A quick access to the spirotricyclic core analogue of mangicol A by a Rh(I)-catalyzed tandem Pauson-Khand/[4+2] cycloaddition
Wei Chen; Jia-Hui Tay; Jun Ying; Michal Sabat; Xiao-Qi Yu; Lin Pu; Chem.Commun. 49 (2013) 170–; doi:10.1039/c2cc37465j

data_7108726
_publ_section_title
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 A quick access to the spirotricyclic core analogue of mangicol A by a
 Rh(I)-catalyzed tandem Pauson-Khand/[4+2] cycloaddition
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_journal_name_full               Chem.Commun.
_journal_page_first              170
_journal_paper_doi               10.1039/c2cc37465j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C17 H24 O2 Si'
_chemical_formula_weight         288.45
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   9.1005(3)
_cell_length_b                   12.8251(5)
_cell_length_c                   13.4859(5)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      37.07
_cell_measurement_theta_min      4.08
_cell_volume                     1574.00(10)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38547
_diffrn_reflns_theta_full        37.08
_diffrn_reflns_theta_max         37.08
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.9401
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         7644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0283
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                7264
_reflns_number_total             7644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37465j.txt
_cod_data_source_block           C17H24O2Si
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1574.0(1)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7108726