Regio- and stereoselectivity of spirodienone formation in 2,14-dithiacalix[4]arene
Kortus, D.; Eigner, V.; Lhoták, P.; New Journal of Chemistry 45 (2021) 8563–8571; doi:10.1039/D1NJ01257F

data_7060532
_publ_section_title
;
 Regio- and stereoselectivity of spirodienone formation in
 2,14-dithiacalix[4]arene
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8563
_journal_page_last               8571
_journal_paper_doi               10.1039/D1NJ01257F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C42 H48 O4 S2'
_chemical_formula_sum            'C42 H48 O4 S2'
_chemical_formula_weight         680.97
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-03-09 deposited with the CCDC.	2021-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5237(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1940(5)
_cell_length_b                   12.1754(4)
_cell_length_c                   10.6117(4)
_cell_measurement_reflns_used    117
_cell_measurement_temperature    180
_cell_measurement_theta_max      56.20
_cell_measurement_theta_min      10.80
_cell_volume                     1832.11(11)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_unetI/netI     0.088
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31721
_diffrn_reflns_theta_full        72.057
_diffrn_reflns_theta_max         72.057
_diffrn_reflns_theta_min         3.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0004765
_refine_ls_shift/su_mean         0.0000534
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.83P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1077
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1077
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                3147
_reflns_number_total             3595
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.99
_oxford_diffrn_Wilson_scale      27.96
_oxford_refine_ls_r_factor_ref   0.0448
_oxford_refine_ls_scale          0.19772(15)
_oxford_reflns_number_all        3595
_cod_data_source_file            d1nj01257f2.cif
_cod_data_source_block           7B12alt
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7060531--7060535.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7060532
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0448
_oxford_refine_ls_wr_factor_all  0.1077