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_7714793
_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 Gd N8 P2 S4, C38 H26 N4 P S2, 3(C4 H8 O), 3(C7 H8)'
_chemical_formula_sum            'C147 H126 Gd N12 O3 P3 S6'
_chemical_formula_weight         2551.11
_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                 93.4490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7279(6)
_cell_length_b                   14.4740(5)
_cell_length_c                   38.0128(12)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.37
_cell_volume                     12482.2(7)
_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 0.998
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            223237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_min         1.955
_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    0.731
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1111 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.9390.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             5284
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         27557
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0469P)^2^+20.2050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22797
_reflns_number_total             27557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03511e2.cif
_cod_data_source_block           sdk181
_cod_depositor_comments
'Adding full bibliography for 7714787--7714793.cif.'
_cod_database_code               7714793
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.880
_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
 C38S-C32S
 1.54 with sigma of 0.02
 C40S-C41S = C42S-C41S = C42S-C43S = O39S-C43S = O39S-C40S
 1.5 with sigma of 0.02
 C37S-C38S \\sim C38S-C33S
 with sigma of 0.02
3. Restrained planarity
 C32S, C33S, C34S, C35S, C36S, C37S, C38S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(O44S) = Uiso(C45S) = Uiso(C48S) = Uiso(C46S) = Uiso(C47S)
Uiso(C33S) = Uiso(C34S) = Uiso(C35S) = Uiso(C36S) = Uiso(C32S) = Uiso(C37S) =
Uiso(C38S)
5. Others
 Sof(O44S)=Sof(C45S)=Sof(H45A)=Sof(H45B)=Sof(C46S)=Sof(H46A)=Sof(H46B)=
 Sof(C47S)=Sof(H47A)=Sof(H47B)=Sof(C48S)=Sof(H48A)=Sof(H48B)=Sof(C34S)=
 Sof(H34S)=Sof(C35S)=Sof(H35S)=Sof(C36S)=Sof(H36S)=Sof(C37S)=Sof(H37S)=
 Sof(C32S)=Sof(C33S)=Sof(H33S)=Sof(C38S)=Sof(H38A)=Sof(H38B)=Sof(H38C)=1-FVAR(1)
 Sof(O39S)=Sof(C40S)=Sof(H40A)=Sof(H40B)=Sof(C41S)=Sof(H41A)=Sof(H41B)=
 Sof(C42S)=Sof(H42A)=Sof(H42B)=Sof(C43S)=Sof(H43A)=Sof(H43B)=Sof(C25S)=
 Sof(C26S)=Sof(H26S)=Sof(C27S)=Sof(H27S)=Sof(C28S)=Sof(H28S)=Sof(C29S)=
 Sof(H29S)=Sof(C30S)=Sof(H30S)=Sof(C31S)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
6.a Free rotating group:
 O44S(C45S,C46S,C47S,C48S)
6.b 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), C40S(H40A,H40B),
 C41S(H41A,H41B), C42S(H42A,H42B), C43S(H43A,H43B), C45S(H45A,H45B), C46S(H46A,
 H46B), C47S(H47A,H47B), C48S(H48A,H48B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62), C64(H64),
  C65(H65), C66(H66), C69(H69), C70(H70), C71(H71), C74(H74), C81(H81),
 C83(H83), C85(H85), C86(H86), C87(H87), C90(H90), C91(H91), C92(H92), C93(H93),
  C98(H98), C99(H99), C101(H101), C104(H104), C105(H105), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C113(H113),
 C114(H114), C115(H115), C116(H116), C120(H120), C121(H121), C2S(H2S), C3S(H3S),
  C4S(H4S), C5S(H5S), C6S(H6S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S),
 C13S(H13S), C26S(H26S), C27S(H27S), C28S(H28S), C29S(H29S), C30S(H30S),
 C34S(H34S), C35S(H35S), C36S(H36S), C37S(H37S), C33S(H33S)
6.d Fitted hexagon refined as free rotating group:
 C25S(C26S,C27S,C28S,C29S,C30S), C34S(C35S,C36S,C37S,C32S,C33S)
6.e Idealised Me refined as rotating group:
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C), C31S(H31A,H31B,H31C), C38S(H38A,
 H38B,H38C)
;
_shelx_res_checksum              14623
_olex2_submission_special_instructions 'No special instructions were received'