Stereoisomeric Composition of Natural Myrtucommulone A.
Hans, Marcus; Charpentier, Maël; Huch, Volker; Jauch, Johann; Bruhn, Torsten; Bringmann, Gerhard; Quandt, Dietmar; Journal of natural products 78 (2015) 2381–2389; doi:10.1021/acs.jnatprod.5b00358

data_1538420
_publ_section_title
;
 Stereoisomeric Composition of Natural Myrtucommulone A.
;
_journal_issue                   10
_journal_name_full               'Journal of natural products'
_journal_page_first              2381
_journal_page_last               2389
_journal_paper_doi               10.1021/acs.jnatprod.5b00358
_journal_volume                  78
_journal_year                    2015
_chemical_formula_moiety         'C48 H55 F3 O10'
_chemical_formula_sum            'C48 H55 F3 O10'
_chemical_formula_weight         848.92
_chemical_name_systematic
; 
 (S)-((12R,14R)-6-isobutyryl-12,14-diisopropyl-2.2.4.4.8.8.10,10-octamethyl- 
 1,3,9,11-teraoxo-1,2,3,4,8,9,10,11,12,14-decahydrochromeno[3,2-b]xanthen-13-yl) 
 3,3,3-trifluoro-2-methoxy-2-phenylpropanoate 
;
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.687(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4479(10)
_cell_length_b                   40.961(5)
_cell_length_c                   17.888(3)
_cell_measurement_reflns_used    4021
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      20.36
_cell_measurement_theta_min      2.33
_cell_volume                     4722.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27828
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_min         0.994
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2010'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.806
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
; 
 Flack x determined using 3121 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.2(8)
_refine_ls_extinction_coef       0.0050(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         15089
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0915
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    0.690
_reflns_Friedel_fraction_max     0.654
_reflns_number_gt                9437
_reflns_number_total             15089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np5b00358_si_001.cif
_cod_data_source_block           sh3365
_cod_original_cell_volume        4722.3(11)
_cod_database_code               1538420
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-3