Photophysical and optoelectronic studies of 1.06 and 13.3 μm emissive neodymium complexes
Ahmed, Zubair; Ali, Asgar; Imam, Faisal; Carvalho, Rafael S.; Cremona, Marco; New Journal of Chemistry 48 (2024) 19266–19282; doi:10.1039/D4NJ03842H

data_7063518
_publ_section_title
;
 Photophysical and optoelectronic studies of 1.06 and 13.3 \mm emissive
 neodymium complexes
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19266
_journal_page_last               19282
_journal_paper_doi               10.1039/D4NJ03842H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C66 H42 F21 Nd O8 P2 S3'
_chemical_formula_sum            'C66 H42 F21 Nd O8 P2 S3'
_chemical_formula_weight         1664.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.727(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4720(9)
_cell_length_b                   14.6171(3)
_cell_length_c                   21.3754(7)
_cell_measurement_reflns_used    11146
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5110
_cell_measurement_theta_min      3.4220
_cell_volume                     7108.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00   1.00   1.00   27.50    --  -16.52 -99.00 -60.00   26
  2  \w    -25.00  24.00   1.00   27.50    --  -16.52 -99.00  60.00   49
  3  \w     -1.00  79.00   1.00   27.50    --   17.77  57.00-150.00   80
  4  \w    -50.00  28.00   1.00   27.50    --   17.77 -57.00 -30.00   78
  5  \w    -51.00  25.00   1.00   27.50    --   17.77 -77.00  60.00   76
  6  \w     45.00  91.00   1.00   27.50    --   17.77-178.00   0.00   46
  7  \w      2.00  83.00   1.00   27.50    --   17.77  19.00 150.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33141
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.451
_diffrn_reflns_theta_min         3.417
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       Block
_exptl_crystal_F_000             3316
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         8522
_refine_ls_number_restraints     798
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0577P)^2^+8.3329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7138
_reflns_number_total             8522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03842h2.cif
_cod_data_source_block           nd_1
_cod_depositor_comments          'Adding full bibliography for 7063518.cif.'
_cod_database_code               7063518
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5-O1 = C7-O2
 1.25 with sigma of 0.02
 C38-F13
 1.33 with sigma of 0.02
 C38-F14
 1.31 with sigma of 0.02
 C38-F12
 1.32 with sigma of 0.02
 C10-F7 = C9-F3
 1.32 with sigma of 0.02
 C10-F5
 1.31 with sigma of 0.02
 C10-F6
 1.29 with sigma of 0.02
 C8-F1
 1.36 with sigma of 0.02
 C8-F2
 1.34 with sigma of 0.02
 C9-F4
 1.33 with sigma of 0.02
 C37-F11 = C36-F8 = C36-F9
 1.35 with sigma of 0.02
 C6-C7
 1.37 with sigma of 0.02
 C37-F10
 1.34 with sigma of 0.02
 C5-C6
 1.42 with sigma of 0.02
 S1-C1 = S1-C4
 1.71 with sigma of 0.02
 C1-C2 = C3-C4
 1.36 with sigma of 0.02
 C2-C3
 1.42 with sigma of 0.02
 C38-C36
 2.62 with sigma of 0.04
 C38-F10
 2.31 with sigma of 0.04
 C38-F11
 2.32 with sigma of 0.04
 C10-C8
 2.61 with sigma of 0.04
 C10-F3
 2.27 with sigma of 0.04
 C10-F4 = C8-F4
 2.32 with sigma of 0.04
 C6-C8
 2.48 with sigma of 0.04
 C7-C9
 2.6 with sigma of 0.04
 C6-O2
 2.36 with sigma of 0.04
 C8-F3
 2.34 with sigma of 0.04
 C5-C7
 2.45 with sigma of 0.04
 C7-F1
 2.4 with sigma of 0.04
 C7-F2
 2.37 with sigma of 0.04
 C37-F8 = C37-F9
 2.33 with sigma of 0.04
 S1-C2 = S1-C3
 2.54 with sigma of 0.04
 C1-C3 = C2-C4
 2.31 with sigma of 0.04
 C36-C38 \\sim C36A-C38
 with sigma of 0.04
 F14-C38 \\sim F12A-C38
 with sigma of 0.02
 F13-C38 \\sim F14A-C38
 with sigma of 0.02
 F12-C38 \\sim F13A-C38
 with sigma of 0.02
 C37-C38 \\sim C37A-C38
 with sigma of 0.02
 F11-C38 \\sim F10A-C38
 with sigma of 0.04
 F10-C38 \\sim F11A-C38
 with sigma of 0.04
 C9-F5 \\sim C9-F6 \\sim C9-F7
 with sigma of 0.04
 C36-C35A \\sim C37-C36 \\sim C38-C37 \\sim C38-C37A \\sim C37A-C36A \\sim
C36A-C35
 with sigma of 0.02
 C10-C9 \\sim C10-F5 \\sim C10-F6 \\sim C10-F7
 with sigma of 0.02
 C38-C37 \\sim C38-C37A
 with sigma of 0.02
 C38-C37A \\sim C38-C37
 with sigma of 0.02
 F5-F6 \\sim F6-F7 \\sim F7-F5
 with sigma of 0.04
 C36-C37 \\sim C36A-C37A
 with sigma of 0.02
 F8-C36 \\sim F8A-C36A
 with sigma of 0.02
 C35-C37 \\sim C35-C37A
 with sigma of 0.04
 F9-C36 \\sim F9A-C36A
 with sigma of 0.02
 C37-C36 \\sim C36-C35A
 with sigma of 0.02
 C37A-C36A \\sim C36A-C35
 with sigma of 0.02
 C35-C36 \\sim C35-C36A
 with sigma of 0.02
 F11-C37 \\sim F10A-C37A
 with sigma of 0.02
 S2-C32 \\sim S2A-C32
 with sigma of 0.02
 F10-C37 \\sim F11A-C37A
 with sigma of 0.02
 F8-C35 \\sim F8A-C35
 with sigma of 0.04
 F8-C37 \\sim F8A-C37A
 with sigma of 0.04
 F9-C37 \\sim F9A-C37A
 with sigma of 0.04
 C34-C35A \\sim C34A-C35A
 with sigma of 0.02
 F9-C35 \\sim F9A-C35
 with sigma of 0.04
 F11-C36 \\sim F10A-C36A
 with sigma of 0.04
 C37-C36A \\sim C37A-C36
 with sigma of 0.02
 O5A-C35A \\sim O5A-C35
 with sigma of 0.02
 F10-C36 \\sim F11A-C36A
 with sigma of 0.04
 S2-C29 \\sim S2A-C29
 with sigma of 0.02
 C32-C31 \\sim C32-C31A
 with sigma of 0.02
 C34-C35A \\sim C34-C35
 with sigma of 0.02
 C35A-C34A \\sim C35-C34A
 with sigma of 0.02
 C29-C30 \\sim C29-C30A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 O5A-C35A \\sim O5-C35A
 with sigma of 0.02
 F8-F9 \\sim F8A-F9A
 with sigma of 0.04
 O5A-C35 \\sim O5-C35
 with sigma of 0.02
 F11-F10 \\sim F10A-F11A
 with sigma of 0.04
 C32-C30 \\sim C32-C30A
 with sigma of 0.04
 C35-C36 \\sim C36A-C35A
 with sigma of 0.02
 C29-C31 \\sim C29-C31A
 with sigma of 0.04
 C33-C34 \\sim C33-C34A
 with sigma of 0.02
 Nd1-O5A \\sim Nd1-O5
 with sigma of 0.02
 S2-C29 \\sim S2-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30
 with sigma of 0.02
 C29-S2A \\sim C29A-S2A
 with sigma of 0.02
 C29-C30A \\sim C29A-C30A
 with sigma of 0.02
 P1-C17 \\sim P1-C17A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C17-C22 \\sim C17A-C22A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 P1-C18 \\sim P1-C18A
 with sigma of 0.04
 P1-C22 \\sim P1-C22A
 with sigma of 0.04
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C17-C21 \\sim C17A-C21A
 with sigma of 0.04
 C18-C22 \\sim C18A-C22A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C22-C20 \\sim C22A-C20A
 with sigma of 0.04
 P1-C23 \\sim P1-C23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C23-C28 \\sim C23A-C28A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
 C28-C27 \\sim C28A-C27A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 C27-C26 \\sim C27A-C26A
 with sigma of 0.02
 P1-C24 \\sim P1-C24A
 with sigma of 0.04
 P1-C28 \\sim P1-C28A
 with sigma of 0.04
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C23-C27 \\sim C23A-C27A
 with sigma of 0.04
 C24-C28 \\sim C24A-C28A
 with sigma of 0.04
 C24-C26 \\sim C24A-C26A
 with sigma of 0.04
 C28-C26 \\sim C28A-C26A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 S1-C1 \\sim S1-C4
 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.03
 C1-C3 \\sim C2-C4
 with sigma of 0.04
 S1-C2 \\sim S1-C3
 with sigma of 0.04
 C9-C7 \\sim C8-C10
 with sigma of 0.02
 C9-C10 \\sim C9-C8
 with sigma of 0.02
3. Restrained planarity
 S1, C1, C2, H2, C3, H3, C4
 with sigma of 0.1
 C23A, C24A, H24A, C25A, H25A, C26A, H26A, C27A, H27A, C28A, H28A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
S1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim O1
\\sim O2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
F8 \\sim F8A \\sim F9 \\sim F9A \\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim
F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim C36 \\sim C36A
\\sim C37 \\sim C37A \\sim C38: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O5A \\sim O5 \\sim C34A \\sim C34 \\sim C35A \\sim C35: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
S1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim C38: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C17) = Uanis(C17A)
5. Rigid body (RIGU) restrains
 S1, F1, F2, F3, F4, F5, F6, F7, O1, O2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 O5A, O5, C34A, C34, C35A, C35
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 F12, F12A, F13, F13A, F14, F14A, C38
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6. Others
 Sof(S2A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=
 Sof(O5A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C34A)=
 Sof(H34A)=Sof(C35)=Sof(C36A)=Sof(C37A)=1-FVAR(1)
 Sof(S2)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(O5)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C34)=Sof(H34)=
 Sof(C35A)=Sof(C36)=Sof(C37)=FVAR(1)
 Sof(C17A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=
 Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=1-FVAR(2)
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=FVAR(2)
 Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=1-FVAR(3)
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=FVAR(3)
 Fixed Sof: S1(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) F7(0.5)
 O1(0.5) O2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5)
 C5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) C9(0.5) C10(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C22A(H22A), C21A(H21A), C20A(H20A), C19A(H19A), C18A(H18A), C18(H18),
  C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C24A(H24A), C25(H25),
 C25A(H25A), C26(H26), C26A(H26A), C27(H27), C27A(H27A), C28(H28), C28A(H28A),
 C29(H29), C29A(H29A), C30(H30), C30A(H30A), C31(H31), C31A(H31A), C34A(H34A),
 C34(H34)
7.b Fitted hexagon refined as free rotating group:
 C17A(C22A,C21A,C20A,C19A,C18A)
;
_shelx_res_checksum              6540
_olex2_submission_special_instructions 'No special instructions were received'