Synthesis and crystal structure analysis of substituted bi-cyclo-[3.3.1]nona-nones.
König, Julien A; Morgenstern, Bernd; Jauch, Johann; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 405–411; doi:10.1107/S2056989025003299

data_2023475
_publ_section_title
;
 Synthesis and crystal structure analysis of substituted
 bi-cyclo-[3.3.1]nona-nones.
;
_journal_coeditor_code           EV2016
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              405
_journal_page_last               411
_journal_paper_doi               10.1107/S2056989025003299
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C26 H42 O3'
_chemical_formula_moiety         'C26 H42 O3'
_chemical_formula_sum            'C26 H42 O3'
_chemical_formula_weight         402.59
_chemical_name_systematic
4-<i>tert</i>-Butyl-4-hydroxy-2-methoxy-8-methyl-7-(3-methylbut-2-en-1-yl)-8-(4-methylpent-3-en-1-yl)bicyclo[3.3.1]non-2-en-9-one
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 113.2180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1165(5)
_cell_length_b                   13.9068(4)
_cell_length_c                   12.8150(4)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.93
_cell_volume                     2475.81(13)
_computing_cell_refinement
;
SAINT  (Bruker, 2021)
;
_computing_data_collection
;
APEX4 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT  (Bruker, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>) and
ShelXle (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            87917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.128
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'INCOATEC I\^A\mS microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0490P)^2^+0.8245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                4697
_reflns_number_total             5484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ev2016.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 2023472--2023475.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023475
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.995
_shelx_hkl_checksum              62365
_shelx_res_checksum              57477