Derivatives of penta-, hexa-, and hepta-coordinated tin with Schiff bases and 1,10-phenanthroline: structure, redox and optoelectronic properties
Krylova, Irina V.; Labutskaya, Liliya D.; Markova, Mariya O.; Balycheva, Victoriya A.; Shangin, Pavel G.; Akyeva, Anna Ya.; Golovina, Victoriya V.; Minyaev, Mikhail E.; Lalov, Andrey V.; Pechennikov, Valery M.; Novikov, Vasiliy T.; Egorov, Mikhail P.; Syroeshkin, Mikhail A.; New Journal of Chemistry 47 (2023) 11890–11902; doi:10.1039/D3NJ01993D

data_7062505
_publ_section_title
;
 Derivatives of penta-, hexa-, and hepta-coordinated tin with Schiff bases
 and 1,10-phenanthroline: structure, redox and optoelectronic properties
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11890
_journal_page_last               11902
_journal_paper_doi               10.1039/D3NJ01993D
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C24 H24 N2 O2 Sn'
_chemical_formula_sum            'C24 H24 N2 O2 Sn'
_chemical_formula_weight         491.14
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-02-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                78.4367(7)
_cell_angle_beta                 76.9185(7)
_cell_angle_gamma                88.6387(6)
_cell_formula_units_Z            4
_cell_length_a                   10.45872(9)
_cell_length_b                   10.81132(8)
_cell_length_c                   18.91626(17)
_cell_measurement_reflns_used    61624
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      36.0030
_cell_measurement_theta_min      4.1310
_cell_volume                     2040.59(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_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      5.00  41.00   0.25    5.00    --   18.02-114.00-161.00  144
  2  \w    -76.00 -51.00   0.25    5.00    --  -17.71 145.00  91.91  100
  3  \w    -59.00 -27.00   0.25    5.00    --  -17.71 114.00 176.87  128
  4  \w    -60.00 -28.00   0.25    5.00    --  -17.71 116.00 -14.23  128
  5  \w    -32.00  53.00   0.25    5.00    --  -17.71  57.00-180.00  340
  6  \w    -59.00 -32.00   0.25    5.00    --  -17.71 114.00  27.28  108
  7  \w    -40.00  21.00   0.25    5.00    --  -17.71  78.00 112.12  244
  8  \w    -88.00 -13.00   0.25    5.00    --  -17.71 -38.00-180.00  300
  9  \w    -59.00 -34.00   0.25    5.00    --  -17.71 114.00-156.40  100
 10  \w    -90.00 -57.00   0.25    5.00    --  -17.71 -57.00  90.00  132
 11  \w    -43.00  -4.00   0.25    5.00    --  -17.71 -57.00  90.00  156
 12  \w    -84.00 -11.00   0.25    5.00    --  -17.71 -38.00  90.00  292
 13  \w    -59.00 -34.00   0.25    5.00    --  -17.71 114.00-121.83  100
 14  \w    -55.00 -30.00   0.25    5.00    --  -17.71 108.00 -27.83  100
 15  \w    -59.00 -34.00   0.25    5.00    --  -17.71 114.00 133.39  100
 16  \w    -90.00  -4.00   0.25    5.00    --  -17.71 -57.00 -30.00  344
 17  \w    -59.00 -26.00   0.25    5.00    --  -17.71 114.00 -99.93  132
 18  \w      6.00  79.00   0.25    5.00    --   18.02  57.00 -90.00  292
 19  \w      0.00  90.00   0.25    5.00    --   18.02  77.00  90.00  360
 20  \w     42.00  89.00   0.25    5.00    --   18.02 178.00   0.00  188
 21  \w    -55.00   2.00   0.25    5.00    --   18.02 -19.00  60.00  228
 22  \w     -1.00  87.00   0.25    5.00    --   18.02  77.00 -30.00  352
 23  \w    -53.00  40.00   0.25    5.00    --   18.02 -77.00   0.00  372
 24  \w     31.00  57.00   0.25    5.00    --   18.02-113.00-161.00  104
 25  \w     47.00  88.00   0.25    5.00    --   18.02 178.00  30.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0502523000
_diffrn_orient_matrix_UB_12      -0.0465169000
_diffrn_orient_matrix_UB_13      0.0168239000
_diffrn_orient_matrix_UB_21      0.0156351000
_diffrn_orient_matrix_UB_22      -0.0023059000
_diffrn_orient_matrix_UB_23      0.0348172000
_diffrn_orient_matrix_UB_31      -0.0456124000
_diffrn_orient_matrix_UB_32      0.0481420000
_diffrn_orient_matrix_UB_33      0.0069717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.932
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         33922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0653P)^2^+0.1965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30984
_reflns_number_total             33922
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9940\% 
around [-0.68 0.73 -0.02] (reciprocal) or [-0.71 0.71 0.00] (direct)
;
_cod_data_source_file            d3nj01993d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7062503--7062507.cif.'
_cod_original_cell_volume        2040.60(3)
_cod_database_code               7062505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H24 N2 O2 Sn'
_chemical_oxdiff_usercomment     625015
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5241(4)
 0.4759(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C23A(H23A,H23B), C21B(H21C,H21D), C23B(H23C,H23D)
3.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C14A(H14A), C16A(H16A), C17A(H17A), C18A(H18A),
 C19A(H19A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C7B(H7B), C9B(H9B),
 C10B(H10B), C11B(H11B), C12B(H12B), C14B(H14B), C16B(H16B), C17B(H17B),
 C18B(H18B), C19B(H19B)
3.c Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C24A(H24A,H24B,H24C), C22B(H22D,H22E,H22F), C24B(H24D,
 H24E,H24F)
;
_shelx_res_checksum              24429
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.767
_oxdiff_exptl_absorpt_empirical_full_min 0.612
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2