Spontaneous Generation of Stable Pnictinyl Radicals from "Jack-in-the-Box" Dipnictines: A Solid-State, Gas-Phase, and Theoretical Investigation of the Origins of Steric Stabilization1
Sarah L. Hinchley; Carole A. Morrison; David W. H. Rankin; Charles L. B. Macdonald; Robert J. Wiacek; Andreas Voigt; Alan H. Cowley; Michael F. Lappert; Grete Gundersen; Jason A. C. Clyburne; Philip P. Power; Journal of the American Chemical Society 123 (2001) 9045–9053; doi:10.1021/ja010615b

data_4115687
_publ_section_title
;
 Spontaneous Generation of Stable Pnictinyl Radicals from
 "Jack-in-the-Box" Dipnictines: A Solid-State, Gas-Phase, and Theoretical
 Investigation of the Origins of Steric Stabilization1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9045
_journal_page_last               9053
_journal_paper_doi               10.1021/ja010615b
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        selfmade
_chemical_formula_analytical     'C14 H38 Cl P Si4'
_chemical_formula_moiety         'C14 H38 Cl P Si4'
_chemical_formula_structural     'C14 H38 Cl P Si4'
_chemical_formula_sum            'C14 H38 Cl P Si4'
_chemical_formula_weight         385.22
_chemical_name_common            bis(disyl)chlorophosphine
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3190(10)
_cell_length_b                   12.406(2)
_cell_length_c                   20.453(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      10.0
_cell_volume                     2355.3(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       '\w 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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6906
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 96
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.96968
_exptl_absorpt_correction_T_min  0.56222
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0931
_refine_ls_wR_factor_obs         0.0806
_reflns_number_observed          3955
_reflns_number_total             5392
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010615b_1.cif
_cod_data_source_block           jason5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.7125P] 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^)+(0.0375P)^2^+0.7125P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115687