Modular Sulfondiimine Synthesis Using a Stable Sulfinylamine Reagent.
Zhang, Ze-Xin; Davies, Thomas Q.; Willis, Michael C.; Journal of the American Chemical Society 141 (2019) 13022–13027; doi:10.1021/jacs.9b06831

data_4127831
_publ_section_title
;
 Modular Sulfondiimine Synthesis Using a Stable Sulfinylamine Reagent.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13022
_journal_page_last               13027
_journal_paper_doi               10.1021/jacs.9b06831
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C27 H32 F1 N3 O4 S2'
_chemical_formula_sum            'C27 H32 F N3 O4 S2'
_chemical_formula_weight         545.70
_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
_cell_angle_alpha                104.834(3)
_cell_angle_beta                 106.298(3)
_cell_angle_gamma                104.704(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0832(4)
_cell_length_b                   11.5760(4)
_cell_length_c                   12.3004(4)
_cell_measurement_reflns_used    7012
_cell_measurement_temperature    170
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1371.07(10)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection
'XtaLAB mini II Rigaku Oxford Diffraction, 2018'
_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 0.985
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction '
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25329
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.843
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9668
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7942
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.0002231
_refine_ls_shift/su_mean         0.0000179
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1297
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1297
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6030
_reflns_number_total             7942
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0657
_oxford_refine_ls_scale          3.80(4)
_oxford_reflns_number_all        7942
_cod_data_source_file            ja9b06831_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C27 H32 F1 N3 O4 S2'
_cod_database_code               4127831
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)