Modular Synthesis of Heterocyclic Carbene Precursors
Attila Paczal; Attila C. Bényei; András Kotschy; Journal of Organic Chemistry 71 (2006) 5969–5979; doi:10.1021/jo060594+

data_4021835
_publ_contact_author_address
;
Department of Chemistry
University of Debrecen
Laboratory for X-ray Diffraction
Debrecen H-4010
Hungary
;
_publ_contact_author_email       abenyei@delfin.klte.hu
_publ_contact_author_fax         36(52)512915
_publ_contact_author_name        'Benyei, Attila Cs.'
_publ_contact_author_phone       '36(52)512900 ext. 2486'
_publ_section_title
;
 Modular Synthesis of Heterocyclic Carbene Precursors
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5969
_journal_page_last               5979
_journal_paper_doi               10.1021/jo060594+
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C28 H39 N2 O, I'
_chemical_formula_sum            'C28 H39 I N2 O'
_chemical_formula_weight         546.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2005-11-03
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.409(10)
_cell_angle_beta                 90.473(10)
_cell_angle_gamma                111.535(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7553(10)
_cell_length_b                   11.861(2)
_cell_length_c                   14.220(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.94
_cell_measurement_theta_min      9.98
_cell_volume                     1373.5(4)
_computing_cell_refinement       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_collection       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5032
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 111
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  0.6697
_exptl_absorpt_correction_T_min  0.5365
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   4
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   5
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.8298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                4479
_reflns_number_total             5032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060594+si20060317_101228.cif
_cod_database_code               4021835