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_7126659
_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         '4(C F3 O3 S), 2(C16 H29 N3)'
_chemical_formula_sum            'C36 H58 F12 N6 O12 S4'
_chemical_formula_weight         1123.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-19
_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                81.547(2)
_cell_angle_beta                 87.795(2)
_cell_angle_gamma                80.681(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2515(2)
_cell_length_b                   15.1873(5)
_cell_length_c                   20.3300(5)
_cell_measurement_reflns_used    17243
_cell_measurement_temperature    119.96(10)
_cell_measurement_theta_max      28.8910
_cell_measurement_theta_min      2.9290
_cell_volume                     2486.50(12)
_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      119.96(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.878
_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    -44.00  21.00   0.50   10.42    --    7.20  19.00  90.00  130
  2  \w    -50.00 -22.00   0.50   10.42    --    7.20 -82.00-120.00   56
  3  \w     58.00  97.00   0.50   10.42    --    7.20  77.00  90.00   78
  4  \w     42.00  82.00   0.50   10.42    --    7.20  19.00  90.00   80
  5  \w      9.00  34.00   0.50   10.42    --    7.20 -82.00-120.00   50
  6  \w    -55.00  50.00   0.50   10.42    --    7.20 -82.00  60.00  210
  7  \w     52.00  95.00   0.50   10.42    --    7.20  77.00-120.00   86
  8  \w    -60.00   9.00   0.50   10.42    --   -7.60 -82.00-180.00  138
  9  \w      6.00  36.00   0.50   10.42    --   -7.60 -82.00   0.00   60
 10  \w    -87.00   0.00   0.50   10.42    --   -7.60 -57.00 -90.00  174
 11  \w     11.00  36.00   0.50   10.42    --   -7.60 -82.00  90.00   50
 12  \w    -37.00 -12.00   0.50   10.42    --   -7.60 -82.00  90.00   50
;
_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      -0.0063707000
_diffrn_orient_matrix_UB_12      -0.0226294000
_diffrn_orient_matrix_UB_13      0.0328718000
_diffrn_orient_matrix_UB_21      0.0863808000
_diffrn_orient_matrix_UB_22      -0.0047572000
_diffrn_orient_matrix_UB_23      0.0032319000
_diffrn_orient_matrix_UB_31      -0.0093630000
_diffrn_orient_matrix_UB_32      0.0418547000
_diffrn_orient_matrix_UB_33      0.0123867000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40324
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87813
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         11593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.5357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9341
_reflns_number_total             11593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02807j2.cif
_cod_data_source_block           aj0722
_cod_depositor_comments
'Adding full bibliography for 7126655--7126664.cif.'
_cod_database_code               7126659
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N S O F '
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.962
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N6(H6), N3(H3), C26(H26), C8(H8), C25(H25), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C28(H28a,H28b)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C4(H4a,H4b,H4c), C15(H15a,H15b,H15c), C6(H6a,H6b,H6c),
 C16(H16a,H16b,H16c), C7(H7a,H7b,H7c), C13(H13a,H13b,H13c), C30(H30a,H30b,H30c),
  C33(H33a,H33b,H33c), C14(H14a,H14b,H14c), C21(H21a,H21b,H21c), C5(H5a,H5b,
 H5c), C22(H22a,H22b,H22c), C32(H32a,H32b,H32c), C20(H20a,H20b,H20c), C31(H31a,
 H31b,H31c)
;
_shelx_res_checksum              72635
_shelx_hkl_checksum              93205
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.738