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_4330524
_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         'C37 H32 N2 O7 P2 W, C4 H10 O'
_chemical_formula_sum            'C41 H42 N2 O8 P2 W'
_chemical_formula_weight         936.56
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.904(2)
_cell_angle_beta                 74.595(2)
_cell_angle_gamma                75.539(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3096(3)
_cell_length_b                   12.1053(4)
_cell_length_c                   16.3865(7)
_cell_measurement_reflns_used    6433
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1988.02(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0679
_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       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21397
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  0.7930
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       'trigonal plate'
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.226
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8581
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                7294
_reflns_number_total             8581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301641z_si_001_4.cif
_cod_data_source_block           Greg1804
_cod_database_code               4330524