Synthesis and Structure of Optically Active 1,12-Diethyl- and 1,12-Diisopropylbenzo[c]phenanthrenes: An Isopropyl Group Can Be Smaller than a Methyl Group
Sugiura, Hiroki; Sakai, Daisuke; Otani, Harunori; Teranishi, Kazuhiro; Takahira, Yusuke; Amemiya, Ryo; Yamaguchi, Masahiko; Chemistry Letters 36 (2007) 72–; doi:10.1246/cl.2007.72

data_8000176
_publ_section_title
;
 Synthesis and Structure of Optically Active 1,12-Diethyl- and
 1,12-Diisopropylbenzo[c]phenanthrenes: An Isopropyl Group Can Be Smaller
 than a Methyl Group
;
_journal_issue                   1
_journal_name_full               'Chemistry Letters'
_journal_page_first              72
_journal_paper_doi               10.1246/cl.2007.72
_journal_volume                  36
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C46 H54 N2 O6 S2 '
_chemical_formula_sum            'C46 H54 N2 O6 S2'
_chemical_formula_weight         795.06
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.993(12)
_cell_length_b                   13.367(11)
_cell_length_c                   28.13(2)
_cell_measurement_reflns_used    11841
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     4134(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.109
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20358
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.36
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2093 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4722
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.5000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                1400
_reflns_number_total             4722
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            36-72sup1.cif
_cod_data_source_block           (P)-9
_cod_original_cell_volume        4133(7)
_cod_original_formula_sum        'C46 H54 N2 O6 S2 '
_cod_database_code               8000176