Temperature-dependent photoluminescence down to 77 K of organotin molecular rotors: eco-friendly synthesis, photophysical characterization, X-ray structures, and DFT studies.
Cantón-Díaz, Arelly M; Muñoz-Flores, Blanca M; Macías-Gamboa, Luis F; Moggio, Ivana; Arias, Eduardo; Turlakov, Gleb; Dias, H. V. Rasika; Colombo, Gioele; Brenna, Stefano; Jiménez-Pérez, Víctor M; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15010–15031; doi:10.1039/d4dt01518e

data_7716824
_publ_section_title
;
 Temperature-dependent photoluminescence down to 77 K of organotin
 molecular rotors: eco-friendly synthesis, photophysical characterization,
 X-ray structures, and DFT studies.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15010
_journal_page_last               15031
_journal_paper_doi               10.1039/d4dt01518e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H24 N2 O4 Sn'
_chemical_formula_sum            'C32 H24 N2 O4 Sn'
_chemical_formula_weight         619.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.065(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1091(10)
_cell_length_b                   21.6813(14)
_cell_length_c                   9.2066(6)
_cell_measurement_reflns_used    9172
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.39
_cell_measurement_wavelength     0.71073
_cell_volume                     2764.0(3)
_computing_cell_refinement       'SAINT V8.37A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_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      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1365
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            157026
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.386
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1156 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.8966.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5649
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0345P)^2^+1.8847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4785
_reflns_number_total             5649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01518e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7716823--7716824.cif.'
_cod_database_code               7716824
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C21A \\sim C22A
\\sim C23A \\sim C24A \\sim C25A \\sim C26A: within 2A with sigma of 0.05 and
sigma for terminal atoms of 0.1 within 2A
3. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26, C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C22, C23, C24, C25, C26, C21A, C22A, C23A, C24A, C25A, C26A, C21} sigma for
1-2: 0.02, 1-3: 0.04
{C21, C22, C23, C24, C25, C26, C21A, C22A, C23A, C24A, C25A, C26A} sigma for
1-2: 0.02, 1-3: 0.04
as in
{C21, C22, C23, C24, C25, C26, C21A, C22A, C23A, C24A, C25A, C26A}
5. Others
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(1)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C14(H14), C15(H15),
 C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32)
6.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              63283
_shelx_hkl_checksum              72382
_olex2_submission_special_instructions 'No special instructions were received'