Lanthanide complexes with an azo-dye chromophore ligand: syntheses, crystal structures, and near-infrared luminescence by long-wavelength excitation.
Chen, Yun-Long; Feng, Min; Zhu, Xiaofei; Zheng, Zhiping; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7350–7357; doi:10.1039/d4dt00577e

data_7715700
_publ_section_title
;
 Lanthanide complexes with an azo-dye chromophore ligand: syntheses,
 crystal structures, and near-infrared luminescence by long-wavelength
 excitation.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7350
_journal_page_last               7357
_journal_paper_doi               10.1039/d4dt00577e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H78 N4 O26 S14 Yb2, 2[C2H6SO]'
_chemical_formula_sum            'C56 H90 N4 O28 S16 Yb2'
_chemical_formula_weight         2126.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                113.027(3)
_cell_angle_beta                 90.449(4)
_cell_angle_gamma                111.806(4)
_cell_formula_units_Z            1
_cell_length_a                   11.2546(8)
_cell_length_b                   14.4042(9)
_cell_length_c                   15.0132(9)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      60.75
_cell_measurement_theta_min      3.80
_cell_volume                     2046.0(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51458
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.877
_diffrn_reflns_theta_min         3.175
_diffrn_source_current           3.0
_diffrn_source_power             0.20955
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.400
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.7707.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       needle
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7724
_reflns_number_total             9428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00577e2.cif
_cod_data_source_block           fa2
_cod_depositor_comments
'Adding full bibliography for 7715696--7715701.cif.'
_cod_database_code               7715700
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C13(H13), C11(H11), C5(H5), C6(H6), C9(H9), C2(H2), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C19(H19A,
 H19B,H19C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74236
_shelx_fab_checksum              78140
_olex2_submission_special_instructions 'No special instructions were received'