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_4084615
_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         'C48 H64 Cl4 N6 O2 Si4 Sn, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H80 Cl4 N6 O4 Si4 Sn'
_chemical_formula_weight         1274.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 95.699(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.794(3)
_cell_length_b                   12.0940(10)
_cell_length_c                   23.9110(19)
_cell_measurement_reflns_used    42486
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     6271.2(11)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42427
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.107
_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     676
_refine_ls_number_reflns         13164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0136P)^2^+18.8361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                9716
_reflns_number_total             13164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500873a_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084614--4084619.cif.'
_cod_original_cell_volume        6271.2(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4084615