Brønsted and Lewis acid adducts of triazenes.
Landman, Iris R.; Suleymanov, Abdusalom A.; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Chadwick, F. Mark; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2317–2322; doi:10.1039/d0dt00049c

data_7703450
_publ_section_title
;
 Br\/onsted and Lewis acid adducts of triazenes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2317
_journal_page_last               2322
_journal_paper_doi               10.1039/d0dt00049c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C12 H24 N3 O, C F3 O3 S'
_chemical_formula_sum            'C13 H24 F3 N3 O4 S'
_chemical_formula_weight         375.41
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-20 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2766(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.05100(19)
_cell_length_b                   10.81512(18)
_cell_length_c                   15.9625(3)
_cell_measurement_reflns_used    13102
_cell_measurement_temperature    139.98(11)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      4.0990
_cell_volume                     1864.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_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      139.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_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    -62.00  31.00   1.00    1.00    --  -40.85  57.00  30.00   93
  2  \w   -115.00 -22.00   1.00    1.00    --  -40.85 -38.00-120.00   93
  3  \w   -113.00 -22.00   1.00    1.00    --  -40.85 -38.00 150.00   91
  4  \w     50.00  92.00   1.00    1.00    --   40.85-125.00-120.00   42
  5  \w      2.00  81.00   1.00    1.00    --   40.85 -99.00 120.00   79
  6  \w     87.00 129.00   1.00    4.00    --  112.00 -30.00 -60.00   42
  7  \w     45.00  71.00   1.00    4.00    --  112.00 -30.00 -60.00   26
  8  \w     42.00  68.00   1.00    4.00    --  112.00 -94.00 -30.00   26
  9  \w    119.00 178.00   1.00    4.00    --  112.00 111.00  60.00   59
 10  \w     36.00 112.00   1.00    4.00    --  112.00-111.00  60.00   76
 11  \w     90.00 137.00   1.00    4.00    --  112.00 -61.00 -30.00   47
 12  \w     37.00  68.00   1.00    4.00    --  112.00-111.00 -60.00   31
 13  \w     80.00 112.00   1.00    4.00    --  112.00-111.00 -60.00   32
 14  \w     30.00  82.00   1.00    4.00    --  112.00 -94.00   0.00   52
 15  \w     91.00 160.00   1.00    4.00    --  112.00  30.00 120.00   69
 16  \w     95.00 140.00   1.00    4.00    --  112.00 -61.00 120.00   45
 17  \w     60.00 113.00   1.00    4.00    --  112.00-111.00-150.00   53
 18  \w     95.00 139.00   1.00    4.00    --  112.00 -77.00 150.00   44
 19  \w     30.00 168.00   1.00    4.00    --  112.00   0.00 -90.00  138
 20  \w     40.00  68.00   1.00    4.00    --  112.00 -94.00 120.00   28
 21  \w     36.00 123.00   1.00    4.00    --  112.00 -30.00 120.00   87
 22  \w     56.00  83.00   1.00    4.00    --  112.00 -61.00 -30.00   27
 23  \w     96.00 123.00   1.00    4.00    --  112.00-132.00 177.59   27
 24  \w     37.00 109.00   1.00    4.00    --  112.00-111.00-180.00   72
 25  \w     88.00 113.00   1.00    4.00    --  112.00-111.00 -90.00   25
 26  \w     85.00 140.00   1.00    4.00    --  112.00 -77.00  30.00   55
 27  \w     73.00 109.00   1.00    4.00    --  112.00-111.00   0.00   36
 28  \w     62.00  92.00   1.00    4.00    --  112.00  15.00  30.00   30
 29  \w     97.00 122.00   1.00    4.00    --  112.00  15.00  30.00   25
 30  \w     41.00  66.00   1.00    4.00    --  112.00-111.00-120.00   25
 31  \w     50.00  86.00   1.00    4.00    --  112.00-132.00 177.59   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0781912000
_diffrn_orient_matrix_UB_12      -0.1189321000
_diffrn_orient_matrix_UB_13      0.0167462000
_diffrn_orient_matrix_UB_21      0.0734915000
_diffrn_orient_matrix_UB_22      0.0406853000
_diffrn_orient_matrix_UB_23      -0.0671744000
_diffrn_orient_matrix_UB_31      0.0939659000
_diffrn_orient_matrix_UB_32      0.0671372000
_diffrn_orient_matrix_UB_33      0.0704068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16719
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.004
_diffrn_reflns_theta_min         4.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.013
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019).
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics as
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.443
_exptl_crystal_size_min          0.366
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0667P)^2^+1.0802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3730
_reflns_number_total             3844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00049c2.cif
_cod_data_source_block           il-1-83
_cod_depositor_comments
'Adding full bibliography for 7703444--7703450.cif.'
_cod_original_cell_volume        1864.18(5)
_cod_database_code               7703450
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C13 H24 N3 O4 F3 S1'
_shelx_estimated_absorpt_t_max   0.526
_shelx_estimated_absorpt_t_min   0.351
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H6D)=Sof(H6E)=Sof(H6F)=1-FVAR(1)
 Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
 Sof(H4D)=Sof(H4E)=Sof(H4F)=1-FVAR(2)
 Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Disordered Me refined as rotating group:
 C4(H4A,H4B,H4C,H4D,H4E,H4F), C6(H6A,H6B,H6C,H6D,H6E,H6F)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C)
;
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 17.741
_oxdiff_exptl_absorpt_empirical_full_min 0.453