Total Synthesis of the Marine Natural Product Solomonamide B Necessitates Stereochemical Revision.
Kashinath, K.; Jachak, Gorakhnath R.; Athawale, Paresh R.; Marelli, Udaya Kiran; Gonnade, Rajesh G.; Reddy, D. Srinivasa; Organic letters 18 (2016) 3178–3181; doi:10.1021/acs.orglett.6b01395

data_1543799
_publ_section_title
;
 Total Synthesis of the Marine Natural Product Solomonamide B Necessitates
 Stereochemical Revision.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3178
_journal_page_last               3181
_journal_paper_doi               10.1021/acs.orglett.6b01395
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C26 H28 N4 O6'
_chemical_formula_sum            'C26 H28 N4 O6'
_chemical_formula_weight         492.52
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.150(10)
_cell_length_b                   4.978(3)
_cell_length_c                   24.550(11)
_cell_measurement_reflns_used    1519
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.94
_cell_measurement_theta_min      2.36
_cell_volume                     2498(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.999
_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  0.1280
_diffrn_reflns_av_unetI/netI     0.1283
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14707
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 824 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -1.4(10)
_refine_ls_extinction_coef       0.0084(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4389
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0834
_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^)+(0.0764P)^2^+0.3010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     1.001
_reflns_number_gt                2757
_reflns_number_total             4389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01395_si_002.cif
_cod_data_source_block           KKNH46
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               1543799
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2013-3
_shelx_res_checksum              57781
_shelx_hkl_checksum              8501