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_7715697
_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 Gd2 N4 O26 S4, 8(H2 O)'
_chemical_formula_sum            'C32 H54 Gd2 N4 O34 S4'
_chemical_formula_weight         1481.53
_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                 107.394(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2177(10)
_cell_length_b                   7.4551(4)
_cell_length_c                   23.3788(13)
_cell_measurement_reflns_used    5873
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      26.436
_cell_measurement_theta_min      2.678
_cell_volume                     2531.0(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20817
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.466
_diffrn_reflns_theta_min         2.678
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0814 before and 0.0719 after correction.
The Ratio of minimum to maximum transmission is 0.8314.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       needle
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0296P)^2^+6.2142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4264
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00577e2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7715696--7715701.cif.'
_cod_database_code               7715697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.700
_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. Restrained distances
 Gd1-H4WB
 2.85 with sigma of 0.02
3.a Free rotating group:
 O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB), O9W(H9WA,H9WB)
3.b Rotating group:
 O4W(H4WA,H4WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB), O5W(H5WA,H5WB), O2W(H2WA,H2WB)
3.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              69321
_olex2_submission_special_instructions 'No special instructions were received'