Hydrostannylation of Ketones and Alkynes with LSnH [L = HC(CMeNAr)2, Ar = 2,6-iPr2C6H3]
Anukul Jana; Herbert W. Roesky; Carola Schulzke; Inorganic Chemistry 48 (2009) 9543–9548; doi:10.1021/ic9012069

data_4303299
_publ_section_title
;
Hydrostannylation of Ketones and Alkynes with LSnH [L = HC(CMeNAr)2, Ar =
2,6-iPr2C6H3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9543
_journal_page_last               9548
_journal_paper_doi               10.1021/ic9012069
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C33 H46 N2 O2 Sn'
_chemical_formula_weight         621.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.84(3)
_cell_angle_beta                 93.10(3)
_cell_angle_gamma                108.12(3)
_cell_formula_units_Z            2
_cell_length_a                   11.067(2)
_cell_length_b                   12.259(3)
_cell_length_c                   13.922(3)
_cell_measurement_reflns_used    14660
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.1
_cell_measurement_theta_min      3.3
_cell_volume                     1575.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  IPDSII
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14660
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.8350
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.493
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                5889
_reflns_number_total             6731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012069_si_001_3.cif
_cod_data_source_block           ja36
_cod_original_cell_volume        1575.4(6)
_cod_database_code               4303299