Towards Diversity-Oriented, Stereoselective Syntheses of Biaryl- or Bis(aryl)metal-Containing Medium Rings
David R. Spring; Shyam Krishnan; Stuart L. Schreiber; Journal of the American Chemical Society 122 (2000) 5656–5657; doi:10.1021/ja0010507

data_4116035
_publ_section_title
;
 Towards Diversity-Oriented, Stereoselective Syntheses of Biaryl- or
 Bis(aryl)metal-Containing Medium Rings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5656
_journal_page_last               5657
_journal_paper_doi               10.1021/ja0010507
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C22 H23 N O S'
_chemical_formula_weight         349.47
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   10.555(2)
_cell_length_b                   10.119(2)
_cell_length_c                   26.478(4)
_cell_measurement_reflns_used    135
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      18.34
_cell_measurement_theta_min      2.67
_cell_volume                     2791.6(9)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            17427
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         0.78
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+13.0778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.2466
_reflns_number_gt                6919
_reflns_number_total             7684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0010507_13.cif
_cod_data_source_block           sls36t
_cod_original_cell_volume        2791.7(8)
_cod_database_code               4116035