Electrophile dependent mechanisms in the asymmetric trapping of α-lithio-<i>N</i>-(<i>tert</i>-butoxythiocarbonyl)azetidine.
Delany, Pascal K.; Mortimer, Claire L.; Hodgson, David M.; Chemical communications (Cambridge, England) 56 (2020) 12174–12177; doi:10.1039/d0cc05396a

data_7127220
_publ_section_title
;
 Electrophile dependent mechanisms in the asymmetric trapping of
 \a-lithio-<i>N</i>-(<i>tert</i>-butoxythiocarbonyl)azetidine.
;
_journal_issue                   81
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12174
_journal_page_last               12177
_journal_paper_doi               10.1039/d0cc05396a
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H22 F3 N O2 Sn'
_chemical_formula_sum            'C16 H22 F3 N O2 Sn'
_chemical_formula_weight         436.04
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-23
_audit_creation_method           'CRYSTALS_ver_14.61_build_7285 '
_audit_update_record
;
2020-09-03 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.528(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7115(5)
_cell_length_b                   12.6744(4)
_cell_length_c                   12.5355(7)
_cell_measurement_reflns_used    4802
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.97
_cell_measurement_theta_min      3.75
_cell_volume                     1809.10(14)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.059
_diffrn_reflns_av_unetI/netI     0.111
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17707
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.343
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl Ether'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.07
_refine_diff_density_min         -1.62
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 3289 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8294
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.0008840
_refine_ls_shift/su_mean         0.0000226
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1349
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1349
_reflns_limit_h_max              14
_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                5775
_reflns_number_total             8301
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.62
_oxford_diffrn_Wilson_scale      0.99
_oxford_refine_ls_r_factor_ref   0.0949
_oxford_refine_ls_scale          1.065(3)
_oxford_reflns_number_all        8294
_oxford_structure_analysis_title 016OS20-KEC
_cod_data_source_file            d0cc05396a2.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

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 7127220.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               7127220
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  -0.052(19)
_oxford_bijvoet_difference       -0.06(2)
_oxford_refined_flack_x          -0.05(3)