Small molecule activation: SbF3 auto-ionization supported by transfer and mesoionic NHC rearrangement.
Alič, Blaž; Štefančič, Aleš; Tavčar, Gašper; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3338–3346; doi:10.1039/c6dt04909e

data_7042043
_publ_section_title
;
 Small molecule activation: SbF3 auto-ionization supported by transfer and
 mesoionic NHC rearrangement.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3338
_journal_page_last               3346
_journal_paper_doi               10.1039/c6dt04909e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C27 H37 N2, 0.5(F8 Sb2), 0.5(C4 H6 N2)'
_chemical_formula_sum            'C29 H40 F4 N3 Sb'
_chemical_formula_weight         628.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-21 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3988(4)
_cell_length_b                   13.5732(3)
_cell_length_c                   10.4153(2)
_cell_measurement_reflns_used    22189
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.2590
_cell_measurement_theta_min      3.8340
_cell_volume                     3025.13(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6426
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -118.00 -72.00   1.00    9.43    --  -39.93 -77.00 -90.00   46
  2  \w   -105.00 -16.00   1.00    9.43    --  -39.93 -38.00 -90.00   89
  3  \w    -71.00  -6.00   1.00    9.43    --  -39.93 -77.00-150.00   65
  4  \w   -118.00  -6.00   1.00    9.43    --  -39.93 -77.00 150.00  112
  5  \w    -59.00  -7.00   1.00    9.43    --  -39.93 -77.00   0.00   52
  6  \w   -105.00  -7.00   1.00    9.43    --  -39.93 -77.00  90.00   98
  7  \w   -106.00 -18.00   1.00    9.43    --  -39.93 -38.00   0.00   88
  8  \w    -96.00  -4.00   1.00    9.43    --  -39.93 125.00-180.00   92
  9  \w    -63.00  -6.00   1.00    9.43    --  -39.93 -77.00 -90.00   57
 10  \w    -33.00  70.00   1.00    9.43    --   39.93 -57.00   0.00  103
 11  \w     68.00 117.00   1.00    9.43    --   39.93 167.00  58.00   49
 12  \w    -18.00  37.00   1.00    9.43    --   39.93 -77.00 150.00   55
 13  \w     73.00  98.00   1.00   37.73    --  106.51  77.00  90.00   25
 14  \w     76.00 103.00   1.00   37.73    --  106.51  61.00  90.00   27
 15  \w     52.00  93.00   1.00   37.73    --  106.51-111.00   0.00   41
 16  \w     23.00 107.00   1.00   37.73    --  106.51 -94.00 -90.00   84
 17  \w     73.00 136.00   1.00   37.73    --  106.51  77.00-180.00   63
 18  \w     76.00 113.00   1.00   37.73    --  106.51  61.00-180.00   37
 19  \w     73.00 100.00   1.00   37.73    --  106.51  77.00-150.00   27
 20  \w     32.00 107.00   1.00   37.73    --  106.51 -94.00  90.00   75
 21  \w     73.00 178.00   1.00   37.73    --  106.51  77.00-120.00  105
 22  \w     76.00 139.00   1.00   37.73    --  106.51  61.00 -30.00   63
 23  \w     76.00 109.00   1.00   37.73    --  106.51  61.00 -60.00   33
 24  \w     73.00 178.00   1.00   37.73    --  106.51  77.00 -30.00  105
 25  \w     73.00  98.00   1.00   37.73    --  106.51  77.00 -90.00   25
 26  \w    114.00 178.00   1.00   37.73    --  106.51  77.00 -90.00   64
 27  \w     73.00 142.00   1.00   37.73    --  106.51  77.00  30.00   69
 28  \w     73.00 178.00   1.00   37.73    --  106.51  77.00  60.00  105
 29  \w     76.00 113.00   1.00   37.73    --  106.51  61.00-120.00   37
 30  \w     77.00 116.00   1.00   37.73    --  106.51  61.00  30.00   39
 31  \w    119.00 178.00   1.00   37.73    --  106.51  77.00   0.00   59
 32  \w     73.00  98.00   1.00   37.73    --  106.51  77.00 150.00   25
 33  \w     73.00  99.00   1.00   37.73    --  106.51  77.00   0.00   26
 34  \w     76.00 162.00   1.00   37.73    --  106.51  61.00-150.00   86
 35  \w     76.00 102.00   1.00   37.73    --  106.51  61.00  60.00   26
 36  \w     76.00 103.00   1.00   37.73    --  106.51  61.00 -90.00   27
 37  \w     76.00 103.00   1.00   37.73    --  106.51  61.00   0.00   27
 38  \w     76.00 110.00   1.00   37.73    --  106.51  61.00 120.00   34
 39  \w     73.00 127.00   1.00   37.73    --  106.51  77.00 -60.00   54
 40  \w    117.00 177.00   1.00   37.73    --  106.51  77.00  90.00   60
 41  \w     28.00 115.00   1.00   37.73    --  106.51-111.00  60.00   87
 42  \w     73.00 104.00   1.00   37.73    --  106.51  77.00 120.00   31
 43  \w     22.00 105.00   1.00   37.73    --  106.51 -94.00-180.00   83
 44  \w     73.00 177.00   1.00   37.73    --  106.51  76.00 135.86  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0474028000
_diffrn_orient_matrix_UB_12      0.0743934000
_diffrn_orient_matrix_UB_13      0.0547107000
_diffrn_orient_matrix_UB_21      0.0529901000
_diffrn_orient_matrix_UB_22      -0.0753399000
_diffrn_orient_matrix_UB_23      -0.0194616000
_diffrn_orient_matrix_UB_31      0.0114648000
_diffrn_orient_matrix_UB_32      0.0405727000
_diffrn_orient_matrix_UB_33      -0.1361458000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            40036
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         4.132
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.622
_exptl_absorpt_correction_T_max  0.147
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.751
_exptl_crystal_size_mid          0.605
_exptl_crystal_size_min          0.596
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0268P)^2^+16.7990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2752
_reflns_number_total             2830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04909e2.cif
_cod_data_source_block           chsbf4-_1
_cod_depositor_comments
'Adding full bibliography for 7042042--7042045.cif.'
_cod_database_code               7042043
_chemical_oxdiff_formula         'C27 H37 N2 Sb F4'
_reflns_odcompleteness_completeness 99.94
_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. Others
 Fixed Sof: Sb1(0.5) F1(0.5) N4(0.5) C21(0.5) H20B(0.5) H20C(0.5)
 Fixed X: H20A(0.46026) H20B(0.39766) H20C(0.39766)
 Fixed Y: H20A(0.25) H20B(0.30775) H20C(0.19225)
 Fixed Z: H20A(0.622231) H20B(0.64347) H20C(0.64347)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              63860
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1788
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 28.148
_oxdiff_exptl_absorpt_empirical_full_min 0.316