Anatomy of Phobanes. Diastereoselective Synthesis of the Three Isomers of n-Butylphobane and a Comparison of their Donor Properties
Monica Carreira; Manutsavin Charernsuk; Michael Eberhard; Natalie Fey; Roel van Ginkel; Alex Hamilton; Wilhelmus P. Mul; A. Guy Orpen; Hirihataya Phetmung; Paul G. Pringle; Journal of the American Chemical Society 131 (2009) 3078–3092; doi:10.1021/ja808807s

data_4103974
_publ_section_title
;
 Anatomy of Phobanes. Diastereoselective Synthesis of the Three Isomers of
 n-Butylphobane and a Comparison of their Donor Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3078
_journal_page_last               3092
_journal_paper_doi               10.1021/ja808807s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C24 H46 Cl2 P2 Pt'
_chemical_formula_sum            'C24 H46 Cl2 P2 Pt'
_chemical_formula_weight         662.54
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.866(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0791(10)
_cell_length_b                   8.1201(3)
_cell_length_c                   19.1417(10)
_cell_measurement_reflns_used    55173
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2645.4(2)
_computing_cell_refinement
; 
DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) 
;
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
; 
DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
; 
Bruker-Nonius APEX II CCD camera on \k-goniostat 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23275
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    5.637
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.695751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.639
_refine_diff_density_min         -2.113
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0000P)^2^+47.2860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                4147
_reflns_number_total             6020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808807s_si_004.cif
_cod_data_source_block           5a7_mcm97
_cod_database_code               4103974