Li Liu; Qian Chen; Yun-Dong Wu; Chaozhong Li; Journal of Organic Chemistry 70 (2005) 1539–1544; doi:10.1021/jo0481349

data_4020133
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1539
_journal_page_last               1544
_journal_paper_doi               10.1021/jo0481349
_journal_volume                  70
_journal_year                    2005
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.80(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   8.607(3)
_cell_length_b                   9.146(3)
_cell_length_c                   15.608(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      21.62
_cell_measurement_theta_min      13.66
_cell_volume                     1228.5(6)
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Bruker CCD 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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.1100
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21327
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         5.16
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    2.5894
_exptl_absorpt_coefficient_mu_cm 25.894
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             624.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          0.200
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1590
_refine_ls_number_reflns         13121
_refine_ls_number_restraints     1399
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                8732
_reflns_number_total             13121
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4020133
_exptl_absorpt_process_descript  psi-scan