Total Syntheses of Herqulines B and C.
Zhu, Xu; McAtee, Christopher C.; Schindler, Corinna S.; Journal of the American Chemical Society 141 (2019) 3409–3413; doi:10.1021/jacs.8b13849

data_4127783
_publ_section_title
;
 Total Syntheses of Herqulines B and C.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3409
_journal_page_last               3413
_journal_paper_doi               10.1021/jacs.8b13849
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H28 N2 O4, 2(H2 O)0.25'
_chemical_formula_sum            'C27 H29 N2 O4.5'
_chemical_formula_weight         453.52
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.11400(10)
_cell_length_b                   12.97770(10)
_cell_length_c                   14.75780(10)
_cell_measurement_reflns_used    20649
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.8100
_cell_measurement_theta_min      4.5240
_cell_volume                     2320.10(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.218
_diffrn_reflns_theta_min         4.537
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 1741 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 

Space Group   P212121
Wavelength    1.54184
Flack x ....  -0.13(8)
Parsons z ..  -0.08(7)
 
 
Bijvoet Pairs    1845
Coverage ...       99
DiffCalcMax.    31.52
Outlier Crit    63.05
Scatter Plot
Sigma Crit..     0.25
Select Pairs      207
Number Plus       144
Number Minus       63
Aver. Ratio     1.240
Slope ......    1.238
 
 
Student-T Prob. Plot
Sample Size.     1835
Corr. Coeff.    0.996
Intercept ..   -0.083
Slope ......    0.851
 
 
Bayesian Statistics
Student_T Nu     7.42
Select Pairs     1845
P2(true)....    1.000
P3(true)....    1.000
P3(rac-twin)  0.2E-14
P3(false) ..  0.6E-48
G ..........   1.2570
G (su) .....   0.1491
Hooft y ....  -0.13(7)

;
_refine_ls_abs_structure_Flack   -0.13(8)
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0473P)^2^+0.6404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4183
_reflns_number_total             4292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13849_si_003.cif
_cod_data_source_block           zx749
_cod_original_formula_sum        'C27 H29 N2 O4.50'
_cod_database_code               4127783
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              51885
_shelx_hkl_checksum              34705