Unexpectedly High Barriers to M–P Rotation in Tertiary Phobane Complexes: PhobPR Behavior That Is Commensurate withtBu2PR
Lister, Julia M.; Carreira, Monica; Haddow, Mairi F.; Hamilton, Alex; McMullin, Claire L.; Orpen, A. Guy; Pringle, Paul G.; Stennett, Tom E.; Organometallics 33 (2014) 702–; doi:10.1021/om400980e

data_4082503
_publ_section_title
;
 Unexpectedly High Barriers to M--P Rotation in Tertiary Phobane
 Complexes: PhobPR Behavior That Is Commensurate withtBu2PR
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              702
_journal_paper_doi               10.1021/om400980e
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C12 H23 P Se'
_chemical_formula_sum            'C12 H23 P Se'
_chemical_formula_weight         277.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.174(1)
_cell_angle_beta                 93.095(1)
_cell_angle_gamma                92.187(1)
_cell_formula_units_Z            2
_cell_length_a                   7.3002(2)
_cell_length_b                   9.1583(2)
_cell_length_c                   10.1355(2)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.41
_cell_volume                     629.75(3)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Apex II kappa 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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18811
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0211P)^2^+0.7742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                2761
_reflns_number_total             2897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400980e_si_002.cif
_cod_data_source_block           a7-PhobPSenBu
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082503