(H79), C80(H80), C81(H81), C82(H82),
 C83(H83), C87(H87), C88(H88), C90(H90), C91(H91), C96(H96), C97(H97), C99(H99),
  C103(H103), C106(H106), C107(H107), C111(H111), C112(H112), C113(H113),
 C7(H7), C13(H13), C17(H17), C22(H22), C24(H24), C28(H28), C39(H39), C40(H40),
 C43(H43), C45(H45), C50(H50), C53(H53), C63(H63), C72(H72), C73(H73), C77(H77),
  C78(H78), C84(H84), C85(H85), C86(H86), C89(H89), C92(H92), C94(H94),
 C95(H95), C101(H101), C110(H110), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S),
 C6S(H6S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S), C13S(H13S)
3.c Idealised Me refined as rotating group:
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C)
;
_shelx_res_checksum              23840
_olex2_submission_special_instructions 'No special instructions were received'