Synthesis and structural confirmation of selaginpulvilin X.
Havlíková, Tereza; Nallappan, Sundaravelu; Císařová, Ivana; Rycek, Lukas; Organic & biomolecular chemistry 22 (2024) 8843–8846; doi:10.1039/d4ob01529k

data_7160164
_publ_section_title
;
 Synthesis and structural confirmation of selaginpulvilin X.
;
_journal_issue                   45
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8843
_journal_page_last               8846
_journal_paper_doi               10.1039/d4ob01529k
_journal_volume                  22
_journal_year                    2024
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C29 H22 O4'
_chemical_formula_sum            'C29 H22 O4'
_chemical_formula_weight         434.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-08-07 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.343(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4717(5)
_cell_length_b                   12.7788(7)
_cell_length_c                   18.5575(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.3069
_cell_measurement_theta_min      4.8448
_cell_volume                     2209.6(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service v8.5.1.2 Release'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTONIII CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31736
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.301
_diffrn_reflns_theta_min         4.845
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.8408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3844
_reflns_number_total             4039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01529k2.cif
_cod_data_source_block           cu_th119_rycek
_cod_depositor_comments          'Adding full bibliography for 7160164.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7160164
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              7518