An isolable stannaimine and its cycloaddition/metathesis reactions with carbon dioxide.
Evans, Matthew J.; Parr, Joseph M.; Nguyen, Dat T.; Jones, Cameron; Chemical communications (Cambridge, England) 60 (2024) 10350–10353; doi:10.1039/d4cc04006f

data_7133598
_publ_section_title
;
 An isolable stannaimine and its cycloaddition/metathesis reactions with
 carbon dioxide.
;
_journal_issue                   75
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10350
_journal_page_last               10353
_journal_paper_doi               10.1039/d4cc04006f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C49 H77 N3 O3 Si2 Sn'
_chemical_formula_weight         931.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     fmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-06 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.850(3)
_cell_length_b                   25.750(5)
_cell_length_c                   28.570(6)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.065
_cell_volume                     11660(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  MX2
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            150791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.065
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  'Value not reported by XDS'
_exptl_absorpt_correction_T_min  'Value not reported by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       colourless
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   'Value not reported by XDS'
_exptl_transmission_factor_min   'Value not reported by XDS'
_refine_diff_density_max         2.359
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 4194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         11929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1833P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10463
_reflns_number_total             11929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04006f2.cif
_cod_data_source_block           cj1689
_cod_depositor_comments
'Adding full bibliography for 7133593--7133605.cif.'
_cod_database_code               7133598
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.990
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
The unit cell contains 8 hexane solvates that were poorly ordered, such
that a suitable crystallographic model could not be derived. Consequently,
these solvates were treated as a diffuse contribution to the overall 
scattering without specific atom positions using the Olex2 implementation of
SQUEEZE (Acta Cryst. (2015). C71, 9-18), also known as Solvent Mask. 
(Acta Cryst. A 1990, A46, 194., J. Appl. Cryst., 42: 339-341. & J. Molec. 
Biol. 1994, 243, 100).
;
_shelx_res_checksum              15323
_shelx_hkl_checksum              66017
_shelx_fab_checksum              41749