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_4127784
_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 H33 N2 O2, Cl, 0.5(H2 O) [+ solvent]'
_chemical_formula_sum            'C27 H34 Cl N2 O2.5'
_chemical_formula_weight         462.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 106.083(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8485(3)
_cell_length_b                   8.5152(3)
_cell_length_c                   15.5978(6)
_cell_measurement_reflns_used    15401
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.0050
_cell_measurement_theta_min      2.9340
_cell_volume                     1384.49(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.985
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21092
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.263
_diffrn_reflns_theta_min         2.948
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68390
_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    1.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
; 
 Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
  
=============================================== 
   "ccm979_sq "  PLATON-BIJVOET 
=============================================== 
Space Group       P21 
Wavelength    1.54184 
Flack x ....   0.05(2) 
Parsons z ..  0.209(6) 
  
  
Bijvoet Pairs    1640 
Coverage ...       68 
DiffCalcMax.   270.23 
Outlier Crit   540.46 
Scatter Plot 
Sigma Crit..     0.25 
Select Pairs     1266 
Number Plus       938 
Number Minus      328 
Aver. Ratio     0.880 
Slope ......    0.512 
  
  
Student-T Prob. Plot 
Sample Size.     1630 
Corr. Coeff.    0.995 
Intercept ..   -0.106 
Slope ......    1.589 
  
  
Bayesian Statistics 
Student_T Nu     6.13 
Select Pairs     1640 
P2(true)....    1.000 
P3(true)....    1.000 
P3(rac-twin)  0.0E+00 
P3(false) ..  0.0E+00 
G ..........   0.8601 
G (su) .....   0.0223 
Hooft y .... 0.070(11) 
  
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_coef       0.0068(12)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4378
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0979P)^2^+1.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1718
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.695
_reflns_Friedel_fraction_max     0.682
_reflns_number_gt                4252
_reflns_number_total             4378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13849_si_002.cif
_cod_data_source_block           ccm979_sq
_cod_original_formula_sum        'C27 H34 Cl N2 O2.50'
_cod_database_code               4127784
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              4155
_shelx_hkl_checksum              94961
_shelx_fab_checksum              78641