Myrtucomvalones A–C, three unusual triketone–sesquiterpene adducts from the leaves of Myrtus communis ‘Variegata’
Chen, Ming; Chen, Li-Feng; Li, Man-Mei; Li, Ni-Ping; Cao, Jia-Qing; Wang, Ying; Li, Yao-Lan; Wang, Lei; Ye, Wen-Cai; RSC Adv. 7 (2017) 22735–; doi:10.1039/C7RA02260C

data_7228114
_publ_section_title
;
 Myrtucomvalones A--C, three unusual triketone--sesquiterpene adducts from
 the leaves of Myrtus communis &#x2018;Variegata&#x2019;
;
_journal_issue                   37
_journal_name_full               'RSC Adv.'
_journal_page_first              22735
_journal_paper_doi               10.1039/C7RA02260C
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C29 H44 O3'
_chemical_formula_sum            'C29 H44 O3'
_chemical_formula_weight         440.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-24 deposited with the CCDC.
2017-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                107.318(7)
_cell_angle_beta                 95.676(6)
_cell_angle_gamma                104.090(7)
_cell_formula_units_Z            2
_cell_length_a                   9.7468(7)
_cell_length_b                   10.0413(9)
_cell_length_c                   14.7257(9)
_cell_measurement_reflns_used    3527
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.1940
_cell_measurement_theta_min      4.7430
_cell_volume                     1311.43(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9591
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -31.00  33.00   1.00    1.00    --  -40.48  57.00   0.00   64
  2  \w     12.00  59.00   1.00    1.00    --   40.48  57.00 -30.00   47
  3  \w     86.00 113.00   1.00    1.00    --   40.48  57.00 -30.00   27
  4  \w     96.00 123.00   1.00    3.67    --  106.95 -30.00  30.00   27
  5  \w     82.00 178.00   1.00    3.67    --  106.95  61.00 120.00   96
  6  \w     94.00 157.00   1.00    3.67    --  106.95 125.00  60.00   63
  7  \w    106.00 133.00   1.00    3.67    --  106.95  77.00-120.00   27
  8  \w    132.00 167.00   1.00    3.67    --  106.95 125.00-150.00   35
  9  \w     81.00 177.00   1.00    3.67    --  106.95  30.00-150.00   96
 10  \w     62.00 108.00   1.00    3.67    --  106.95 -94.00-120.00   46
 11  \w     39.00 109.00   1.00    3.67    --  106.95 -94.00 -30.00   70
 12  \w     40.00  96.00   1.00    1.00    --   40.48-125.00  60.00   56
 13  \w     29.00 108.00   1.00    3.67    --  106.95 -94.00 150.00   79
 14  \w     83.00 121.00   1.00    3.67    --  106.95-125.00 120.00   38
 15  \w     39.00 126.00   1.00    3.67    --  106.95 -45.00 150.00   87
 16  \w     34.00 133.00   1.00    3.67    --  106.95 -45.00 -30.00   99
 17  \w    -71.00  33.00   1.00    1.00    --  -40.48  77.00-150.00  104
 18  \w   -115.00 -17.00   1.00    1.00    --  -40.48 -37.00  60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0129013000
_diffrn_orient_matrix_UB_12      -0.1445845000
_diffrn_orient_matrix_UB_13      0.0109219000
_diffrn_orient_matrix_UB_21      -0.0942915000
_diffrn_orient_matrix_UB_22      -0.0839053000
_diffrn_orient_matrix_UB_23      -0.1010071000
_diffrn_orient_matrix_UB_31      0.1357970000
_diffrn_orient_matrix_UB_32      0.0143288000
_diffrn_orient_matrix_UB_33      -0.0459695000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8553
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.61
_diffrn_reflns_theta_min         4.76
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0774
_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^)+(0.0821P)^2^+3.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3977
_reflns_number_total             5070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra02260c2.cif
_cod_data_source_block           exp_119
_cod_original_cell_volume        1311.43(18)
_cod_database_code               7228114
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.855
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C007(H007), C008(H008), C00A(H00C), C00C(H00D), C00H(H00I), C00I(H00J),
 C00L(H00N)
2.b Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00D(H00E,H00F), C00E(H00G,H00H), C00N(H00O,H00P), C00O(H00Q,
 H00R)
2.c Idealised Me refined as rotating group:
 C00K(H00K,H00L,H00M), C00P(H00S,H00T,H00U), C00Q(H00V,H00W,H00X), C00R(H00Y,H,
 HA), C00S(H00Z,HB,HC), C00T(H00,HD,HE), C00U(H0AA,HF,HG), C00V(H1AA,HH,HI),
 C00W(H2AA,HJ,HK)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.729
_oxdiff_exptl_absorpt_empirical_full_min 0.186