Syntheses and exploration of the catalytic activities of organotin(IV) compounds.
Kumar, Manish; Nayek, Hari Pada; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9827–9837; doi:10.1039/d4dt00646a

data_7716050
_publ_section_title
;
 Syntheses and exploration of the catalytic activities of organotin(IV)
 compounds.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9827
_journal_page_last               9837
_journal_paper_doi               10.1039/d4dt00646a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H26 N2 O4 Sn'
_chemical_formula_sum            'C29 H26 N2 O4 Sn'
_chemical_formula_weight         585.21
_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             2023-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                64.844(4)
_cell_angle_beta                 65.315(3)
_cell_angle_gamma                66.761(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4626(3)
_cell_length_b                   12.2766(4)
_cell_length_c                   12.4511(5)
_cell_measurement_reflns_used    11091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3460
_cell_measurement_theta_min      3.0630
_cell_volume                     1268.69(9)
_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 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 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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -51.00  18.00   1.00   20.00    --   13.76 -19.00-150.00   69
  2  \w    -11.00  33.00   1.00   20.00    --   13.76  77.00-120.00   44
  3  \w     -1.00  77.00   1.00   20.00    --   13.76  57.00  60.00   78
  4  \w    -56.00  83.00   1.00   20.00    --   13.76   0.00 -90.00  139
  5  \w     -8.00  42.00   1.00   20.00    --   13.76  77.00 150.00   50
  6  \w     -4.00  82.00   1.00   20.00    --   13.76  38.00 -30.00   86
  7  \w    -23.00  44.00   1.00   20.00    --  -15.95  19.00-150.00   67
  8  \w    -72.00 -30.00   1.00   20.00    --  -15.95 131.00 -94.90   42
  9  \w    -73.00  -9.00   1.00   20.00    --  -15.95 132.00  37.92   64
 10  \w    -80.00 -45.00   1.00   20.00    --  -15.95 143.00 148.62   35
;
_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      0.0602618000
_diffrn_orient_matrix_UB_12      -0.0489545000
_diffrn_orient_matrix_UB_13      0.0161152000
_diffrn_orient_matrix_UB_21      0.0124210000
_diffrn_orient_matrix_UB_22      -0.0204824000
_diffrn_orient_matrix_UB_23      -0.0497432000
_diffrn_orient_matrix_UB_31      0.0468818000
_diffrn_orient_matrix_UB_32      0.0395381000
_diffrn_orient_matrix_UB_33      -0.0402487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19775
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.900
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43490
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4778
_reflns_number_total             5491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00646a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7716050--7716055.cif.'
_cod_database_code               7716050
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H52 N4 O8 Sn2 '
_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
Uanis(C16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 C14, C16
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29)
4.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              36388
_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 1.853
_oxdiff_exptl_absorpt_empirical_full_min 0.721