The Mosaic of Rottlerin.
Hong, Kenneth K. C.; Ball, Graham E.; Black, David StC; Kumar, Naresh; The Journal of organic chemistry 80 (2015) 10668–10674; doi:10.1021/acs.joc.5b01827

data_4031702
_publ_section_title
;
 The Mosaic of Rottlerin.
;
_journal_issue                   21
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10668
_journal_page_last               10674
_journal_paper_doi               10.1021/acs.joc.5b01827
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C42 H39 O8, C4 H8 O'
_chemical_formula_sum            'C46 H47 O9'
_chemical_formula_weight         743.83
_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   mixed
_audit_creation_date             2015-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                91.419(4)
_cell_angle_beta                 106.952(4)
_cell_angle_gamma                91.256(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0335(9)
_cell_length_b                   12.8124(12)
_cell_length_c                   15.7773(14)
_cell_measurement_reflns_used    7800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.041
_cell_measurement_theta_min      2.614
_cell_volume                     1938.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.976
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30680
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         3.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1218 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.9308.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       plate
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8345
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+0.8564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5565
_reflns_number_total             8345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b01827_si_002.cif
_cod_data_source_block           p1bar_a
_cod_depositor_comments
'Adding full bibliography for 4031702--4031703.cif.'
_cod_database_code               4031702
_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, All O(H) groups
2. Shared sites
{C1TA, C1TB}
{C2TA, C2TB}
3. Uiso/Uaniso restraints and constraints
Uanis(C1TA) = Uanis(C1TB)
Uanis(C2TA) = Uanis(C2TB)
4. Rigid body (RIGU) restrains
 O1TB, C1TB, C2TB, C3TB, C4TB
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1TA, C1TA, C2TA, C3TA, C4TA
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Others
 Fixed Sof: O1TA(0.5) C1TA(0.5) H1TA(0.5) H1TB(0.5) C2TA(0.5) H2TA(0.5)
 H2TB(0.5) C3TA(0.5) H3TA(0.5) H3TB(0.5) C4TA(0.5) H4TA(0.5) H4TB(0.5)
 O1TB(0.5) C1TB(0.5) H1TC(0.5) H1TD(0.5) C2TB(0.5) H2TC(0.5) H2TD(0.5)
 C3TB(0.5) H3TC(0.5) H3TD(0.5) C4TB(0.5) H4TC(0.5) H4TD(0.5)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C16'(H16'), C17'(H17')
6.b Secondary CH2 refined with riding coordinates:
 C1TA(H1TA,H1TB), C2TA(H2TA,H2TB), C3TA(H3TA,H3TB), C4TA(H4TA,H4TB), C1TB(H1TC,
 H1TD), C2TB(H2TC,H2TD), C3TB(H3TC,H3TD), C4TB(H4TC,H4TD)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C8'(H8'), C9'(H9'),
 C11'(H11'), C12'(H12'), C13'(H13'), C14'(H14'), C15'(H15'), C6AA(H6AA),
 C7AA(H7AA)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C19'(H19D,H19E,
 H19F), C20'(H20D,H20E,H20F), C21'(H21D,H21E,H21F)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1'(H1'), O4'(H4')
;
_shelx_res_checksum              27649
_shelx_hkl_checksum              93948
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'