Oxidative addition/cycloaddition of arenesulfonamides and triflamide to N-allyltriflamide and N,N-diallyltriflamide
Shainyan, B. A.; Astakhova, V. V.; Ganin, A. S.; Moskalik, M. Yu; Sterkhova, I. V.; RSC Adv. 7 (2017) 38951–; doi:10.1039/C7RA05831D

data_7228892
_publ_section_title
;
 Oxidative addition/cycloaddition of arenesulfonamides and triflamide to
 N-allyltriflamide and N,N-diallyltriflamide
;
_journal_issue                   62
_journal_name_full               'RSC Adv.'
_journal_page_first              38951
_journal_paper_doi               10.1039/C7RA05831D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C9 H10 F9 N3 O6 S3'
_chemical_formula_weight         523.88
_chemical_melting_point          456
_chemical_name_systematic
3,7,9-tris[(trifluoromethyl)sulfonyl]-3,7,9-triazabicyclo[3.3.1]nonane
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                73.267(14)
_cell_angle_beta                 78.954(14)
_cell_angle_gamma                80.979(14)
_cell_formula_units_Z            4
_cell_length_a                   11.214(4)
_cell_length_b                   11.857(5)
_cell_length_c                   14.874(7)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     1848.0(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40457
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.439
_diffrn_reflns_theta_min         2.174
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1050
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1227P)^2^+9.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7103
_reflns_number_total             9983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra05831d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
;

2017-10-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1848.0(13)
_cod_original_formula_sum        'C18 H21 F18 N6 O12 S6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1047.77
_cod_database_code               7228892
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.830
_shelxl_version_number           2013-3
_shelx_res_checksum              65704