Solvent-free Hydrosilylation of Carbonyl Compounds Catalyzed by Organotin(IV) Compounds
Basu, Debayan; Chakraborty, Sudipta; Chakraborty, Gourav; Bhattacharya, Saptarshi; Patra, Niladri; Nayek, Hari Pada; Dalton Transactions  (2025) –; doi:10.1039/D5DT01033K

data_7718878
_publ_section_title
;
 Solvent-free Hydrosilylation of Carbonyl Compounds Catalyzed by
 Organotin(IV) Compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT01033K
_journal_year                    2025
_chemical_formula_moiety         'C26 H19 Cl2 N O2 Sn'
_chemical_formula_sum            'C26 H19 Cl2 N O2 Sn'
_chemical_formula_weight         567.01
_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
_audit_creation_date             2025-06-04
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_audit_update_record
;
2025-06-06 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                81.600(7)
_cell_angle_beta                 81.173(7)
_cell_angle_gamma                83.295(7)
_cell_formula_units_Z            2
_cell_length_a                   9.5600(8)
_cell_length_b                   10.2045(9)
_cell_length_c                   12.3475(11)
_cell_measurement_reflns_used    3422
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5440
_cell_measurement_theta_min      2.8110
_cell_volume                     1172.03(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -39.00  40.00   1.00   17.50    --   14.69 -77.00  60.00   79
  2  \w    -28.00   2.00   1.00   17.50    --  -16.80 -77.00  90.00   30
  3  \w    -33.00   9.00   1.00   17.50    --  -16.80 -77.00 -60.00   42
  4  \w    -76.00 -47.00   1.00   17.50    --  -16.80 -57.00 120.00   29
  5  \w    -40.00  10.00   1.00   17.50    --  -16.80 -77.00-180.00   50
  6  \w    -34.00  47.00   1.00   17.50    --  -16.80  57.00 -60.00   81
  7  \w    -82.00 -46.00   1.00   17.50    --  -16.80-178.00-150.00   36
  8  \w    -86.00 -13.00   1.00   17.50    --  -16.80 -38.00 150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0019276000
_diffrn_orient_matrix_UB_12      -0.0405427000
_diffrn_orient_matrix_UB_13      0.0519168000
_diffrn_orient_matrix_UB_21      -0.0731509000
_diffrn_orient_matrix_UB_22      -0.0062978000
_diffrn_orient_matrix_UB_23      0.0001988000
_diffrn_orient_matrix_UB_31      0.0183267000
_diffrn_orient_matrix_UB_32      -0.0574444000
_diffrn_orient_matrix_UB_33      -0.0272534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8550
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2578
_reflns_number_total             4127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01033k2.cif
_cod_data_source_block           1
_cod_database_code               7718878
_chemical_oxdiff_formula         'C H N O Cl Sn'
_diffrn_oxdiff_digest_frames
;
01a7396846bf03fdfcc05443a32754d2c40002790b8
;
_diffrn_oxdiff_digest_hkl
;
01335f7d83e3a8f638ed0d700555a5df431d91
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Me refined with riding coordinates:
 C14(H14A,H14B,H14C)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
;
_shelx_shelxl_version_number     2014/7
_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 1.674
_oxdiff_exptl_absorpt_empirical_full_min 0.694