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_7126663
_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         '2(C F3 O3 S), C28 H45 N3'
_chemical_formula_sum            'C30 H45 F6 N3 O6 S2'
_chemical_formula_weight         721.81
_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             2019-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.195(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4405(6)
_cell_length_b                   19.9990(8)
_cell_length_c                   16.0796(8)
_cell_measurement_reflns_used    10051
_cell_measurement_temperature    120.03(10)
_cell_measurement_theta_max      28.6610
_cell_measurement_theta_min      2.8370
_cell_volume                     3514.6(3)
_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      120.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.872
_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    -32.00  12.00   0.50   48.00    --    7.20  38.00-120.00   88
  2  \w    -61.00  41.00   0.50   48.00    --    7.20 -77.00-120.00  204
  3  \w      4.00  30.00   0.50   48.00    --   -7.60 -82.00  90.00   52
  4  \w    -61.00   4.00   0.50   48.00    --   -7.60 -82.00 -30.00  130
  5  \w    -60.00  -5.00   0.50   48.00    --   -7.60 -82.00  90.00  110
;
_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      -0.0278654000
_diffrn_orient_matrix_UB_12      -0.0043721000
_diffrn_orient_matrix_UB_13      0.0336261000
_diffrn_orient_matrix_UB_21      -0.0227475000
_diffrn_orient_matrix_UB_22      0.0331699000
_diffrn_orient_matrix_UB_23      -0.0064821000
_diffrn_orient_matrix_UB_31      -0.0540813000
_diffrn_orient_matrix_UB_32      -0.0117257000
_diffrn_orient_matrix_UB_33      -0.0309259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28458
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.017
_diffrn_reflns_theta_min         2.761
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51235
_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    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8163
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.3676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6350
_reflns_number_total             8163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02807j2.cif
_cod_data_source_block           aj0723
_cod_depositor_comments
'Adding full bibliography for 7126655--7126664.cif.'
_cod_database_code               7126663
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N S O F'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.971
_reflns_odcompleteness_completeness 99.50
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2-O5 \\sim S2A-O5A
 with sigma of 0.02
 S2-O4 \\sim S2A-O4A
 with sigma of 0.02
 S2-O6 \\sim S2A-O6A
 with sigma of 0.02
 S2-C30 \\sim S2A-C30
 with sigma of 0.02
 O5-O4 \\sim O5A-O4A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O5-C30 \\sim O5A-C30
 with sigma of 0.04
 O4-O6 \\sim O4A-O6A
 with sigma of 0.04
 O4-C30 \\sim O4A-C30
 with sigma of 0.04
 O6-C30 \\sim O6A-C30
 with sigma of 0.04
 F4-C30 \\sim F4A-C30
 with sigma of 0.02
 F5-C30 \\sim F5A-C30
 with sigma of 0.02
 F6-C30 \\sim F6A-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F6A)
4. Rigid body (RIGU) restrains
 S2, O5, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6A, O5A, O4A, S2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4A, F6A, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O6A)=Sof(O5A)=Sof(O4A)=Sof(S2A)=1-FVAR(1)
 Sof(S2)=Sof(O5)=Sof(O4)=Sof(O6)=FVAR(1)
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C26(H26), C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21)
6.d X=CH2 refined with riding coordinates:
 C13(H13A,H13B)
6.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C25(H25A,H25B,
 H25C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C24(H24A,
 H24B,H24C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              56491
_shelx_hkl_checksum              97404
_shelx_fab_checksum              25873
_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 1.420
_oxdiff_exptl_absorpt_empirical_full_min 0.446