Bond Dissociation Energies in the Gas Phase for Large Molecular Ions by Threshold Collision-Induced Dissociation Experiments: a Benchmarking Study.
Bot, Marek; Gorbachev, Vladimir M.; Tsybizova, Alexandra; Chen, Peter; The journal of physical chemistry. A  (2020) –; doi:10.1021/acs.jpca.0c05712

data_1559334
_publ_section_title
;
 Bond Dissociation Energies in the Gas Phase for Large Molecular Ions by
 Threshold Collision-Induced Dissociation Experiments: a Benchmarking
 Study.
;
_journal_name_full               'The journal of physical chemistry. A'
_journal_paper_doi               10.1021/acs.jpca.0c05712
_journal_year                    2020
_chemical_formula_moiety         'C32 H12 B F24, C23 H25.43 N, C23 H25.57 N'
_chemical_formula_sum            'C78 H63 B F24 N2'
_chemical_formula_weight         1495.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-16
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.89560(10)
_cell_length_b                   18.1458(2)
_cell_length_c                   19.42110(10)
_cell_measurement_reflns_used    34444
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      79.4660
_cell_measurement_theta_min      3.2940
_cell_volume                     7009.38(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -20.00  29.00   0.50    0.70    --   49.37 -38.00 -30.00   98
  2  \w    -25.00   3.00   0.50    0.70    --   49.37 -19.00-150.00   56
  3  \w     39.00  68.00   0.50    2.20    --  110.00 -57.00-180.00   58
  4  \w     63.00  89.00   0.50    2.20    --  110.00 -77.00-180.00   52
  5  \w    109.00 134.00   0.50    2.20    --  110.00 -77.00-180.00   50
  6  \w     71.00 103.00   0.50    2.20    --  110.00-125.00 -90.00   64
  7  \w     52.00 112.00   0.50    2.20    --  110.00-125.00 -30.00  120
  8  \w     47.00  98.00   0.50    2.20    --  110.00 -99.00  90.00  102
  9  \w     42.00  68.00   0.50    2.20    --  110.00 -57.00 150.00   52
 10  \w     38.00  65.00   0.50    2.20    --  110.00 -57.00 -30.00   54
 11  \w     41.00  68.00   0.50    2.20    --  110.00-125.00 -90.00   54
 12  \w    108.00 136.00   0.50    2.20    --  110.00  19.00-120.00   56
 13  \w    109.00 135.00   0.50    2.20    --  110.00  38.00-120.00   52
 14  \w    127.00 171.00   0.50    2.20    --  110.00  77.00-150.00   88
 15  \w    135.00 167.00   0.50    2.20    --  110.00  77.00 -90.00   64
 16  \w    142.00 176.00   0.50    2.20    --  110.00  57.00 -60.00   68
 17  \w    133.00 174.00   0.50    2.20    --  110.00  77.00-120.00   82
 18  \w    145.00 170.00   0.50    2.20    --  110.00  77.00 -60.00   50
 19  \w    104.00 140.00   0.50    2.20    --  110.00  38.00-180.00   72
 20  \w    134.00 172.00   0.50    2.20    --  110.00  77.00-180.00   76
 21  \w    103.00 128.00   0.50    2.20    --  110.00  38.00 -90.00   50
 22  \w     98.00 126.00   0.50    2.20    --  110.00  57.00 -60.00   56
 23  \w     98.00 135.00   0.50    2.20    --  110.00  57.00 -90.00   74
 24  \w     97.00 143.00   0.50    2.20    --  110.00  57.00-120.00   92
 25  \w     99.00 132.00   0.50    2.20    --  110.00  44.00 -58.90   66
 26  \w     89.00 114.00   0.50    2.20    --  110.00  77.00-120.00   50
 27  \w     99.00 125.00   0.50    2.20    --  110.00  57.00-150.00   52
 28  \w     96.00 142.00   0.50    2.20    --  110.00  57.00-180.00   92
 29  \w     87.00 113.00   0.50    2.20    --  110.00  77.00 -90.00   52
 30  \w     86.00 111.00   0.50    2.20    --  110.00  77.00-150.00   50
 31  \w     87.00 112.00   0.50    2.20    --  110.00  77.00-180.00   50
 32  \w     93.00 118.00   0.50    2.20    --  110.00  77.00 -60.00   50
 33  \w     93.00 162.00   0.50    2.20    --  110.00  60.00 -54.50  138
 34  \w    141.00 175.00   0.50    2.20    --  110.00  77.00 150.00   68
 35  \w     86.00 112.00   0.50    2.20    --  110.00  77.00 150.00   52
 36  \w     -6.00  24.00   0.50    0.70    --  -49.87  19.00   0.00   60
 37  \w    -23.00  14.00   0.50    0.70    --  -49.87  57.00-120.00   74
 38  \w    -38.00   5.00   0.50    2.20    --  -70.00  38.00-120.00   86
 39  \w    -62.00 -32.00   0.50    0.70    --  -49.87  57.00-120.00   60
 40  \w    -85.00 -37.00   0.50    0.70    --  -49.87 -19.00-150.00   96
 41  \w    -62.00 -35.00   0.50    0.70    --  -49.87 -57.00 -90.00   54
 42  \w    -59.00 -26.00   0.50    0.70    --  -49.87 -77.00-120.00   66
 43  \w    -65.00 -36.00   0.50    0.70    --  -49.87 -57.00-120.00   58
 44  \w    -73.00 -44.00   0.50    2.20    --  -70.00 -81.00-151.31   58
 45  \w    -73.00 -44.00   0.50    2.20    --  -70.00 -82.00-104.59   58
 46  \w    -84.00 -58.00   0.50    2.20    --  -70.00 -77.00-150.00   52
 47  \w    -75.00 -44.00   0.50    2.20    --  -70.00 -81.00-122.14   62
 48  \w    -85.00 -47.00   0.50    2.20    --  -70.00 -77.00-180.00   76
 49  \w    -82.00 -57.00   0.50    2.20    --  -70.00 -78.00 -95.76   50
 50  \w    -71.00 -46.00   0.50    2.20    --  -70.00 -77.00 -90.00   50
 51  \w   -108.00 -43.00   0.50    0.70    --  -49.87 -18.00-102.08  130
 52  \w   -121.00 -91.00   0.50    0.70    --  -49.87 -57.00-120.00   60
 53  \w   -114.00 -84.00   0.50    0.70    --  -49.87 -77.00-120.00   60
 54  \w   -122.00 -97.00   0.50    0.70    --  -49.87 -19.00-150.00   50
 55  \w   -133.00 -75.00   0.50    2.20    --  -70.00-125.00 150.00  116
 56  \w    -83.00 -46.00   0.50    2.20    --  -70.00 -77.00 150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0608333000
_diffrn_orient_matrix_UB_12      0.0130684000
_diffrn_orient_matrix_UB_13      0.0460224000
_diffrn_orient_matrix_UB_21      -0.0449134000
_diffrn_orient_matrix_UB_22      0.0131566000
_diffrn_orient_matrix_UB_23      -0.0645555000
_diffrn_orient_matrix_UB_31      -0.0167273000
_diffrn_orient_matrix_UB_32      -0.0828719000
_diffrn_orient_matrix_UB_33      -0.0029900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51067
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.779
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+4.8371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6824
_reflns_number_total             7495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp0c05712_si_002.cif
_cod_data_source_block           c150120_1_1
_cod_database_code               1559334
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C78H62BF24N2
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 99.85
_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) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1D-C7C \\sim F2C-C7C \\sim F1C-C7C \\sim F2D-C7C \\sim F3C-C7C \\sim F3D-C7C
 with sigma of 0.01
 F1D-F2D \\sim F2D-F3D \\sim F3D-F1D \\sim F1C-F2C \\sim F2C-F3C \\sim F3C-F1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3C \\sim F3C \\sim F1D \\sim F2D \\sim F3D \\sim C7C \\sim F1C \\sim F2C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F1D) \\sim Ueq, Uanis(F2D) \\sim Ueq, Uanis(F3D) \\sim Ueq, Uanis(C7C)
\\sim Ueq, Uanis(F1C) \\sim Ueq, Uanis(F2C) \\sim Ueq, Uanis(F3C) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C3C, F2D, F3D, C7C, F1C, F2C, F1D, F3C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1D)=Sof(F2D)=Sof(F3D)=1-FVAR(1)
 Sof(H1B)=0.5*(1-FVAR(2))
 Sof(H1A)=0.5*FVAR(2)
 Sof(F1C)=Sof(F2C)=Sof(F3C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C4B(H4BA,H4BB)
6.b Aromatic/amide H refined with riding coordinates:
 C2C(H2C), C4C(H4C), C6C(H6C), C10C(H10C), C12C(H12C), C14C(H14C), N1A(H1A),
 C1A(H1AA), C2A(H2A), C6A(H6A), C8A(H8A), C10A(H10A), N1B(H1B), C1B(H1BA),
 C2B(H2B), C6B(H6B), C8B(H8B), C10B(H10B)
6.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12D), C11B(H11D,H11E,H11F), C12B(H12E,
 H12F,H12G)
;
_shelx_res_checksum              72984
_shelx_hkl_checksum              76318
_olex2_date_sample_data_collection 2020-01-15
_olex2_date_sample_submission    2020-01-14
_olex2_submission_original_sample_id c150120_1_1
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.982
_oxdiff_exptl_absorpt_empirical_full_min 0.701