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_7126664
_publ_section_title
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 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         'C28 H45 N3'
_chemical_formula_sum            'C28 H45 N3'
_chemical_formula_weight         423.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-04
_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                73.417(3)
_cell_angle_beta                 88.835(3)
_cell_angle_gamma                73.820(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4090(3)
_cell_length_b                   10.8582(4)
_cell_length_c                   13.6751(5)
_cell_measurement_reflns_used    11401
_cell_measurement_temperature    119.96(10)
_cell_measurement_theta_max      28.9570
_cell_measurement_theta_min      2.6580
_cell_volume                     1283.31(8)
_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  'olex2.refine (Bourhis et al., 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 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_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    -42.00 -16.00   0.50   10.00    --    7.10 -63.00  44.00   52
  2  \w     -3.00  22.00   0.50   10.00    --   -7.50  63.00-178.00   50
  3  \w    -36.00 -11.00   0.50   10.00    --   -7.50 -63.00  44.00   50
  4  \w    -73.00 -47.00   0.50   10.00    --   -7.50 -63.00  44.00   52
  5  \w     50.00  94.00   0.50   10.00    --    7.10  77.00  90.00   88
  6  \w    -34.00  96.00   0.50   10.00    --    7.10  38.00  30.00  260
  7  \w     50.00  96.00   0.50   10.00    --    7.10  77.00-120.00   92
  8  \w     30.00  56.00   0.50   10.00    --    7.10  63.00-178.00   52
  9  \w     51.00  94.00   0.50   10.00    --    7.10  77.00  30.00   86
 10  \w     67.00  93.00   0.50   10.00    --    7.10  77.00 -60.00   52
 11  \w    -61.00  35.00   0.50   10.00    --   -7.50 -82.00 150.00  192
 12  \w    -82.00 -34.00   0.50   10.00    --   -7.50 -57.00  60.00   96
 13  \w     -1.00  35.00   0.50   10.00    --   -7.50 -82.00-120.00   72
 14  \w    -48.00 -23.00   0.50   10.00    --   -7.50 -82.00-120.00   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      -0.0421788000
_diffrn_orient_matrix_UB_12      -0.0463994000
_diffrn_orient_matrix_UB_13      0.0153770000
_diffrn_orient_matrix_UB_21      0.0332152000
_diffrn_orient_matrix_UB_22      -0.0325061000
_diffrn_orient_matrix_UB_23      -0.0364365000
_diffrn_orient_matrix_UB_31      0.0574856000
_diffrn_orient_matrix_UB_32      -0.0429653000
_diffrn_orient_matrix_UB_33      0.0371074000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22678
_diffrn_reflns_theta_full        24.9986
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68808
_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    1.0964
_exptl_crystal_description       block
_exptl_crystal_F_000             468.1519
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.2770
_refine_diff_density_min         -0.2136
_refine_diff_density_rms         0.0380
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.9019
_refine_ls_goodness_of_fit_ref   1.0320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0320
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.4817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4018
_reflns_number_total             4504
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc02807j2.cif
_cod_data_source_block           AJ0705
_cod_depositor_comments
'Adding full bibliography for 7126655--7126664.cif.'
_cod_database_code               7126664
_chemical_oxdiff_formula         'C H N '
_reflns_odcompleteness_completeness 99.62
_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.a Ternary CH refined with riding coordinates:
 C5(H5), C20(H20), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C4(H4)
2.d Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C18(H18a,H18b,H18c), C24(H24a,H24b,H24c), C25(H25a,H25b,
 H25c), C22(H22a,H22b,H22c), C19(H19a,H19b,H19c), C28(H28a,H28b,H28c), C21(H21a,
 H21b,H21c), C17(H17a,H17b,H17c), C26(H26a,H26b,H26c), C16(H16a,H16b,H16c),
 C27(H27a,H27b,H27c)
;
_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 1.493
_oxdiff_exptl_absorpt_empirical_full_min 0.662