Synthesis, Structure, and Redox Properties of the Extremely Crowded Triarylpnictogens: Tris(2,4,6-triisopropylphenyl)phosphine, Arsine, Stibine, and Bismuthine
Shigeru Sasaki; Katsuhide Sutoh; Fumiki Murakami; Masaaki Yoshifuji; Journal of the American Chemical Society 124 (2002) 14830–14831; doi:10.1021/ja027493n

data_4115382
_publ_contact_author_address
;
    Department of Chemistry, Graduate School of Science, Tohoku University,
 Aoba, Sendai 980-8578, Japan
;
_publ_contact_author_email       ' sasaki@mail.cc.tohoku.ac.jp '
_publ_contact_author_fax         ' 81-22-217-6562 '
_publ_contact_author_name        ' Shigeru Sasaki '
_publ_contact_author_phone       ' 81-22-217-6561 '
_publ_section_title
;
 Synthesis, Structure, and Redox Properties of the Extremely Crowded
 Triarylpnictogens: Tris(2,4,6-triisopropylphenyl)phosphine, Arsine,
 Stibine, and Bismuthine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14830
_journal_page_last               14831
_journal_paper_doi               10.1021/ja027493n
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C45 H69 P '
_chemical_formula_sum            'C45 H69 P'
_chemical_formula_weight         641.01
_chemical_melting_point          438(1)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                100.96(2)
_cell_angle_beta                 91.82(1)
_cell_angle_gamma                96.24(2)
_cell_formula_units_Z            2
_cell_length_a                   11.492(2)
_cell_length_b                   18.212(7)
_cell_length_c                   10.496(2)
_cell_measurement_temperature    200.2
_cell_volume                     2140.8(10)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 0.010000
_diffrn_measured_fraction_theta_full 0.8544
_diffrn_measured_fraction_theta_max 0.8544
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7248
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.750
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.49
_refine_ls_extinction_coef       0.036(10)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.664
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7248
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.0075
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00810|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                6960
_reflns_number_total             7248
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja027493n-2_s2_2.cif
_cod_data_source_block           Tip3P/200K
_cod_original_cell_volume        2140.8(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H69 P '
_cod_database_code               4115382