A biomimetic approach for the concise total synthesis of greenwaylactams A-C.
Kratena, Nicolas; Weil, Matthias; Gärtner, Peter; Organic & biomolecular chemistry 21 (2023) 6317–6319; doi:10.1039/d3ob01001e

data_7159488
_publ_section_title
;
 A biomimetic approach for the concise total synthesis of greenwaylactams
 A-C.
;
_journal_issue                   31
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6317
_journal_page_last               6319
_journal_paper_doi               10.1039/d3ob01001e
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C30 H37 N O3 S'
_chemical_formula_sum            'C30 H37 N O3 S'
_chemical_formula_weight         491.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-06-20 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0786(4)
_cell_length_b                   21.5444(7)
_cell_length_c                   7.8455(2)
_cell_measurement_reflns_used    28093
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.58
_cell_measurement_theta_min      2.94
_cell_volume                     2544.74(13)
_computing_cell_refinement
;
X-Area (STOE, 2021)
;
_computing_data_collection
;
X-Area (STOE, 2021)
;
_computing_data_reduction
;
X-Area (STOE, 2021)
;
_computing_molecular_graphics    MERCURY
_computing_publication_material  'SHELXL (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      ' 3371 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            27134
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        65.215
_diffrn_reflns_theta_max         65.215
_diffrn_reflns_theta_min         2.935
_diffrn_source                   Axo_Cu
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  0.6537
_exptl_absorpt_correction_T_min  0.5546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0451P)^2^+1.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3398
_reflns_number_total             4191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01001e2.cif
_cod_data_source_block           C30H37NO3S
_cod_depositor_comments          'Adding full bibliography for 7159488.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7159488
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.770
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              92717