Reactivity of Tin(II) Guanidinate with 1,2- and 1,3-Diones: Oxidative Cycloaddition or Ligand Substitution ?
Chlupatý, Tomáš; Růžičková, Zdeňka; Horáček, Michal; Merna, Jan; Alonso, Mercedes; De Proft, Frank; Růžička, Aleš; Organometallics 34 (2015) 2202–; doi:10.1021/om500873a

data_4084619
_publ_section_title
;
 Reactivity of Tin(II) Guanidinate with 1,2- and 1,3-Diones: Oxidative
 Cycloaddition or Ligand Substitution ?
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2202
_journal_paper_doi               10.1021/om500873a
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C28 H30 F3 N3 O2 Si Sn'
_chemical_formula_sum            'C28 H30 F3 N3 O2 Si Sn'
_chemical_formula_weight         644.33
_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                100.708(4)
_cell_angle_beta                 101.886(4)
_cell_angle_gamma                102.090(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0430(4)
_cell_length_b                   11.5469(7)
_cell_length_c                   11.8801(6)
_cell_measurement_reflns_used    33091
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1407.40(13)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32985
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                6027
_reflns_number_total             6444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500873a_si_001.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4084614--4084619.cif.'
_cod_database_code               4084619