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_7716052
_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         'C25 H34 N2 O4 Sn'
_chemical_formula_sum            'C25 H34 N2 O4 Sn'
_chemical_formula_weight         545.270
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.04.08 svn.rfee37e2d for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.075(4)
_cell_angle_beta                 110.462(5)
_cell_angle_gamma                111.715(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3748(7)
_cell_length_b                   10.7560(6)
_cell_length_c                   13.2715(6)
_cell_measurement_reflns_used    3869
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9360
_cell_measurement_theta_min      2.8260
_cell_volume                     1274.47(15)
_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-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_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  86.00   1.00   17.82    --   14.53 178.00  60.00   47
  2  \w     17.00  53.00   1.00   17.82    --   14.53 -99.00 -90.00   36
  3  \w    -12.00  13.00   1.00   17.82    --   14.53  77.00-120.00   25
  4  \w    -12.00  37.00   1.00   17.82    --   14.53  77.00  90.00   49
  5  \w    -66.00  40.00   1.00   17.82    --  -16.64  -4.00 134.00  106
  6  \w    -35.00   5.00   1.00   17.82    --  -16.64 -77.00 -30.00   40
  7  \w    -78.00   1.00   1.00   17.82    --  -16.64 -38.00  90.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.1125
_diffrn_reflns_Laue_measured_fraction_full 0.9998
_diffrn_reflns_Laue_measured_fraction_max 0.9998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11420
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.9998
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56734
_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    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             559.089
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8753
_refine_diff_density_min         -0.7555
_refine_diff_density_rms         0.1467
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.8795
_refine_ls_goodness_of_fit_ref   0.8868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4491
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      0.8648
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3130
_reflns_number_total             4491
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00646a2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7716050--7716055.cif.'
_cod_database_code               7716052
_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. Restrained distances
 C22-C23A \\sim C22A-C23B
 with sigma of 0.02
 C22-Sn1 \\sim C22A-Sn1
 with sigma of 0.02
 C23A-H23a \\sim C23B-H23c
 with sigma of 0.02
 C23A-H23b \\sim C23B-H23d
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 C24A-H24a \\sim C24B-H24c
 with sigma of 0.02
 C24A-H24b \\sim C24B-H24d
 with sigma of 0.02
 C24A-C25 \\sim C24B-C25A
 with sigma of 0.02
 C25-H25a \\sim C25A-H25d
 with sigma of 0.02
 C25-H25b \\sim C25A-H25e
 with sigma of 0.02
 C25-H25c \\sim C25A-H25f
 with sigma of 0.02
 C22-H23a \\sim C22A-H23c
 with sigma of 0.04
 C22-H23b \\sim C22A-H23d
 with sigma of 0.04
 C22-C24A \\sim C22A-C24B
 with sigma of 0.04
 C23A-H24a \\sim C23B-H24c
 with sigma of 0.04
 C23A-H24b \\sim C23B-H24d
 with sigma of 0.04
 C23A-C25 \\sim C23B-C25A
 with sigma of 0.04
 C23A-Sn1 \\sim C23B-Sn1
 with sigma of 0.04
 H23a-H23b \\sim H23c-H23d
 with sigma of 0.04
 H23a-C24A \\sim H23c-C24B
 with sigma of 0.04
 H23b-C24A \\sim H23d-C24B
 with sigma of 0.04
 C24A-H25a \\sim C24B-H25d
 with sigma of 0.04
 C24A-H25b \\sim C24B-H25e
 with sigma of 0.04
 C24A-H25c \\sim C24B-H25f
 with sigma of 0.04
 H24a-H24b \\sim H24c-H24d
 with sigma of 0.04
 H24a-C25 \\sim H24c-C25A
 with sigma of 0.04
 H24b-C25 \\sim H24d-C25A
 with sigma of 0.04
 H25a-H25b \\sim H25d-H25e
 with sigma of 0.04
 H25a-H25c \\sim H25d-H25f
 with sigma of 0.04
 H25b-H25c \\sim H25e-H25f
 with sigma of 0.04
 C10-C14 \\sim C10-C14a
 with sigma of 0.02
 C14-C15 \\sim C14a-C15a
 with sigma of 0.02
 C15-H15a \\sim C15a-H15d
 with sigma of 0.02
 C15-H15b \\sim C15a-H15e
 with sigma of 0.02
 C15-H15c \\sim C15a-H15f
 with sigma of 0.02
 C10-C15 \\sim C10-C15a
 with sigma of 0.04
 C14-H15a \\sim C14a-H15d
 with sigma of 0.04
 C14-H15b \\sim C14a-H15e
 with sigma of 0.04
 C14-H15c \\sim C14a-H15f
 with sigma of 0.04
 H15a-H15b \\sim H15d-H15e
 with sigma of 0.04
 H15a-H15c \\sim H15d-H15f
 with sigma of 0.04
 H15b-H15c \\sim H15e-H15f
 with sigma of 0.04
 C14-C17 \\sim C14a-C17a
 with sigma of 0.02
 C17-H17a \\sim C17a-H17d
 with sigma of 0.02
 C17-H17b \\sim C17a-H17e
 with sigma of 0.02
 C17-H17c \\sim C17a-H17f
 with sigma of 0.02
 C10-C17 \\sim C10-C17a
 with sigma of 0.04
 C14-H17a \\sim C14a-H17d
 with sigma of 0.04
 C14-H17b \\sim C14a-H17e
 with sigma of 0.04
 C14-H17c \\sim C14a-H17f
 with sigma of 0.04
 C15-C17 \\sim C15a-C17a
 with sigma of 0.04
 H17a-H17b \\sim H17d-H17e
 with sigma of 0.04
 H17a-H17c \\sim H17d-H17f
 with sigma of 0.04
 H17b-H17c \\sim H17e-H17f
 with sigma of 0.04
 C14-C16 \\sim C14a-C16a
 with sigma of 0.02
 C16-H16a \\sim C16a-H16d
 with sigma of 0.02
 C16-H16b \\sim C16a-H16e
 with sigma of 0.02
 C16-H16c \\sim C16a-H16f
 with sigma of 0.02
 C10-C16 \\sim C10-C16a
 with sigma of 0.04
 C14-H16a \\sim C14a-H16d
 with sigma of 0.04
 C14-H16b \\sim C14a-H16e
 with sigma of 0.04
 C14-H16c \\sim C14a-H16f
 with sigma of 0.04
 C15-C16 \\sim C15a-C16a
 with sigma of 0.04
 C16-C17 \\sim C16a-C17a
 with sigma of 0.04
 H16a-H16b \\sim H16d-H16e
 with sigma of 0.04
 H16a-H16c \\sim H16d-H16f
 with sigma of 0.04
 H16b-H16c \\sim H16e-H16f
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14a) = Uanis(C14)
4. Rigid body (RIGU) restrains
 C23A, C22, C24A, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C22A, C23B, C24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C14a, C15a, C16a, C17a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C22A)=Sof(H22c)=Sof(H22d)=Sof(C23B)=Sof(H23c)=Sof(H23d)=Sof(C24B)=
 Sof(H24c)=Sof(H24d)=Sof(C25A)=Sof(H25d)=Sof(H25e)=Sof(H25f)=1-FVAR(1)
 Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(C23A)=Sof(H23a)=Sof(H23b)=Sof(C24A)=
 Sof(H24a)=Sof(H24b)=Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(H25c)=FVAR(1)
 Sof(C14a)=Sof(C15a)=Sof(H15d)=Sof(H15e)=Sof(H15f)=Sof(C17a)=Sof(H17d)=
 Sof(H17e)=Sof(H17f)=Sof(C16a)=Sof(H16d)=Sof(H16e)=Sof(H16f)=1-FVAR(2)
 Sof(C14)=Sof(C15)=Sof(H15a)=Sof(H15b)=Sof(H15c)=Sof(C16)=Sof(H16a)=Sof(H16b)=
 Sof(H16c)=Sof(C17)=Sof(H17a)=Sof(H17b)=Sof(H17c)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b), C22(H22a,H22b), C23A(H23a,
 H23b), C24A(H24a,H24b), C22A(H22c,H22d), C23B(H23c,H23d), C24B(H24c,H24d)
6.b Me refined with riding coordinates:
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C21(H21a,H21b,
 H21c), C15a(H15d,H15e,H15f), C17a(H17d,H17e,H17f), C16a(H16d,H16e,H16f)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12)
6.d Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C25A(H25d,H25e,H25f)
;
_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
;