N,N-Addition of Frustrated Lewis Pairs to Nitric Oxide: An Easy Entry to a Unique Family of Aminoxyl Radicals
Muhammad Sajid; Annika Stute; Allan Jay P. Cardenas; Brooks J. Culotta; Johannes A. M. Hepperle; Timothy H. Warren; Birgitta Schirmer; Stefan Grimme; Armido Studer; Constantin G. Daniliuc; Roland Fröhlich; Jeffrey L. Petersen; Gerald Kehr; Gerhard Erker; Journal of the American Chemical Society 134 (2012) 10156–10168; doi:10.1021/ja302652a

data_4118089
_publ_section_title
;
 N,N-Addition of Frustrated Lewis Pairs to Nitric Oxide: An Easy Entry to
 a Unique Family of Aminoxyl Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10156
_journal_page_last               10168
_journal_paper_doi               10.1021/ja302652a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C41 H45 B F10 N O P'
_chemical_formula_weight         799.56
_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   'at O1 from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.147(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4646(2)
_cell_length_b                   10.6452(1)
_cell_length_c                   20.7316(2)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     3853.53(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f 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  0.069
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41168
_diffrn_reflns_theta_full        66.94
_diffrn_reflns_theta_max         66.94
_diffrn_reflns_theta_min         4.67
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.8990
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+2.5771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                5252
_reflns_number_total             6761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302652a_si_006.cif
_cod_data_source_block           erk5996
_cod_database_code               4118089