Intramolecular Oxymercuration of Stereoisomeric Cyclohexyl-Belted Poly(spirotetrahydrofuranyl) Platforms
Leo A. Paquette; David G. Bolin; Marshall Stepanian; Bruce M. Branan; Uppuluri V. Mallavadhani; Jinsung Tae; Shawn W. E. Eisenberg; Robin D. Rogers; Journal of the American Chemical Society 120 (1998) 11603–11615; doi:10.1021/ja981756p

data_4116874
_publ_section_title
;
 Intramolecular Oxymercuration of Stereoisomeric Cyclohexyl-Belted
 Poly(spirotetrahydrofuranyl) Platforms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11603
_journal_page_last               11615
_journal_paper_doi               10.1021/ja981756p
_journal_volume                  120
_journal_year                    1998
_chemical_formula_structural     'LAP211 (II-DGB-222A)'
_chemical_formula_sum            'C21 H31 Cl Hg O5'
_chemical_formula_weight         599.50
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.499(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6396(2)
_cell_length_b                   7.4269(2)
_cell_length_c                   16.2254(3)
_cell_measurement_reflns_used    5873
_cell_measurement_temperature    173(2)
_cell_volume                     1026.83(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'area detector'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6643
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    7.655
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_description       plates
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.406
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0000(5)
_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_all   1.094
_refine_ls_goodness_of_fit_obs   1.113
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_obs          0.0304
_refine_ls_shift/esd_max         -1.067
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      '0.0333, 1.9501'
_refine_ls_wR_factor_all         0.0778
_refine_ls_wR_factor_obs         0.0759
_reflns_number_observed          3764
_reflns_number_total             3991
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981756p_03.cif
_cod_data_source_block           33
_cod_database_code               4116874