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_7703446
_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         'C14 H20 N3 O2, C F3 O3 S'
_chemical_formula_sum            'C15 H20 F3 N3 O5 S'
_chemical_formula_weight         411.40
_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   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                117.321(9)
_cell_angle_beta                 91.458(6)
_cell_angle_gamma                97.837(6)
_cell_formula_units_Z            2
_cell_length_a                   8.8991(5)
_cell_length_b                   10.8721(10)
_cell_length_c                   11.4526(9)
_cell_measurement_reflns_used    2033
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.5440
_cell_measurement_theta_min      4.3270
_cell_volume                     970.37(15)
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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   -129.00  42.00   1.00    9.00    --  -42.88   0.00 -90.00  171
  2  \w      0.00  52.00   1.00    9.00    --   42.88 -37.00   0.00   52
  3  \w     32.00  76.00   1.00    9.00    --   42.88-125.00-150.00   44
  4  \w     31.00  87.00   1.00    9.00    --   42.88-125.00   0.00   56
  5  \w     47.00 133.00   1.00   32.50    --  105.68 -30.00   0.00   86
  6  \w     78.00 171.00   1.00   32.50    --  105.68  30.00   0.00   93
  7  \w     92.00 118.00   1.00   32.50    --  105.68-125.00  60.00   26
  8  \w     97.00 128.00   1.00   32.50    --  105.68 -61.00 150.00   31
  9  \w     80.00 114.00   1.00   32.50    --  105.68 163.00-101.00   34
 10  \w     92.00 148.00   1.00   32.50    --  105.68  61.00  30.00   56
 11  \w     38.00 137.00   1.00   32.50    --  105.68 -77.00 -30.00   99
 12  \w     40.00 109.00   1.00   32.50    --  105.68-125.00 -90.00   69
 13  \w     57.00 118.00   1.00   32.50    --  105.68-125.00-180.00   61
 14  \w     98.00 132.00   1.00   32.50    --  105.68  77.00-120.00   34
 15  \w     96.00 177.00   1.00   32.50    --  105.68 125.00  60.00   81
 16  \w     35.00  77.00   1.00   32.50    --  105.68 -61.00 150.00   42
 17  \w     37.00  64.00   1.00   32.50    --  105.68-125.00  60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148291000
_diffrn_orient_matrix_UB_12      0.1564707000
_diffrn_orient_matrix_UB_13      0.0616400000
_diffrn_orient_matrix_UB_21      0.0542103000
_diffrn_orient_matrix_UB_22      0.0195508000
_diffrn_orient_matrix_UB_23      0.1371873000
_diffrn_orient_matrix_UB_31      0.1663930000
_diffrn_orient_matrix_UB_32      0.0360327000
_diffrn_orient_matrix_UB_33      -0.0231379000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6582
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.411
_diffrn_reflns_theta_min         4.367
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.744
_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    1.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0582P)^2^+0.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2904
_reflns_number_total             3768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00049c2.cif
_cod_data_source_block           il-2-250_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7703444--7703450.cif.'
_cod_database_code               7703446
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C15 H20 N3 O5 F3 S1'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.615
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
;
_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 1.584
_oxdiff_exptl_absorpt_empirical_full_min 0.629