Conformational Studies by Dynamic NMR. 94. Cogwheel Pathway for the Stereomutations of Durene Derivatives Containing the Mesityl Ring
Carmine Coluccini; Stefano Grilli; Lodovico Lunazzi; Andrea Mazzanti; Journal of Organic Chemistry 68 (2003) 7266–7273; doi:10.1021/jo034737t

data_4022510
_publ_contact_author
;
Dr. Andrea Mazzanti
Universita di Bologna
Dipartimento di Chimica Organica A.Mangini
Viale Risorgimento 4
40136 Bologna
Italy
;
_publ_contact_author_email       mazzand@ms.fci.unibo.it
_publ_contact_author_fax         '[039]051 209 3654'
_publ_contact_author_phone       '[039]051 209 3633'
_publ_section_title
;
 Conformational Studies by Dynamic NMR. 94.
 Cogwheel Pathway for the Stereomutations of Durene
 Derivatives Containing the Mesityl Ring
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7266
_journal_page_last               7273
_journal_paper_doi               10.1021/jo034737t
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C30 H34 O2'
_chemical_formula_weight         426.57
_chemical_name_systematic
;
 1,4-bis-(mesitoyl)-2,3,5,6-tetramethylbenzene
;
_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_date             27/05/2003
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.8740(10)
_cell_angle_beta                 84.1620(10)
_cell_angle_gamma                76.7850(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4917(4)
_cell_length_b                   8.6147(4)
_cell_length_c                   9.2869(5)
_cell_measurement_temperature    293(2)
_cell_volume                     608.18(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0108
_diffrn_reflns_av_sigmaI/netI    0.0115
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7900
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.9011
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colouless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             230
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          1.50
_exptl_crystal_size_min          0.80
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.078(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0586
_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^)+(0.1128P)^2^+0.0583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                2983
_reflns_number_total             3530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo034737tsi20030604_012816.cif
_cod_data_source_block           p-1
_cod_database_code               4022510