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_2023472
_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          'C10 H12 O3'
_chemical_formula_moiety         'C10 H12 O3'
_chemical_formula_sum            'C10 H12 O3'
_chemical_formula_weight         180.20
_chemical_name_systematic
;
4-Methoxybicyclo[3.3.1]non-3-ene-2,9-dione
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 99.546(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4819(4)
_cell_length_b                   7.4766(5)
_cell_length_c                   9.0627(5)
_cell_measurement_reflns_used    6064
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.28
_cell_volume                     433.12(5)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8258
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         2.279
_diffrn_source                   'INCOATEC I\^A\mS microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6992
_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    1.382
_exptl_crystal_description       rod
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.151
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2031
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0364P)^2^+0.0624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                1948
_reflns_number_total             2031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ev2016.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2023472--2023475.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2023472
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              16501
_shelx_res_checksum              828