Diverse saturated heterocycles from a hydroacylation/conjugate addition cascade
Iwumene, Ndidi U. N.; Moseley, Daniel. F.; Pullin, Robert D. C.; Willis, Michael C.; Chemical Science 13 (2022) 1504–1511; doi:10.1039/D1SC06900D

data_1566047
_publ_section_title
;
 Diverse saturated heterocycles from a hydroacylation/conjugate addition
 cascade
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1504
_journal_page_last               1511
_journal_paper_doi               10.1039/D1SC06900D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C14 H20 O3 S1'
_chemical_formula_sum            'C14 H20 O3 S'
_chemical_formula_weight         268.38
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-06-24 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.199(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2921(5)
_cell_length_b                   7.3930(3)
_cell_length_c                   15.8524(5)
_cell_measurement_reflns_used    5580
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.89
_cell_measurement_theta_min      2.38
_cell_volume                     1402.54(9)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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_temperature      170
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.043
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15714
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         30.542
_diffrn_reflns_theta_min         1.900
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       205(16)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9736
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.0015630
_refine_ls_shift/su_mean         0.0000827
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.55P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0962
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0962
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3190
_reflns_number_total             4140
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      0.17
_oxford_refine_ls_r_factor_ref   0.0548
_oxford_refine_ls_scale          2.48(2)
_oxford_reflns_number_all        4140
_cod_data_source_file            d1sc06900d2.cif
_cod_data_source_block           DM04_b_v2
_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 1566046--1566049.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C14 H20 O3 S1'
_cod_database_code               1566047
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0548
_oxford_refine_ls_wr_factor_all  0.0962