Absolute structure of (3a<i>S</i>,5<i>S</i>,7a<i>S</i>,7b<i>S</i>,9a<i>R</i>,10<i>R</i>,12a<i>R</i>,12b<i>S</i>)-7b-hydroxy-4,4,7a,9a,12a-pentamethyl-10-[(2'<i>R</i>)-6-methylheptan-2-yl]-2,8,9-trioxooctadecahydrobenzo[<i>d</i>]indeno[4,5-<i>b</i>]azepin-5-yl acetate from 62-year-old crystals
Suescun, Leopoldo; Heinzen, Horacio; Acta Crystallographica Section E 75 (2019) 1348–1351; doi:10.1107/S205698901901140X

data_2243063
_publ_section_title
;
 Absolute structure of
 (3a<i>S</i>,5<i>S</i>,7a<i>S</i>,7b<i>S</i>,9a<i>R</i>,10<i>R</i>,12a<i>R</i>,12b<i>S</i>)-7b-hydroxy-4,4,7a,9a,12a-pentamethyl-10-[(2'<i>R</i>)-6-methylheptan-2-yl]-2,8,9-trioxooctadecahydrobenzo[<i>d</i>]indeno[4,5-<i>b</i>]azepin-5-yl
 acetate from 62-year-old crystals
;
_journal_coeditor_code           EX2022
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1348
_journal_page_last               1351
_journal_paper_doi               10.1107/S205698901901140X
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C32 H51 N O6'
_chemical_formula_moiety         'C32 H51 N O6'
_chemical_formula_sum            'C32 H51 N O6'
_chemical_formula_weight         545.73
_chemical_name_systematic
'(3a<i>S</i>,5<i>S</i>,7a<i>S</i>,7b<i>S</i>,9a<i>R</i>,10<i>R</i>,12a<i>R</i>,12b<i>S</i>)-7b-Hydroxy-4,4,7a,9a,12a-pentamethyl-10-[(2'<i>R</i>)-6-methylheptan-2-yl]-2,8,9-trioxooctadecahydrobenzo[<i>d</i>]indeno[4,5-<i>b</i>]azepin-5-yl acetate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.599(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.882(4)
_cell_length_b                   6.5332(11)
_cell_length_c                   13.6021(16)
_cell_measurement_reflns_used    95
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.34
_cell_measurement_theta_min      12.3
_cell_volume                     3046.9(7)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14487
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.438
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'Incoatec I microsource'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       'flat needles'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.442
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2070 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.09(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0771P)^2^+1.6616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                5056
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2022sup1.cif
_cod_data_source_block           I
_cod_database_code               2243063
_cod_database_fobs_code          2243063
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              28480
_shelx_res_checksum              90517