Seven-Membered Cyclic Dialkylstannylene and -Plumbylene Compounds Stabilized by Agostic-type B−H···E Interactions [E = Sn, Pb]
Izod, Keith; Wills, Corinne; Clegg, William; Harrington, Ross W.; Organometallics 28 (2009) 2211–; doi:10.1021/om801189h

data_4068983
_publ_section_title
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 Seven-Membered Cyclic Dialkylstannylene and -Plumbylene Compounds
 Stabilized by Agostic-type B&#x2212;H&#x00B7;&#x00B7;&#x00B7;E
 Interactions [E = Sn, Pb]
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_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2211
_journal_paper_doi               10.1021/om801189h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C18 H52 B2 P2 Si4 Sn, C4 H10 O'
_chemical_formula_sum            'C22 H62 B2 O P2 Si4 Sn'
_chemical_formula_weight         657.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   difmap
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.220(4)
_cell_length_b                   20.048(7)
_cell_length_c                   21.707(6)
_cell_measurement_reflns_used    290
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.50
_cell_volume                     7059(4)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23985
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                2563
_reflns_number_total             4031
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om801189h_si_001.cif
_cod_data_source_block           ki315_compound10
_cod_database_code               4068983