Synthesis of Zwitterionic Group 14 Centered Complexes: Traditional Coordination and Unusual Insertion Chemistry
Weicker, Sarah A.; Dube, Jonathan W.; Ragogna, Paul J.; Organometallics 32 (2013) 6681–; doi:10.1021/om400186m

data_4081717
_publ_section_title
;
 Synthesis of Zwitterionic Group 14 Centered Complexes: Traditional
 Coordination and Unusual Insertion Chemistry
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6681
_journal_paper_doi               10.1021/om400186m
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H34 B Cl P2 Sn'
_chemical_formula_sum            'C38 H34 B Cl P2 Sn'
_chemical_formula_weight         717.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   33.107(5)
_cell_length_b                   33.107(5)
_cell_length_c                   17.609(4)
_cell_measurement_reflns_used    8470
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_volume                     16715(5)
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Cappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16894
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
'Residual electron density consistent with 18 Diethyl ether
molecules in the unit cell (1 per asymmetric unit) were treated
as a diffuse contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON. Repeated attempts to model the 
highly disordered molecule were met with failure'
;
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                5276
_reflns_number_total             8482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400186m_si_002.cif
_cod_data_source_block           1Sn
_cod_original_cell_volume        16716(5)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4081717