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_7152193
_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 O P Si'
_chemical_formula_weight         454.60
_chemical_name_common            'compound 10'
_chemical_name_systematic
;
3-(Dimethylisopropylsilyl)biphenyl-2-yl]diphenylphosphine oxide
;
_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             12/10/2010
_audit_creation_method           SHELXL-97
_audit_update_record             09/29/2011
_cell_angle_alpha                90.00
_cell_angle_beta                 91.632(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3039(19)
_cell_length_b                   11.1280(17)
_cell_length_c                   18.544(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2538.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area 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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28424
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.9257
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0481P)^2^+0.7135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                5050
_reflns_number_total             6101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ob06688a.txt
_cod_data_source_block           b5g
_cod_original_cell_volume        2537.9(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7152193