Trisubstituted geminal diazaalkene derived transient 1,2-carbodications.
Mandal, Debdeep; Stein, Felix; Chandra, Shubhadeep; Neuman, Nicolás I; Sarkar, Pallavi; Das, Shubhajit; Kundu, Abhinanda; Sarkar, Arighna; Rawat, Hemant; Pati, Swapan K.; Chandrasekhar, Vadapalli; Sarkar, Biprajit; Jana, Anukul; Chemical communications (Cambridge, England) 56 (2020) 8233–8236; doi:10.1039/d0cc02807j

data_7126655
_publ_section_title
;
 Trisubstituted geminal diazaalkene derived transient 1,2-carbodications.
;
_journal_issue                   59
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8233
_journal_page_last               8236
_journal_paper_doi               10.1039/d0cc02807j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C F3 O3 S, C19 H36 N3'
_chemical_formula_sum            'C20 H36 F3 N3 O3 S'
_chemical_formula_weight         455.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-06 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.002(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5596(6)
_cell_length_b                   16.1768(9)
_cell_length_c                   12.4775(8)
_cell_measurement_reflns_used    7527
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5040
_cell_measurement_theta_min      2.9950
_cell_volume                     2324.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     70.00  95.00   0.50   40.00    --    7.10  77.00 -60.00   50
  2  \w     62.00  93.00   0.50   40.00    --    7.10  38.00-150.00   62
  3  \w     59.00  96.00   0.50   40.00    --    7.10  77.00-150.00   74
  4  \w    -26.00  30.00   0.50   40.00    --   -7.50  57.00 -90.00  112
  5  \w    -63.00  35.00   0.50   40.00    --   -7.50 -82.00 -90.00  196
  6  \w      5.00  35.00   0.50   40.00    --   -7.50 -82.00 -60.00   60
  7  \w     46.00  71.00   0.50   40.00    --   -7.50  57.00 -90.00   50
  8  \w    -59.00 -32.00   0.50   40.00    --   -7.50 -82.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0190717000
_diffrn_orient_matrix_UB_12      0.0173498000
_diffrn_orient_matrix_UB_13      -0.0475859000
_diffrn_orient_matrix_UB_21      0.0130111000
_diffrn_orient_matrix_UB_22      -0.0401321000
_diffrn_orient_matrix_UB_23      -0.0185083000
_diffrn_orient_matrix_UB_31      -0.0570687000
_diffrn_orient_matrix_UB_32      -0.0034050000
_diffrn_orient_matrix_UB_33      -0.0255363000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5448
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.965
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5448
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.1055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+6.6290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2703
_refine_ls_wR_factor_ref         0.2841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4226
_reflns_number_total             5448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02807j2.cif
_cod_data_source_block           aj0629
_cod_depositor_comments
'Adding full bibliography for 7126655--7126664.cif.'
_cod_database_code               7126655
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O S F'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.859(5)
 0.141(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1-O5 \\sim S1-O3
 with sigma of 0.02
 S1-O2 \\sim S1-O6
 with sigma of 0.02
 S1-O4 \\sim S1-O1
 with sigma of 0.02
 C20-F5 \\sim C20-F2
 with sigma of 0.02
 C20-F1 \\sim C20-F4
 with sigma of 0.02
 C20-F3 \\sim C20-F6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3)=Sof(O1)=Sof(O6)=Sof(F2)=Sof(F4)=Sof(F6)=1-FVAR(1)
 Sof(O5)=Sof(F5)=Sof(O2)=Sof(F1)=Sof(F3)=Sof(O4)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C9(H9), C5(H5)
7.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B)
7.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              9103
_shelx_hkl_checksum              44344
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.791