Determination of the absolute configuration of compounds bearing chiral quaternary carbon centers using the crystalline sponge method
Sairenji, Shiho; Kikuchi, Takashi; Abozeid, Mohamed Ahmed; Takizawa, Shinobu; Sasai, Hiroaki; Ando, Yuichiro; Ohmatsu, Kohsuke; Ooi, Takashi; Fujita, Makoto; Chem. Sci.  (2017) –; doi:10.1039/C7SC01524K

data_1546131
_publ_section_title
;
 Determination of the absolute configuration of compounds bearing chiral
 quaternary carbon centers using the crystalline sponge method
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01524K
_journal_year                    2017
_chemical_absolute_configuration '3S, 3aR, 8aS'
_chemical_formula_moiety
'(C72 H48 N24 I12 Zn6), 2(C20 H24 N2), 1.83(C6 H12)'
_chemical_formula_sum            'C122.98 H117.96 I12 N28 Zn6'
_chemical_formula_weight         3903.19
_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-2016/6
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.275(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.8690(6)
_cell_length_b                   14.91350(10)
_cell_length_c                   31.5649(5)
_cell_measurement_reflns_used    71317
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.7350
_cell_measurement_theta_min      3.6260
_cell_volume                     16039.1(4)
_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    'shelXle (Hubschle et al., 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.3040
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            296791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         76.286
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.505
_exptl_absorpt_correction_T_max  0.306
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             7471
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.107
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 11435 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2008
_refine_ls_number_reflns         33308
_refine_ls_number_restraints     997
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1171P)^2^+64.0597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2054
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                28713
_reflns_number_total             33308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01524k2.cif
_cod_data_source_block           SHELXT_a
_cod_database_code               1546131
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.085
_shelx_estimated_absorpt_t_max   0.229
_shelx_res_checksum              44342