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_7714788
_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 Sm, C38 H26 N4 P S2, 0.5(C4 H8 O), 2(C7 H8)'
_chemical_formula_sum            'C130 H98 N12 O0.5 P3 S6 Sm'
_chemical_formula_weight         2271.82
_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                 94.110(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.211(2)
_cell_length_b                   14.6820(14)
_cell_length_c                   38.175(4)
_cell_measurement_reflns_used    9367
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.32
_cell_volume                     10739.8(19)
_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 0.993
_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  0.1170
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_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       -44
_diffrn_reflns_number            104935
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.454
_diffrn_reflns_theta_max         24.454
_diffrn_reflns_theta_min         1.850
_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    0.768
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1453 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.7155.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plank
_exptl_crystal_F_000             4676
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1364
_refine_ls_number_reflns         17657
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0841
_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^)+119.6716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13369
_reflns_number_total             17657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03511e2.cif
_cod_data_source_block           sdk186-2
_cod_depositor_comments
'Adding full bibliography for 7714787--7714793.cif.'
_cod_original_cell_volume        10739.5(18)
_cod_original_formula_sum        'C130 H98 N12 O0.50 P3 S6 Sm'
_cod_database_code               7714788
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.861
_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
 C8S-C13S \\sim C13S-C12S \\sim C12S-C11S \\sim C11S-C10S \\sim C10S-C9S \\sim
C9S-C8S
 with sigma of 0.02
 C8S-C10S \\sim C8S-C12S \\sim C9S-C11S \\sim C13S-C9S \\sim C12S-C10S \\sim
C13S-C11S
 with sigma of 0.04
 C14S-C9S \\sim C14S-C13S
 with sigma of 0.04
 C15S-C20S \\sim C20S-C19S \\sim C19S-C18S \\sim C18S-C17S \\sim C17S-C16S
\\sim C16S-C15S
 with sigma of 0.02
 C15S-C17S \\sim C15S-C19S \\sim C16S-C18S \\sim C20S-C16S \\sim C19S-C17S
\\sim C20S-C18S
 with sigma of 0.04
 C21S-C16S \\sim C21S-C20S
 with sigma of 0.04
 C23S-C24S \\sim C24S-C25S \\sim C25S-C26S
 with sigma of 0.02
 O22S-C23S \\sim O22S-C26S
 with sigma of 0.02
 O22S-C24S \\sim O22S-C25S
 with sigma of 0.04
 C24S-C26S \\sim C23S-C25S
 with sigma of 0.04
3. Restrained planarity
 C8S, C9S, C10S, C11S, C12S, C13S, C14S
 with sigma of 0.1
 C15S, C16S, C17S, C18S, C19S, C20S, C21S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8S \\sim C9S \\sim C10S \\sim C11S \\sim C12S \\sim C13S \\sim C14S: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C15S \\sim C16S \\sim C17S \\sim C18S \\sim C19S \\sim C20S \\sim C21S: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O22S \\sim C23S \\sim C24S \\sim C25S \\sim C26S: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uiso(C24S) = Uiso(O22S) = Uiso(C23S) = Uiso(C26S) = Uiso(C25S)
5. Rigid body (RIGU) restrains
 C8S, C9S, C10S, C11S, C12S, C13S, C14S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15S, C16S, C17S, C18S, C19S, C20S, C21S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O22S, C23S, C24S, C25S, C26S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C52, C61, C110, C111, C112
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C15S)=Sof(C16S)=Sof(H16S)=Sof(C17S)=Sof(H17S)=Sof(C18S)=Sof(H18S)=
 Sof(C19S)=Sof(H19S)=Sof(C20S)=Sof(H20S)=Sof(C21S)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=1-FVAR(1)
 Sof(C8S)=Sof(C9S)=Sof(H9S)=Sof(C10S)=Sof(H10S)=Sof(C11S)=Sof(H11S)=Sof(C12S)=
 Sof(H12S)=Sof(C13S)=Sof(H13S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Fixed Sof: O22S(0.5) C23S(0.5) H23A(0.5) H23B(0.5) C24S(0.5) H24A(0.5)
 H24B(0.5) C25S(0.5) H25A(0.5) H25B(0.5) C26S(0.5) H26A(0.5) H26B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C23S(H23A,H23B), C24S(H24A,H24B), C25S(H25A,H25B), C26S(H26A,H26B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6(H6), C6S(H6S), C8(H8),
 C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S), C13S(H13S), C10(H10), C11(H11),
 C12(H12), C13(H13), C16S(H16S), C17S(H17S), C18(H18), C18S(H18S), C19S(H19S),
 C20(H20), C20S(H20S), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36),
  C37(H37), C39(H39), C41(H41), C45(H45), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51), C53(H53), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62),
  C63(H63), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
 C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
  C81(H81), C83(H83), C85(H85), C86(H86), C87(H87), C89(H89), C91(H91),
 C92(H92), C93(H93), C94(H94), C95(H95), C97(H97), C98(H98), C99(H99),
 C100(H100), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C109(H109), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114)
7.c Idealised Me refined as rotating group:
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C), C21S(H21A,H21B,H21C)
;
_shelx_res_checksum              54504
_olex2_submission_special_instructions 'No special instructions were received'