Rhodomentones A and B, novel meroterpenoids with unique NMR characteristics from Rhodomyrtus tomentosa.
Liu, Hong-Xin; Chen, Kai; Yuan, Yao; Xu, Zhi-Fang; Tan, Hai-Bo; Qiu, Sheng-Xiang; Organic & biomolecular chemistry 14 (2016) 7354–7360; doi:10.1039/c6ob01215a

data_7155196
_publ_section_title
;
 Rhodomentones A and B, novel meroterpenoids with unique NMR
 characteristics from Rhodomyrtus tomentosa.
;
_journal_issue                   30
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7354
_journal_page_last               7360
_journal_paper_doi               10.1039/c6ob01215a
_journal_volume                  14
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H46 O3'
_chemical_formula_sum            'C30 H46 O3'
_chemical_formula_weight         454.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-29 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.82201(13)
_cell_length_b                   19.9887(2)
_cell_length_c                   23.1114(3)
_cell_measurement_reflns_used    24816
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      66.9360
_cell_measurement_theta_min      2.8900
_cell_volume                     5461.38(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5058
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -99.00  -19.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -      -40.7938  126.0000   90.0000 80

  2 omega   14.00  117.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -       40.7938   38.0000  -30.0000 103

  3 omega  -35.00   67.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -       40.7938  -38.0000 -180.0000 102

  4 omega   19.00   96.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -126.0000  -90.0000 77

  5 omega   10.00   84.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -180.0000 74

  6 omega    9.00  133.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   98.8874 124

  7 omega   63.00  171.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 108

  8 omega   16.00   69.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 53

  9 omega   19.00   77.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 58

 10 omega    8.00  132.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000  -47.6432 124

 11 omega   60.00  172.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -30.0000 112

 12 omega    7.00  120.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -       40.7938   77.0000  150.0000 113

 13 omega   11.00  115.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -       40.7938   57.0000   60.0000 104

 14 omega    7.00  120.00   1.0000    1.9350
omega____ theta____ kappa____ phi______ frames
    -       40.7938   77.0000 -120.0000 113

 15 omega   63.00  168.00   1.0000    7.7350
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  120.0000 105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0135269000
_diffrn_orient_matrix_UB_12      0.0139283000
_diffrn_orient_matrix_UB_13      -0.0651596000
_diffrn_orient_matrix_UB_21      -0.0133981000
_diffrn_orient_matrix_UB_22      0.0752707000
_diffrn_orient_matrix_UB_23      0.0128762000
_diffrn_orient_matrix_UB_31      0.1288797000
_diffrn_orient_matrix_UB_32      0.0092469000
_diffrn_orient_matrix_UB_33      -0.0055053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47405
_diffrn_reflns_theta_full        67.04
_diffrn_reflns_theta_max         67.04
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.6752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                9136
_reflns_number_total             9638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob01215a2.cif
_cod_data_source_block           01287a
_cod_depositor_comments          'Adding full bibliography for 7155196.cif.'
_cod_original_cell_volume        5461.39(11)
_cod_database_code               7155196
_chemical_oxdiff_formula         'C20 H20 O4'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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:
 C12(H12), C17(H17), C18(H18), C28(H28), C6(H6), C21(H21), C31(H31), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C22(H22A,H22B), C30(H30A,H30B), C36(H36A,H36B), C37(H37A,H37B),
 C49(H49A,H49B), C63(H63A,H63B), C10(H10A,H10B), C14(H14A,H14B), C19(H19A,H19B),
  C27(H27A,H27B), C33(H33A,H33B), C41(H41A,H41B), C60(H60A,H60B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C20(H20)
2.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'