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_7060534
_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 H50 O4 S2, C H Cl3, C2 H3 N'
_chemical_formula_sum            'C45 H54 Cl3 N O4 S2'
_chemical_formula_weight         843.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-03-09 deposited with the CCDC.	2021-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                81.7910(14)
_cell_angle_beta                 89.8885(13)
_cell_angle_gamma                67.4880(12)
_cell_formula_units_Z            2
_cell_length_a                   12.5766(4)
_cell_length_b                   13.5696(4)
_cell_length_c                   13.9792(4)
_cell_measurement_reflns_used    206
_cell_measurement_temperature    180
_cell_measurement_theta_max      56.35
_cell_measurement_theta_min      12.24
_cell_volume                     2177.68(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_unetI/netI     0.049
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            80210
_diffrn_reflns_theta_full        68.338
_diffrn_reflns_theta_max         68.338
_diffrn_reflns_theta_min         3.568
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.134
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             891.986
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9828
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7965
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.0069543
_refine_ls_shift/su_mean         0.0001992
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ + 2.60P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1683
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1683
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                7188
_reflns_number_total             7965
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.45
_oxford_diffrn_Wilson_scale      40.57
_oxford_refine_ls_r_factor_ref   0.0610
_oxford_refine_ls_scale          0.19150(17)
_oxford_reflns_number_all        7965
_cod_data_source_file            d1nj01257f2.cif
_cod_data_source_block           8
_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 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H54 Cl3 N1 O4 S2'
_cod_database_code               7060534
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0610
_oxford_refine_ls_wr_factor_all  0.1683