Isolable Fluorinated Triphenymethyl Cation Salts of [HCB11Cl11]-: Demonstration of Remarkable Hydride Affinity
Gunther, S. Olivia; Lee, Chun-I; Song, Ellen; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Chemical Science  (2022) –; doi:10.1039/D1SC05936J

data_1566740
_publ_section_title
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 Isolable Fluorinated Triphenymethyl Cation Salts of [HCB11Cl11]-:
 Demonstration of Remarkable Hydride Affinity
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05936J
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C H B11 Cl11, C19 H9 F6'
_chemical_formula_sum            'C20 H10 B11 Cl11 F6'
_chemical_formula_weight         873.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
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_audit_update_record
;
2021-04-23 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   21.8423(11)
_cell_length_b                   11.6968(6)
_cell_length_c                   19.7476(10)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      30.459
_cell_measurement_theta_min      2.171
_cell_volume                     4988.8(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker QUEST PHOTON-III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            186799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.886
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0972 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8842.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 6446 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(9)
_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     673
_refine_ls_number_reflns         15290
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+1.2258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14149
_reflns_number_total             15290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05936j3.cif
_cod_data_source_block           sog556
_cod_database_code               1566740
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H11 of C11, H3 of C3, H7 of C7, H15 of C15, H17 of C17, H13 of C13, H19 of
  C19, H1C of C1C, H5 of C5, H9 of C9, H28 of C28, H24 of C24, H26 of C26, H30
  of C30, H22 of C22
 At 1.5 times of:
  H6B of C6B
2. Shared sites
{B6B, C6B}
3. Restrained distances
 Cl5C-B5B \\sim Cl5B-B5B \\sim Cl4C-B4B \\sim Cl4B-B4B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Cl4B \\sim Cl5B \\sim B4B \\sim B5B \\sim Cl5C \\sim Cl4C: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(B6B) = Uanis(C6B)
5. Rigid body (RIGU) restrains
 Cl4B, Cl5B, B4B, B5B, Cl5C, Cl4C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: Cl4B(0.5) Cl5B(0.5) Cl6B(0.5) B6B(0.5) C6B(0.5) H6B(0.5) Cl5C(0.5)
 Cl4C(0.5)
7.a Riding coordinates:
 C6B(H6B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C13(H13), C15(H15), C17(H17),
 C19(H19), C22(H22), C24(H24), C26(H26), C28(H28), C30(H30)
7.c Boron cage BH refined with riding coordinates:
 C1C(H1C)
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_shelx_res_checksum              49670
_shelx_hkl_checksum              99575
_olex2_submission_special_instructions 'No special instructions were received'