Stable Radicals from Commonly Used Precursors Trichlorosi-lane and Diphenylchlorophosphine.
Roy, Sudipta; Stückl, A Claudia; Demeshko, Serhiy; Dittrich, Birger; Meyer, Jann; Maity, Bholanath; Koley, Debasis; Schwederski, Brigitte; Kaim, Wolfgang; Roesky, Herbert W.; Journal of the American Chemical Society  (2015) 150403102455008–; doi:10.1021/jacs.5b02403

data_4123545
_publ_section_title
;
 Stable Radicals from Commonly Used Precursors Trichlorosi-lane and
 Diphenylchlorophosphine.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150403102455008
_journal_paper_doi               10.1021/jacs.5b02403
_journal_year                    2015
_chemical_formula_moiety         'C32 H41 Cl2 N P Si'
_chemical_formula_sum            'C32 H41 Cl2 N P Si'
_chemical_formula_weight         569.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 101.258(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3343(10)
_cell_length_b                   11.2426(7)
_cell_length_c                   16.7723(11)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.4184
_cell_measurement_theta_min      2.7583
_cell_volume                     3020.8(3)
_computing_molecular_graphics    'H\"ubschle, (2011)'
_computing_publication_material  'L\"ubben, (to be published)'
_computing_structure_refinement
;
SHELXL-2014/6 (Sheldrick, 2014)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART 6000 Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            109809
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.417
_diffrn_reflns_theta_min         2.758
_exptl_absorpt_coefficient_mu    2.967
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2014/1, multi-scan. (G. M. Sheldrick, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.023
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+5.5902P
] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4955
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b02403_si_004.cif
_cod_data_source_block           sr94
_cod_database_code               4123545
_shelx_res_checksum              10440
_shelxl_version_number           2014/6
_shelx_hkl_checksum              55371