High-Yield Thermolytic Conversion of Imidazolium Salts into Arduengo Carbene Adducts with BF3and PF5
Tian, Chong; Nie, Wanli; Borzov, Maxim V.; Su, Pengfei; Organometallics 31 (2012) 1751–; doi:10.1021/om201086d

data_4076364
_publ_section_title
;
 High-Yield Thermolytic Conversion of Imidazolium Salts into Arduengo
 Carbene Adducts with BF3and PF5
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1751
_journal_paper_doi               10.1021/om201086d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C6 H10 F5 N2 P'
_chemical_formula_sum            'C6 H10 F5 N2 P'
_chemical_formula_weight         236.13
_chemical_name_systematic
;
(1,3-Dimethyl-1<i>H</i>-imidazolium-2-yl)methylpentafluorophosphate
;
_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                 94.799(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3723(12)
_cell_length_b                   7.5087(10)
_cell_length_c                   14.914(2)
_cell_measurement_reflns_used    3396
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.44
_cell_volume                     934.3(2)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 2007)'
_computing_data_collection       'BRUKER AXS APEX-2 v2009.5-1 (Bruker, 2007)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
SHELXTL97 (Sheldrick, 2008), OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER SMART APEXII'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4232
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.8833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         4233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0915P)^2^+0.1008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                2948
_reflns_number_total             4233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201086d_si_002.cif
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076364