Application of nonmetallic frustrated cations in the activation of small molecules
Kaniewska-Laskowska, Kinga; Czapla, Marcin; Chojnacki, Jarosław; Grubba, Rafał; Dalton Transactions  (2023) –; doi:10.1039/D3DT01433A

data_7713089
_publ_section_title
;
 Application of nonmetallic frustrated cations in the activation of small
 molecules
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01433A
_journal_year                    2023
_chemical_formula_moiety         'C16 Al F36 O4 -,C21 H46 B N3 P +'
_chemical_formula_sum            'C37 H46 Al B F36 N3 O4 P'
_chemical_formula_weight         1349.53
_chemical_properties_physical    Air-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.263(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5987(11)
_cell_length_b                   16.314(3)
_cell_length_c                   32.120(3)
_cell_measurement_reflns_used    4488
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.05
_cell_volume                     5496.1(13)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.77.0.0 (STOE, 2019) X-Area X-Red32 1.65.0.0 (STOE, 2018)'
_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      120.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            45571
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         10771
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0516P)^2^+26.4022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8023
_reflns_number_total             10771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01433a2.cif
_cod_data_source_block           4
_cod_database_code               7713089
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.920
_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. Restrained distances
 C23-F1 \\sim C23-F2 \\sim C23-F3
 with sigma of 0.02
 C23A-F1A \\sim C23A-F2A \\sim C23A-F3A
 with sigma of 0.02
 C24-F4 \\sim C24-F5 \\sim C24-F6
 with sigma of 0.02
 C24A-F4A \\sim C24A-F5A \\sim C24A-F6A
 with sigma of 0.02
 C25-F7 \\sim C25-F8 \\sim C25-F9
 with sigma of 0.02
 C25A-F7A \\sim C25A-F8A \\sim C25A-F9A
 with sigma of 0.02
 C22-C23 \\sim C22-C23A \\sim C22-C24 \\sim C22-C24A \\sim C22-C25 \\sim
C22-C25A
 with sigma of 0.02
 C31-F19 \\sim C31-F20 \\sim C31-F21
 with sigma of 0.02
 C31A-F19A \\sim C31A-F20A \\sim C31A-F21A
 with sigma of 0.02
 C32-F22 \\sim C32-F23 \\sim C32-F24
 with sigma of 0.02
 C32A-F22A \\sim C32A-F23A \\sim C32A-F24A
 with sigma of 0.02
 C33-F25 \\sim C33-F26 \\sim C33-F27
 with sigma of 0.02
 C33A-F25A \\sim C33A-F26A \\sim C33A-F27A
 with sigma of 0.02
 C30-C31 \\sim C30-C31A \\sim C30-C32 \\sim C30-C33 \\sim C30-C32A \\sim
C30-C33A
 with sigma of 0.02
 C29-F17 \\sim C29-F18 \\sim C29-F16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F17 \\sim F18: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=
 Sof(F9A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(C23)=Sof(C24)=Sof(C25)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(F25A)=
 Sof(F26A)=Sof(F27A)=Sof(C31A)=Sof(C32A)=Sof(C33A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(F25)=Sof(F26)=
 Sof(F27)=Sof(C31)=Sof(C32)=Sof(C33)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C11(H11)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              53723
_olex2_submission_special_instructions 'No special instructions were received'