N-Heterocyclic carbenes versus transition metals for stabilizing phosphinyl radicals
Back, Olivier; Donnadieu, Bruno; von Hopffgarten, Moritz; Klein, Susanne; Tonner, Ralf; Frenking, Gernot; Bertrand, Guy; Chemical Science 2 (2011) 858–; doi:10.1039/c1sc00027f

data_1515554
_publ_section_title
;
 N-Heterocyclic carbenes versus transition metals for stabilizing
 phosphinyl radicals
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              858
_journal_paper_doi               10.1039/c1sc00027f
_journal_volume                  2
_journal_year                    2011
_chemical_formula_sum            'C66 H98 N7 P V'
_chemical_formula_weight         1071.42
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.889(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.516(6)
_cell_length_b                   22.439(11)
_cell_length_c                   25.370(12)
_cell_measurement_reflns_used    1784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      2.40
_cell_volume                     6477(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.2194
_diffrn_reflns_av_sigmaI/netI    0.1918
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28265
_diffrn_reflns_theta_full        21.17
_diffrn_reflns_theta_max         21.17
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.9740
_exptl_absorpt_correction_T_min  0.9470
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00117(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         6944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                3430
_reflns_number_total             6944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00027f.txt
_cod_data_source_block           shelxl_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1515554