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_4123544
_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         '2(C32 H41 N P), C7 H8, 2(Cl)'
_chemical_formula_sum            'C71 H90 Cl2 N2 P2'
_chemical_formula_weight         1104.28
_chemical_name_common            '(cAAC)P(Ph)2+ Cl-'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                74.67(3)
_cell_angle_beta                 76.59(3)
_cell_angle_gamma                62.93(3)
_cell_formula_units_Z            1
_cell_length_a                   10.128(5)
_cell_length_b                   10.623(3)
_cell_length_c                   17.485(10)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      1.062
_cell_volume                     1601.8(14)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.905
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27030
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         26.265
_diffrn_reflns_theta_min         1.062
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.8202
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2014/1, multi-scan. (G. M. Sheldrick, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0562P)^2^+0.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6957
_reflns_number_total             8846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b02403_si_002.cif
_cod_data_source_block           srcp
_cod_database_code               4123544
_shelxl_version_number           2014/6
_shelx_res_checksum              32505
_shelx_hkl_checksum              75091