Easy Access to Polyfunctionalized Chiral Decalins
Santalla, Hugo; Gándara, Zoila; Gómez-Bouzó, Uxía; Gómez, Generosa; Fall, Yagamare; ACS Omega  (2020) –; doi:10.1021/acsomega.0c03504

data_4518101
_publ_section_title
;
 Easy Access to Polyfunctionalized Chiral Decalins
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c03504
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H38 O2 S2'
_chemical_formula_weight         422.66
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.54320(10)
_cell_length_b                   17.2692(3)
_cell_length_c                   18.1411(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      70.79
_cell_measurement_theta_min      3.53
_cell_volume                     2363.15(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec QuazarTM MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20592
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.014
_diffrn_reflns_theta_min         3.533
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.5469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
; 
 Flack x determined using 1821 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0486P)^2^+0.2170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4370
_reflns_number_total             4497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03504_si_002.cif
_cod_data_source_block           yf160950_1_0m_a
_cod_database_code               4518101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.796
_shelx_res_checksum              53493
_shelx_hkl_checksum              89469