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_4127829
_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         'C21 H28 F1 N3 O4 S2'
_chemical_formula_sum            'C21 H28 F N3 O4 S2'
_chemical_formula_weight         469.60
_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                87.164(3)
_cell_angle_beta                 86.258(3)
_cell_angle_gamma                68.098(4)
_cell_formula_units_Z            2
_cell_length_a                   7.0268(3)
_cell_length_b                   7.1474(3)
_cell_length_c                   24.4123(9)
_cell_measurement_reflns_used    5674
_cell_measurement_temperature    170
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1134.73(9)
_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 0.982
_diffrn_measured_fraction_theta_max 0.940
_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  0.038
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20580
_diffrn_reflns_theta_full        25.738
_diffrn_reflns_theta_max         30.640
_diffrn_reflns_theta_min         2.509
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0463
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.0062488
_refine_ls_shift/su_mean         0.0011970
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.44P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1380
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1356
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                5250
_reflns_number_total             6575
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.87
_oxford_diffrn_Wilson_scale      0.43
_oxford_refine_ls_r_factor_ref   0.0719
_oxford_refine_ls_scale          1.614(8)
_oxford_reflns_number_all        6575
_cod_data_source_file            ja9b06831_si_003.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        'C21 H28 F1 N3 O4 S2'
_cod_database_code               4127829
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)