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_7042042
_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 H35 Cl2 N2, C7 H8, F4 Sb'
_chemical_formula_sum            'C34 H43 Cl2 F4 N2 Sb'
_chemical_formula_weight         748.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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2016-12-21 deposited with the CCDC.
2017-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0196(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.07389(10)
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_cell_measurement_reflns_used    15289
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0140
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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_diffrn_ambient_environment      N~2~
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -74.00   39.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263   77.0000  120.0000 113

  2 omega -114.00  -10.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263  -57.0000   90.0000 104

  3 omega -114.00  -10.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263  -57.0000 -180.0000 104

  4 omega   79.00  178.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101   45.0000  -30.0000 99

  5 omega   32.00   98.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101  -45.0000  -60.0000 66

  6 omega   32.00   98.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101  -45.0000 -150.0000 66

  7 omega   79.00  178.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101   45.0000   60.0000 99

  8 omega   32.00   98.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101  -45.0000  150.0000 66

  9 omega   28.00  140.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101  -77.0000  -60.0000 112

 10 omega   32.00   98.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101  -45.0000    0.0000 66

 11 omega -114.00  -10.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263  -57.0000  -30.0000 104

 12 omega -114.00  -10.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263  -57.0000 -120.0000 104

 13 omega  -70.00   34.00   1.0000   20.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9263   57.0000  -60.0000 104

 14 omega   79.00  106.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5101   45.0000  -90.0000 27
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.1052392000
_diffrn_orient_matrix_UB_12      -0.0179584000
_diffrn_orient_matrix_UB_13      -0.0389048000
_diffrn_orient_matrix_UB_21      0.0830582000
_diffrn_orient_matrix_UB_22      -0.0255168000
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_diffrn_orient_matrix_UB_31      -0.0544830000
_diffrn_orient_matrix_UB_32      -0.0736698000
_diffrn_orient_matrix_UB_33      -0.0186659000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.890
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
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_exptl_crystal_size_min          0.1042
_refine_diff_density_max         1.902
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0948P)^2^+8.4846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
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_reflns_number_gt                5761
_reflns_number_total             6306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04909e2.cif
_cod_data_source_block           exp_1136_186_cl2c_sbf3tmeda_tol
_cod_depositor_comments
'Adding full bibliography for 7042042--7042045.cif.'
_cod_database_code               7042042
_chemical_oxdiff_formula         'C27 H46 Cl2 N2 Sb F3'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
Uanis(C30) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) =
Uanis(C36)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              21840
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_olex2_date_sample_data_collection 2016-09-26
_olex2_submission_special_instructions 'No special instructions were received'