Comatulins A-E, Taurine-Conjugated Anthraquinones from the Australian Crinoid <i>Comatula rotalaria</i>.
Lum, Kah Yean; Taki, Aya C.; Gasser, Robin B.; Tietjen, Ian; Ekins, Merrick G.; White, Jonathan M.; Addison, Russell S.; Hayes, Sasha; St John, James; Davis, Rohan A.; Journal of natural products 83 (2020) 1971–1979; doi:10.1021/acs.jnatprod.0c00267

data_1558163
_publ_section_title
;
 Comatulins A-E, Taurine-Conjugated Anthraquinones from the Australian
 Crinoid <i>Comatula rotalaria</i>.
;
_journal_issue                   6
_journal_name_full               'Journal of natural products'
_journal_page_first              1971
_journal_page_last               1979
_journal_paper_doi               10.1021/acs.jnatprod.0c00267
_journal_volume                  83
_journal_year                    2020
_chemical_formula_moiety         '(C20 H18 O8), (H2 O)'
_chemical_formula_sum            'C20 H20 O8'
_chemical_formula_weight         388.36
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 92.098(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2710(2)
_cell_length_b                   9.6883(3)
_cell_length_c                   19.4904(4)
_cell_measurement_reflns_used    10212
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4230
_cell_measurement_theta_min      4.4530
_cell_volume                     1749.46(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20845
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.190
_diffrn_reflns_theta_min         4.540
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.29a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.527
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0827
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2628
_refine_ls_wR_factor_ref         0.2739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3281
_reflns_number_total             3675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np0c00267_si_001.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 1558163.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1558163
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'Rohan Davis Anopterine KYLU02_98_44'
_oxdiff_exptl_absorpt_empirical_full_min 0.542
_oxdiff_exptl_absorpt_empirical_full_max 2.000
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              24300
_shelx_hkl_checksum              45