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_7714789
_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 N8 P2 S4 Y, C38 H26 N4 P S2, 0.5(C4 H8 O), 1.5(C7 H8)'
_chemical_formula_sum            'C126.5 H94 N12 O0.5 P3 S6 Y'
_chemical_formula_weight         2164.31
_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                 94.156(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.092(2)
_cell_length_b                   14.6554(16)
_cell_length_c                   38.107(4)
_cell_measurement_reflns_used    8485
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.38
_cell_measurement_theta_min      2.32
_cell_volume                     10634(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1600
_diffrn_reflns_av_unetI/netI     0.1473
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            94414
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.802
_diffrn_reflns_theta_max         24.802
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1045 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.7357.
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             4484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         18182
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+59.7991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10454
_reflns_number_total             18182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03511e2.cif
_cod_data_source_block           ek95_1
_cod_depositor_comments
'Adding full bibliography for 7714787--7714793.cif.'
_cod_original_formula_sum        'C126.50 H94 N12 O0.50 P3 S6 Y'
_cod_database_code               7714789
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.874
_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
 C7S-C1S
 1.55 with sigma of 0.02
 C16S-C17S = C17S-C18S = C18S-C19S
 1.5 with sigma of 0.02
 O15S-C16S = O15S-C19S
 1.45 with sigma of 0.02
 C9S-C8S = C9S-C10S = C11S-C10S = C12S-C11S = C13S-C12S = C8S-C13S
 1.39 with sigma of 0.01
 C8S-C14S
 1.54 with sigma of 0.02
 C17S-C19S = C16S-C18S = C19S-C16S
 2.5 with sigma of 0.04
 O15S-C17S = O15S-C18S
 2.45 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(C19S) = Uiso(O15S) = Uiso(C16S) = Uiso(C17S) = Uiso(C18S) = Uiso(C13S) =
Uiso(C8S) = Uiso(C9S) = Uiso(C14S) = Uiso(C10S) = Uiso(C12S) = Uiso(C11S)
4. Others
 Fixed Sof: O15S(0.5) C16S(0.5) H16A(0.5) H16B(0.5) C17S(0.5) H17A(0.5)
 H17B(0.5) C18S(0.5) H18A(0.5) H18B(0.5) C19S(0.5) H19A(0.5) H19B(0.5) C8S(0.5)
 C9S(0.5) H9S(0.5) C10S(0.5) H10S(0.5) C11S(0.5) H11S(0.5) C12S(0.5) H12S(0.5)
 C13S(0.5) H13S(0.5) C14S(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C16S(H16A,H16B), C17S(H17A,H17B), C18S(H18A,H18B), C19S(H19A,H19B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C10(H10), C12(H12), C18(H18), C19(H19), C21(H21),
 C23(H23), C24(H24), C25(H25), C33(H33), C35(H35), C37(H37), C39(H39), C42(H42),
  C43(H43), C44(H44), C47(H47), C49(H49), C51(H51), C55(H55), C61(H61),
 C62(H62), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C77(H77), C78(H78),
  C80(H80), C84(H84), C85(H85), C87(H87), C88(H88), C89(H89), C92(H92),
 C93(H93), C94(H94), C95(H95), C96(H96), C98(H98), C100(H100), C101(H101),
 C102(H102), C103(H103), C104(H104), C106(H106), C107(H107), C108(H108),
 C113(H113), C2(H2), C15(H15), C17(H17), C29(H29), C31(H31), C41(H41), C45(H45),
  C46(H46), C50(H50), C56(H56), C59(H59), C63(H63), C65(H65), C71(H71),
 C72(H72), C73(H73), C76(H76), C79(H79), C82(H82), C86(H86), C90(H90), C97(H97),
  C99(H99), C105(H105), C111(H111), C112(H112), C6S(H6S), C5S(H5S), C4S(H4S),
 C3S(H3S), C2S(H2S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S), C13S(H13S)
5.c Fitted hexagon refined as free rotating group:
 C1S(C6S,C5S,C4S,C3S,C2S)
5.d Idealised Me refined as rotating group:
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C)
;
_shelx_res_checksum              41757
_olex2_submission_special_instructions 'No special instructions were received'