1-(2,4,6-Tri-tert-butylphenyl)-3-methylphosphole: A Phosphole with a Significantly Flattened Phosphorus Pyramid Having Pronounced Characteristics of Aromaticity
György Keglevich; Zsolt Böcskei; György Miklós Keserü; Kálmán Újszászy; Louis D. Quin; Journal of the American Chemical Society 119 (1997) 5095–5099; doi:10.1021/ja970463d

data_4116979
_publ_section_title
;
 1-(2,4,6-Tri-tert-butylphenyl)-3-methylphosphole: A Phosphole with a
 Significantly Flattened Phosphorus Pyramid Having Pronounced
 Characteristics of Aromaticity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5095
_journal_page_last               5099
_journal_paper_doi               10.1021/ja970463d
_journal_volume                  119
_journal_year                    1997
_chemical_formula_moiety         'C23 H35 P'
_chemical_formula_sum            'C23 H35 P'
_chemical_formula_weight         342.48
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.137(4)
_cell_length_b                   22.327(5)
_cell_length_c                   9.149(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      58.0
_cell_measurement_theta_min      40.3
_cell_volume                     4317.6(16)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2797
_diffrn_reflns_theta_max         62.57
_diffrn_reflns_theta_min         3.96
_diffrn_standards_decay_%        1.14
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    none
_exptl_crystal_description       column
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.1961
_refine_ls_R_factor_obs          0.0729
_refine_ls_shift/esd_max         0.161
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+12.1607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2797
_refine_ls_wR_factor_obs         0.1854
_reflns_number_observed          1215
_reflns_number_total             2797
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja970463d.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+12.1607P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+12.1607P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4317.5(16)
_cod_database_code               4116979