Synthesis of Backbone P-Functionalized Imidazol-2-ylidene Complexes: En Route to Novel Functional Ionic Liquids
Paresh Kumar Majhi; Susanne Sauerbrey; Gregor Schnakenburg; Anthony J. Arduengo; Rainer Streubel; Inorganic Chemistry 51 (2012) 10408–10416; doi:10.1021/ic301641z

data_4330521
_publ_contact_author_address
;
University of Bonn
Institute of Inorganic Chemistry
Gerhard-Domagk-Strasse 1
53121 Bonn
Germany
;
_publ_contact_author_email       r.streubel@uni-bonn.de
_publ_contact_author_fax         '049 228 73-9616'
_publ_contact_author_name        'Streubel, Rainer'
_publ_contact_author_phone       '049 228 73-5345'
_publ_section_title
;
 Synthesis of Backbone P-Functionalized Imidazol-2-ylidene Complexes: En
 Route to Novel Functional Ionic Liquids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10408
_journal_page_last               10416
_journal_paper_doi               10.1021/ic301641z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C34 H26 N2 O7 P2 W'
_chemical_formula_sum            'C34 H26 N2 O7 P2 W'
_chemical_formula_weight         820.36
_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                 97.591(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.2946(7)
_cell_length_b                   26.3024(12)
_cell_length_c                   22.2793(9)
_cell_measurement_reflns_used    4980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.39
_cell_volume                     6560.6(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w CCD rotation images, thin slices'
_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    0.0479
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10269
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.670
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.2168
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'TWINABS (2009/2), Bruker AXS 2009'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       'flat rod'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         10281
_refine_ls_number_restraints     693
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+30.5533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                9208
_reflns_number_total             10281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301641z_si_001_1.cif
_cod_data_source_block           Greg1766_0t
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4330521