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_4115381
_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 As '
_chemical_formula_sum            'C45 H69 As'
_chemical_formula_weight         684.96
_chemical_melting_point          418(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                99.54(1)
_cell_angle_beta                 110.68(1)
_cell_angle_gamma                107.37(2)
_cell_formula_units_Z            4
_cell_length_a                   17.686(2)
_cell_length_b                   18.44(1)
_cell_length_c                   14.890(2)
_cell_measurement_temperature    123.2
_cell_volume                     4131(2)
_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 0.8343
_diffrn_measured_fraction_theta_max 0.8343
_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  0.033
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15947
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.75
_refine_diff_density_min         -1.08
_refine_ls_extinction_coef       0.0090(6)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.655
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     830
_refine_ls_number_reflns         15947
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.0015
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                13330
_reflns_number_total             15947
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja027493n-2_s2_1.cif
_cod_data_source_block           Tip3As/124K
_cod_original_cell_volume        4130(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H69 As '
_cod_database_code               4115381