Rotational barriers of biphenyls having heavy heteroatoms as ortho-substituents: experimental and theoretical determination of steric effects.
Lunazzi, Lodovico; Mancinelli, Michele; Mazzanti, Andrea; Lepri, Susan; Ruzziconi, Renzo; Schlosser, Manfred; Organic & biomolecular chemistry 10 (2012) 1847–1855; doi:10.1039/c1ob06688a

data_7152192
_publ_section_title
;
 Rotational barriers of biphenyls having heavy heteroatoms as
 ortho-substituents: experimental and theoretical determination of steric
 effects.
;
_journal_issue                   9
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1847
_journal_page_last               1855
_journal_paper_doi               10.1039/c1ob06688a
_journal_volume                  10
_journal_year                    2012
_chemical_formula_sum            'C29 H31 O0.47 P Si'
_chemical_formula_weight         446.12
_chemical_name_common            'compound 9'
_chemical_name_systematic
;
3-(Dimethylisopropylsilyl)biphenyl-2-yl]diphenylphosphine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12/11/2010
_audit_creation_method           SHELXL-97
_audit_update_record             09/29/2011
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3538(14)
_cell_length_b                   11.1227(12)
_cell_length_c                   18.446(2)
_cell_measurement_temperature    296(2)
_cell_volume                     2533.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD are a detector'
_diffrn_measurement_method       'phi and omega 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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25500
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.9503
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             951
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0566P)^2^+1.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                4337
_reflns_number_total             4987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ob06688a.txt
_cod_data_source_block           b5_f
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7152192