Chlorine-containing polyacetoxybriarane diterpenoids from the octocoral Junceella fragilis
Do, Hai Nhat; Chen, Yu-Ta; Chien, Su-Ying; Chen, You-Ying; Zhang, Mingzi M.; Tsou, Lun Kelvin; Chen, Jih-Jung; Wen, Zhi-Hong; Lo, Yi-Hao; Zheng, Li-Guo; Sung, Ping-Jyun; RSC Advances 14 (2024) 17195–17201; doi:10.1039/D4RA03062A

data_7248731
_publ_section_title
;
 Chlorine-containing polyacetoxybriarane diterpenoids from the octocoral
 Junceella fragilis
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              17195
_journal_page_last               17201
_journal_paper_doi               10.1039/D4RA03062A
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H35 Cl O12'
_chemical_formula_weight         599.01
_chemical_name_systematic        'Frajunolide I'
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-05-20 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.8317(3)
_cell_length_b                   22.8317(3)
_cell_length_c                   10.2937(2)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.91
_cell_measurement_theta_min      2.23
_cell_volume                     4647.06(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Bruker APEX4'
_computing_publication_material  'Bruker APEX4'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47636
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.402
_diffrn_reflns_theta_min         3.872
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.8637
_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    1.284
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
; 
 Flack x determined using 2491 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0660P)^2^+0.4273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                5789
_reflns_number_total             6221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03062a2.cif
_cod_data_source_block           ic22479_sq
_cod_original_cell_volume        4647.06(15)
_cod_database_code               7248731
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              44368
_shelx_hkl_checksum              98268
_shelx_fab_checksum              22509