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_7126658
_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         'C8 H15 N2, C F3 O3 S'
_chemical_formula_sum            'C9 H15 F3 N2 O3 S'
_chemical_formula_weight         288.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5710(17)
_cell_length_b                   6.9720(14)
_cell_length_c                   21.017(4)
_cell_measurement_reflns_used    7751
_cell_measurement_temperature    119.98(10)
_cell_measurement_theta_max      28.6370
_cell_measurement_theta_min      3.0630
_cell_volume                     1255.9(4)
_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      119.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_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     49.00  74.00   0.50    6.00    --    7.10  75.00 125.00   50
  2  \w      5.00  30.00   0.50    6.00    --   -7.50 -75.00  -1.00   50
  3  \w    -49.00 -23.00   0.50    6.00    --   -7.50 -75.00  -1.00   52
  4  \w     17.00  42.00   0.50    6.00    --   -7.50  75.00 125.00   50
  5  \w     58.00  95.00   0.50    6.00    --    7.10  77.00-120.00   74
  6  \w    -43.00 -17.00   0.50    6.00    --    7.10 -75.00  -1.00   52
  7  \w     57.00  86.00   0.50    6.00    --    7.10  77.00  90.00   58
  8  \w     63.00  88.00   0.50    6.00    --    7.10  77.00 -30.00   50
  9  \w     56.00  92.00   0.50    6.00    --    7.10  77.00  30.00   72
 10  \w     51.00  76.00   0.50    6.00    --    7.10  77.00-150.00   50
 11  \w    -96.00  80.00   0.50    6.00    --   -7.50 -19.00 -30.00  352
;
_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      -0.0192021000
_diffrn_orient_matrix_UB_12      0.0392647000
_diffrn_orient_matrix_UB_13      0.0300655000
_diffrn_orient_matrix_UB_21      -0.0423429000
_diffrn_orient_matrix_UB_22      0.0739955000
_diffrn_orient_matrix_UB_23      -0.0152039000
_diffrn_orient_matrix_UB_31      -0.0684234000
_diffrn_orient_matrix_UB_32      -0.0567951000
_diffrn_orient_matrix_UB_33      0.0009716000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15371
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.930
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64496
_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    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0636P)^2^+1.4087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1485
_reflns_number_total             1670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02807j2.cif
_cod_data_source_block           aj0622
_cod_depositor_comments
'Adding full bibliography for 7126655--7126664.cif.'
_cod_database_code               7126658
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O S F '
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B), C5(H5A,H5B)
;
_shelx_res_checksum              45000
_shelx_hkl_checksum              48459
_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 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.693