Crystal structures of two 1,2,3,4-tetra-hydro-naphthalenes obtained during efforts towards the total synthesis of elisabethin A.
Kaiser, Maximilian; Weil, Matthias; Gärtner, Peter; Enev, Valentin; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 177–181; doi:10.1107/S2056989023001226

data_2312162
_publ_section_title
;
 Crystal structures of two 1,2,3,4-tetra-hydro-naphthalenes obtained
 during efforts towards the total synthesis of elisabethin A.
;
_journal_coeditor_code           VM2277
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              177
_journal_page_last               181
_journal_paper_doi               10.1107/S2056989023001226
_journal_volume                  79
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C26 H42 O5 Si'
_chemical_formula_moiety         'C26 H42 O5 Si'
_chemical_formula_sum            'C26 H42 O5 Si'
_chemical_formula_weight         462.68
_chemical_name_systematic
'Methyl (<i>E</i>)-3-{(1<i>R</i>,4<i>S</i>)-8-hydroxy-6-methoxy-4,7-dimethyl-5-[(triisopropylsilyl)oxy]-1,2,3,4-tetrahydronaphthalen-1-yl}acrylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.0912(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0078(7)
_cell_length_b                   9.2620(6)
_cell_length_c                   12.1411(8)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.206
_cell_measurement_theta_min      2.743
_cell_volume                     1309.66(14)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39668
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.347
_diffrn_reflns_theta_min         1.729
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       fragment
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.179
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4647 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         11727
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0515P)^2^+0.0894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                10749
_reflns_number_total             11727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2277sup1.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2312162
_shelx_hkl_checksum              60852
_shelx_res_checksum              35326
_cod_database_fobs_code 2312162