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_7716055
_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         'C26 H36 N2 O5 Sn'
_chemical_formula_sum            'C26 H36 N2 O5 Sn'
_chemical_formula_weight         575.25
_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
_audit_creation_date             2024-05-04
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                112.274(5)
_cell_angle_beta                 93.904(5)
_cell_angle_gamma                96.094(4)
_cell_formula_units_Z            4
_cell_length_a                   10.3278(6)
_cell_length_b                   15.8695(8)
_cell_length_c                   17.9400(12)
_cell_measurement_reflns_used    8022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9640
_cell_measurement_theta_min      2.5590
_cell_volume                     2686.7(3)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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      2.00  51.00   1.00   52.10    --   13.76 -99.00 120.00   49
  2  \w    -82.00  -1.00   1.00   52.10    --  -15.95 -57.00 -30.00   81
  3  \w    -25.00  52.00   1.00   52.10    --  -15.95  19.00 -90.00   77
  4  \w    -42.00   9.00   1.00   52.10    --  -15.95 -77.00-120.00   51
  5  \w    -30.00   2.00   1.00   52.10    --  -15.95 -77.00 150.00   32
  6  \w    -85.00 -43.00   1.00   52.10    --  -15.95-178.00  60.00   42
  7  \w    -30.00  53.00   1.00   52.10    --  -15.95  38.00 150.00   83
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25148
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.997
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41543
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0958P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8189
_reflns_number_total             11557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00646a2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
Adding full bibliography for 7716050--7716055.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H72 N4 O10 Sn2'
_cod_original_formula_weight         1150.51
_cod_original_formula_moiety         '2(C26 H36 N2 O5 Sn)'
_cod_original_formula_units_Z            2
_cod_database_code               7716055
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.882
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C40(H40A,H40B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
2.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C52(H52A,H52B,H52C)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C28(H28), C29(H29),
 C31(H31), C33(H33), C35(H35), C37(H37)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C48(H48A,H48B,H48C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16(H16A,
 H16B,H16C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O8(H8)
;
_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
;