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_7714792
_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, 1.229(C7 H8), 0.369(C6 H14)'
_chemical_formula_sum            'C124.81 H92.99 N12 P3 S6 Y'
_chemical_formula_weight         2134.96
_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             2023-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-06 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.667(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0929(19)
_cell_length_b                   14.6218(18)
_cell_length_c                   38.215(5)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.55
_cell_measurement_theta_min      2.32
_cell_volume                     10633(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  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1596
_diffrn_reflns_av_unetI/netI     0.1325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47109
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.816
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         1.810
_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    0.769
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.6473.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       plate
_exptl_crystal_F_000             4423
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         11109
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+43.3399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6757
_reflns_number_total             11109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03511e2.cif
_cod_data_source_block           sdk-y
_cod_depositor_comments
'Adding full bibliography for 7714787--7714793.cif.'
_cod_database_code               7714792
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.887
_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
 C15S-C16S = C16S-C17S = C17S-C18S = C18S-C19S = C19S-C20S
 1.54 with sigma of 0.02
 C15S-C17S = C17S-C19S = C16S-C18S = C18S-C20S
 2.54 with sigma of 0.04
 Y1-N3 \\sim Y1-N3A
 with sigma of 0.02
 S1-C4 \\sim S1A-C4A
 with sigma of 0.02
 S1-C60 \\sim S1A-C60A
 with sigma of 0.02
 N3-C4 \\sim N3A-C4A
 with sigma of 0.02
 N3-C52 \\sim N3A-C52A
 with sigma of 0.02
 C4-C20 \\sim C4A-C20
 with sigma of 0.02
 C37-C52 \\sim C37A-C52A
 with sigma of 0.02
 C37-C98 \\sim C37A-C98A
 with sigma of 0.02
 C51-C60 \\sim C51A-C60A
 with sigma of 0.02
 C52-C60 \\sim C52A-C60A
 with sigma of 0.02
 C98-C104 \\sim C98A-C115
 with sigma of 0.02
 Y1-C4 \\sim Y1-C4A
 with sigma of 0.04
 Y1-C52 \\sim Y1-C52A
 with sigma of 0.04
 S1-N3 \\sim S1A-N3A
 with sigma of 0.04
 S1-C20 \\sim S1A-C20
 with sigma of 0.04
 S1-C51 \\sim S1A-C51A
 with sigma of 0.04
 S1-C52 \\sim S1A-C52A
 with sigma of 0.04
 N3-C20 \\sim N3A-C20
 with sigma of 0.04
 N3-C37 \\sim N3A-C37A
 with sigma of 0.04
 C51-C104 \\sim C51A-C115
 with sigma of 0.02
 N3-C60 \\sim N3A-C60A
 with sigma of 0.04
 C4-C52 \\sim C4A-C52A
 with sigma of 0.04
 C4-C60 \\sim C4A-C60A
 with sigma of 0.04
 C37-C60 \\sim C37A-C60A
 with sigma of 0.04
 C37-C104 \\sim C37A-C115
 with sigma of 0.04
 C51-C52 \\sim C51A-C52A
 with sigma of 0.04
 C51-C98 \\sim C51A-C98A
 with sigma of 0.04
 C52-C98 \\sim C52A-C98A
 with sigma of 0.04
 C60-C104 \\sim C60A-C115
 with sigma of 0.04
 C4A-C20 \\sim C4-C20
 with sigma of 0.02
3. Restrained planarity
 S1, N3, C4, C37, C51, C52, C60, C98, C104
 with sigma of 0.1
 S1A, N3A, C4A, C37A, C51A, C52A, C60A, C98A, C115
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C51A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C14S) = Uiso(C8S) = Uiso(C9S) = Uiso(C13S) = Uiso(C10S) = Uiso(C12S) =
Uiso(C11S)
Uanis(N3) = Uanis(N3A)
Uanis(C4A) = Uanis(C4)
Uanis(C37) = Uanis(C37A)
Uiso(C15S) = Uiso(C16S) = Uiso(C17S) = Uiso(C18S) = Uiso(C19S) = Uiso(C20S)
5. Rigid body (RIGU) restrains
 S1, N3, C4, C37, C51, C52, C60, C98, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, N3A, C4A, C37A, C51A, C52A, C60A, C98A, C115
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S1A)=Sof(N3A)=Sof(C4A)=Sof(C37A)=Sof(H37A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=
 Sof(C60A)=Sof(C98A)=Sof(H98A)=Sof(C115)=Sof(H115)=1-FVAR(1)
 Sof(S1)=Sof(N3)=Sof(C4)=Sof(C37)=Sof(H37)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(C60)=
 Sof(C98)=Sof(H98)=Sof(C104)=Sof(H104)=FVAR(1)
 Sof(C14S)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C8S)=Sof(C9S)=Sof(H9S)=Sof(C10S)=
 Sof(H10S)=Sof(C11S)=Sof(H11S)=Sof(C12S)=Sof(H12S)=Sof(C13S)=Sof(H13S)=FVAR(2)
 Sof(C15S)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16S)=Sof(H16A)=Sof(H16B)=
 Sof(C17S)=Sof(H17A)=Sof(H17B)=Sof(C18S)=Sof(H18A)=Sof(H18B)=Sof(C19S)=
 Sof(H19A)=Sof(H19B)=Sof(C20S)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
 Fixed Uiso: C15S(0.1) C16S(0.1) C17S(0.1) C18S(0.1) C19S(0.1) C20S(0.1)
7.a Free rotating group:
 C14S(C8S,C9S,C10S,C11S,C12S,C13S)
7.b Secondary CH2 refined with riding coordinates:
 C16S(H16A,H16B), C17S(H17A,H17B), C18S(H18A,H18B), C19S(H19A,H19B)
7.c Me refined with riding coordinates:
 C15S(H15A,H15B,H15C), C20S(H20A,H20B,H20C)
7.d 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), C37A(H37A),
 C39(H39), C42(H42), C43(H43), C44(H44), C47(H47), C49(H49), C51(H51),
 C51A(H51A), 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), C98A(H98A), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104), C106(H106), C107(H107), C108(H108), C113(H113), C115(H115), 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)
7.e Fitted hexagon refined as free rotating group:
 C1S(C6S,C5S,C4S,C3S,C2S)
7.f Idealised Me refined with riding coordinates:
 C7S(H7SA,H7SB,H7SC)
7.g Idealised Me refined as rotating group:
 C14S(H14A,H14B,H14C)
;
_shelx_res_checksum              84451
_olex2_submission_special_instructions 'No special instructions were received'