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_7715699
_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 Er2 N4 O26 S14'
_chemical_formula_sum            'C56 H90 Er2 N4 O28 S16'
_chemical_formula_weight         2114.79
_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     dual
_audit_creation_date             2023-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                113.056(3)
_cell_angle_beta                 90.302(3)
_cell_angle_gamma                111.853(3)
_cell_formula_units_Z            1
_cell_length_a                   11.2494(6)
_cell_length_b                   14.5051(7)
_cell_length_c                   15.0460(8)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      70.76
_cell_measurement_theta_min      3.74
_cell_volume                     2063.6(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24195
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.998
_diffrn_reflns_theta_min         2.821
_diffrn_source_current           3.0
_diffrn_source_power             0.20958
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.526
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0962 after correction.
The Ratio of minimum to maximum transmission is 0.8225.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       needle
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0473P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5960
_reflns_number_total             7841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00577e2.cif
_cod_data_source_block           c
_cod_depositor_comments
'Adding full bibliography for 7715696--7715701.cif.'
_cod_original_cell_volume        2063.62(19)
_cod_database_code               7715699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.085
_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), C11(H11), C13(H13), C2(H2), C9(H9), C6(H6), C5(H5), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C18(H18A,H18B,H18C), C23(H23A,
 H23B,H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20902
_shelx_fab_checksum              84853
_olex2_submission_special_instructions 'No special instructions were received'