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_7060533
_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         '2(C42 H48 O4 S2), C H2 Cl2'
_chemical_formula_sum            'C85 H98 Cl2 O8 S4'
_chemical_formula_weight         1446.90
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 110.3901(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2615(4)
_cell_length_b                   25.8210(6)
_cell_length_c                   19.9165(4)
_cell_measurement_reflns_used    208
_cell_measurement_temperature    180
_cell_measurement_theta_max      53.20
_cell_measurement_theta_min      11.70
_cell_volume                     7838.7(3)
_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     0.044
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80775
_diffrn_reflns_theta_full        70.262
_diffrn_reflns_theta_max         70.262
_diffrn_reflns_theta_min         3.367
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3080.052
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9527
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7470
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.0257804
_refine_ls_shift/su_mean         0.0001326
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +12.54P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1240
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6674
_reflns_number_total             7472
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      242.70
_oxford_refine_ls_r_factor_ref   0.0486
_oxford_refine_ls_scale          0.065942(14)
_oxford_reflns_number_all        7470
_cod_data_source_file            d1nj01257f2.cif
_cod_data_source_block           7A13alt7A12altCH2Cl2
_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     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7060533
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0486
_oxford_refine_ls_wr_factor_all  0.1240