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_7062504
_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         'C23 H23 N3 O2 Sn'
_chemical_formula_sum            'C23 H23 N3 O2 Sn'
_chemical_formula_weight         492.13
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.794(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9435(3)
_cell_length_b                   15.3162(6)
_cell_length_c                   14.8791(6)
_cell_measurement_reflns_used    6114
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.8650
_cell_measurement_theta_min      4.1500
_cell_volume                     2019.32(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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   -120.00 -30.00   0.50    5.00    --  -48.70 -70.00  17.00  180
  2  \w    -67.00  24.00   0.50    5.00    --  -48.70  70.00 148.00  182
  3  \w    -22.00  67.00   0.50    5.00    --   48.70 -70.00  17.00  178
  4  \w    -87.00 -14.00   0.50   20.00    --  -86.25  70.00 148.00  146
  5  \w   -137.00-112.00   0.50   20.00    --  -86.25 -70.00  17.00   50
  6  \w     89.00 130.00   0.50   20.00    --  107.75  70.00 148.00   82
  7  \w     41.00  87.00   0.50   20.00    --  107.75 -70.00  17.00   92
  8  \w   -117.00 -74.00   0.50    5.00    --  -48.70-125.00-180.00   86
  9  \w     30.00  76.00   0.50    5.00    --   48.70  70.00 148.00   92
 10  \w     38.00  93.00   0.50    5.00    --   48.70-125.00   0.00  110
 11  \w    -43.00 -17.00   0.50   20.00    --  -86.25  45.00 -30.00   52
 12  \w     40.00  96.00   0.50   20.00    --  107.75-111.00  96.59  112
 13  \w     37.00  63.00   0.50   20.00    --  107.75 -80.00  93.98   52
 14  \w    128.00 153.00   0.50   20.00    --  107.75  45.00  90.00   50
 15  \w    107.00 139.00   0.50   20.00    --  107.75  61.00-180.00   64
 16  \w     39.00  69.00   0.50   20.00    --  107.75 -61.00  90.00   60
 17  \w    147.00 176.00   0.50   20.00    --  107.75  61.00-180.00   58
 18  \w     73.00 103.00   0.50   20.00    --  107.75 -77.00   0.00   60
 19  \w    102.00 127.00   0.50   20.00    --  107.75  30.00-120.00   50
 20  \w    130.00 176.00   0.50   20.00    --  107.75  30.00-120.00   92
 21  \w     36.00  61.00   0.50   20.00    --  107.75 -61.00 120.00   50
 22  \w    122.00 176.00   0.50   20.00    --  107.75 117.00  73.77  108
 23  \w     42.00  69.00   0.50   20.00    --  107.75-125.00 -30.00   54
 24  \w    106.00 146.00   0.50   20.00    --  107.75  74.00-116.13   80
 25  \w     39.00  74.00   0.50   20.00    --  107.75-103.00 120.30   70
 26  \w     41.00  71.00   0.50   20.00    --  107.75 -61.00 150.00   60
 27  \w     40.00  97.00   0.50   20.00    --  107.75-113.00  37.84  114
 28  \w     99.00 151.00   0.50   20.00    --  107.75  30.00 120.00  104
 29  \w     70.00 128.00   0.50   20.00    --  107.75 -85.00-107.05  116
 30  \w     37.00  66.00   0.50   20.00    --  107.75 -61.00  60.00   58
 31  \w     55.00 104.00   0.50   20.00    --  107.75 -95.00-180.00   98
 32  \w     86.00 136.00   0.50   20.00    --  107.75  77.00 -30.00  100
 33  \w    140.00 165.00   0.50   20.00    --  107.75  77.00 -30.00   50
 34  \w     37.00  63.00   0.50   20.00    --  107.75 -77.00-150.00   52
 35  \w     42.00  67.00   0.50   20.00    --  107.75 -77.00 -60.00   50
 36  \w     74.00 100.00   0.50   20.00    --  107.75 -77.00 -60.00   52
 37  \w     54.00 103.00   0.50   20.00    --  107.75 -95.00 120.00   98
 38  \w    118.00 177.00   0.50   20.00    --  107.75  15.00 -30.00  118
 39  \w     87.00 117.00   0.50   20.00    --  107.75 -80.00  93.98   60
 40  \w     97.00 135.00   0.50   20.00    --  107.75  30.00 150.00   76
 41  \w     46.00  72.00   0.50   20.00    --  107.75 -95.00 -90.00   52
 42  \w     50.00  76.00   0.50   20.00    --  107.75-118.00 -78.66   52
 43  \w     83.00 109.00   0.50   20.00    --  107.75-118.00 -78.66   52
 44  \w     45.00  71.00   0.50   20.00    --  107.75-125.00-120.00   52
 45  \w     62.00  88.00   0.50   20.00    --  107.75-125.00 120.00   52
 46  \w    103.00 129.00   0.50   20.00    --  107.75 125.00   0.00   52
 47  \w    142.00 168.00   0.50   20.00    --  107.75 125.00   0.00   52
 48  \w     99.00 126.00   0.50   20.00    --  107.75  61.00   0.00   54
 49  \w    137.00 174.00   0.50   20.00    --  107.75  61.00   0.00   74
 50  \w     45.00  71.00   0.50   20.00    --  107.75 -61.00-120.00   52
;
_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      -0.0362837000
_diffrn_orient_matrix_UB_12      0.0091145000
_diffrn_orient_matrix_UB_13      0.0978945000
_diffrn_orient_matrix_UB_21      -0.1019649000
_diffrn_orient_matrix_UB_22      0.0786608000
_diffrn_orient_matrix_UB_23      -0.0290025000
_diffrn_orient_matrix_UB_31      -0.1360622000
_diffrn_orient_matrix_UB_32      -0.0619583000
_diffrn_orient_matrix_UB_33      -0.0224764000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.969
_diffrn_reflns_theta_min         4.162
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+1.4427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3910
_reflns_number_total             4290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01993d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7062503--7062507.cif.'
_cod_database_code               7062504
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sn O2 N3 C23 H29'
_chemical_oxdiff_usercomment     702016_msyr
_shelx_estimated_absorpt_t_max   0.578
_shelx_estimated_absorpt_t_min   0.349
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              29368
_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 1.847
_oxdiff_exptl_absorpt_empirical_full_min 0.621