Pinacol Coupling Strategy for the Construction of the Bicyclo[6.4.1]tridecane Framework of Schiglautone A.
Werner, Bettina; Kalesse, Markus; Organic letters 19 (2017) 1524–1526; doi:10.1021/acs.orglett.7b00288

data_1545938
_publ_section_title
;
 Pinacol Coupling Strategy for the Construction of the
 Bicyclo[6.4.1]tridecane Framework of Schiglautone A.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1524
_journal_page_last               1526
_journal_paper_doi               10.1021/acs.orglett.7b00288
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C26 H48 O2 Si'
_chemical_formula_weight         420.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.434(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.621(6)
_cell_length_b                   7.7207(16)
_cell_length_c                   12.441(2)
_cell_measurement_reflns_used    4869
_cell_measurement_temperature    200.(2)
_cell_measurement_theta_max      20.5232
_cell_measurement_theta_min      2.7351
_cell_volume                     2652.3(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1630
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37395
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                2731
_reflns_number_total             4466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00288_si_001.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-03-17
Z value and formula changed from the absurd ones in the original
file.                 miguel
;
_cod_original_formula_sum            'C2.36 H4.36 O0.18 Si0.09'
_cod_original_formula_weight         38.25
_cod_original_formula_units_Z            44
_cod_database_code               1545938