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_7715698
_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         'C32 H38 Er2 N4 O26 S4, 8(H2 O)'
_chemical_formula_sum            'C32 H54 Er2 N4 O34 S4'
_chemical_formula_weight         1501.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-11
_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                90
_cell_angle_beta                 107.3690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1450(6)
_cell_length_b                   7.4186(3)
_cell_length_c                   23.3610(8)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      27.541
_cell_measurement_theta_min      2.682
_cell_volume                     2505.04(17)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.05
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         2.682
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1151 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.8278.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0229P)^2^+5.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             5775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00577e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715696--7715701.cif.'
_cod_database_code               7715698
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.644
_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 O(H,H) groups
2.a Free rotating group:
 O6W(H6Wa,H6Wb), O7W(H7Wa,H7Wb), O8W(H8Wa,H8Wb), O9W(H9Wa,H9Wb)
2.b Rotating group:
 O4W(H4Wa,H4Wb), O3W(H3Wa,H3Wb), O1W(H1Wa,H1Wb), O5W(H5Wa,H5Wb), O2W(H2Wa,H2Wb)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C9(H9), C6(H6), C13(H13), C11(H11), C2(H2), C3(H3), C5(H5), C4(H4)
;
_shelx_res_checksum              15397
_olex2_submission_special_instructions 'No special instructions were received'