Diverging Rh(I)-Catalyzed Carbocylization Strategy to Prepare a Library of Unique Cyclic Ethers
Mao, Shuli; Probst, Donald; Werner, Stefan; Chen, Jianzhong; Xie, Xiangqun; Brummond, Kay M.; Journal of Combinatorial Chemistry 10 (2008) 235–; doi:10.1021/cc7001843

data_1504331
_publ_section_title
;
 Diverging Rh(I)-Catalyzed Carbocylization Strategy to Prepare a Library
 of Unique Cyclic Ethers
;
_journal_issue                   2
_journal_name_full               'Journal of Combinatorial Chemistry'
_journal_page_first              235
_journal_paper_doi               10.1021/cc7001843
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C19 H26 F3 N O2'
_chemical_formula_weight         357.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.503(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2115(7)
_cell_length_b                   24.220(2)
_cell_length_c                   10.2340(9)
_cell_measurement_temperature    295(2)
_cell_volume                     1918.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15150
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.9644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.357
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.315
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1830
_reflns_number_gt                2161
_reflns_number_total             3373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cc7001843_si.cif
_cod_data_source_block           shuli1s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1504331