Toward the total synthesis of palhinine A: expedient assembly of multifunctionalized isotwistane ring system with contiguous quaternary stereocenters.
Zhang, Guo-Biao; Wang, Fang-Xin; Du, Ji-Yuan; Qu, Hu; Ma, Xiao-Yan; Wei, Meng-Xue; Wang, Cheng-Tao; Li, Qiong; Fan, Chun-An; Organic letters 14 (2012) 3696–3699; doi:10.1021/ol301534r

data_1508302
_publ_section_title
;
 Toward the total synthesis of palhinine A: expedient assembly of
 multifunctionalized isotwistane ring system with contiguous quaternary
 stereocenters.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3696
_journal_page_last               3699
_journal_paper_doi               10.1021/ol301534r
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C22 H40 I2 O Si'
_chemical_formula_weight         602.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.718(4)
_cell_angle_beta                 73.818(4)
_cell_angle_gamma                89.647(4)
_cell_formula_units_Z            4
_cell_length_a                   12.045(5)
_cell_length_b                   12.170(5)
_cell_length_c                   18.967(8)
_cell_measurement_reflns_used    3720
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.20
_cell_measurement_theta_min      2.32
_cell_volume                     2569.0(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.1333
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18291
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    2.504
_exptl_absorpt_correction_T_max  0.6901
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.688
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+14.6943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                4088
_reflns_number_total             9398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol301534r_si_002.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 1508302--1508303.cif.
;
_cod_original_cell_volume        2569.0(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1508302