A Stable Four-Membered N-Heterocyclic Carbene
Emmanuelle Despagnet-Ayoub; Robert H. Grubbs; Journal of the American Chemical Society 126 (2004) 10198–10199; doi:10.1021/ja047892d

data_4112875
_publ_contact_author
;       Michael W. Day
        Beckman Institute
        California Institute of Technology
        Pasadena, CA  91125
        USA
;
_publ_contact_author_email       mikeday@caltech.edu
_publ_contact_author_fax         '(626) 449 4159'
_publ_contact_author_phone       '(626) 395 2734'
_publ_section_title
;
 A Stable Four-Membered N-Heterocyclic Carbene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10198
_journal_page_last               10199
_journal_paper_doi               10.1021/ja047892d
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C24 H33 F3 N3 O3 P S'
_chemical_formula_weight         531.56
_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                67.7490(10)
_cell_angle_beta                 65.7880(10)
_cell_angle_gamma                67.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5668(3)
_cell_length_b                   11.8758(4)
_cell_length_c                   12.7952(4)
_cell_measurement_reflns_used    22548
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      41.26
_cell_measurement_theta_min      2.19
_cell_volume                     1305.19(7)
_computing_cell_refinement       'Bruker SAINT v6.45'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.45'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.838
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method
'\q=-28 and \q=-40; \w scans at 7 & 3 \f settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'norma-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50465
_diffrn_reflns_theta_full        41.76
_diffrn_reflns_theta_max         41.76
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       Block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.703
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     348
_refine_ls_number_reflns         15049
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.709
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                10187
_reflns_number_total             15049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047892dsi20040413_013058.cif
_cod_data_source_block           emd04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4112875