Palladium-catalyzed approach to stereodefined ten-membered cycles from 1,5-bisallenes.
Cheng, Jiajia; Jiang, Xuefeng; Ma, Shengming; Organic letters 13 (2011) 5200–5203; doi:10.1021/ol202074e

data_1502473
_publ_section_title
;
 Palladium-catalyzed approach to stereodefined ten-membered cycles from
 1,5-bisallenes.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5200
_journal_page_last               5203
_journal_paper_doi               10.1021/ol202074e
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C34 H34 N2 O2 S'
_chemical_formula_weight         534.69
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.1485(16)
_cell_length_b                   16.858(2)
_cell_length_c                   25.981(3)
_cell_measurement_reflns_used    1644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.835
_cell_measurement_theta_min      4.833
_cell_volume                     5758.9(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1070
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28914
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79914
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0081(7)
_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   0.853
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5349
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                2161
_reflns_number_total             5349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol202074e_si_001.cif
_cod_data_source_block           cd25306
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5758.7(12)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1502473