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_7713088
_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 -, C18 H38 B N3 P +'
_chemical_formula_sum            'C34 H38 Al B F36 N3 O4 P'
_chemical_formula_weight         1305.43
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 113.9820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6108(4)
_cell_length_b                   14.3902(4)
_cell_length_c                   20.5231(4)
_cell_measurement_reflns_used    3147
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.37
_cell_measurement_theta_min      2.44
_cell_volume                     5021.9(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49002
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.382
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         9860
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0979
_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^)+(0.1381P)^2^+18.8270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8240
_reflns_number_total             9860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01433a2.cif
_cod_data_source_block           5
_cod_database_code               7713088
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.914
_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
 C32-F28 \\sim C32-F29 \\sim C32-F30
 with sigma of 0.02
 C30-F25 \\sim C30-F26 \\sim C30-F27
 with sigma of 0.02
 C31A-F31A \\sim C31A-F32A \\sim C31A-F33A \\sim C33-F31 \\sim C33-F32 \\sim
C33-F33
 with sigma of 0.02
 C34-F34 \\sim C34-F35 \\sim C34-F36 \\sim C32A-F34A \\sim C32A-F35A \\sim
C32A-F36A
 with sigma of 0.02
 C21A-C22A \\sim C21A-C23A \\sim C21A-C24A \\sim C23-C24 \\sim C23-C25 \\sim
C23-C26
 with sigma of 0.02
 C31-C32 \\sim C31-C33 \\sim C31-C34 \\sim C29A-C30A \\sim C29A-C31A \\sim
C29A-C32A
 with sigma of 0.02
 C27-C28 \\sim C27-C29 \\sim C27-C30 \\sim C25A-C26A \\sim C25A-C27A \\sim
C25A-C28A
 with sigma of 0.02
 C26-F16 \\sim C26-F17 \\sim C26-F18 \\sim C24A-F16A \\sim C24A-F17A \\sim
C24A-F18A
 with sigma of 0.02
 C28-F19 \\sim C28-F20 \\sim C28-F21 \\sim C26A-F19A \\sim C26A-F20A \\sim
C26A-F21A
 with sigma of 0.02
 O1-C19 \\sim O2-C23 \\sim O2A-C21A
 with sigma of 0.02
3. Others
 Sof(F28A)=Sof(F29A)=Sof(F30A)=Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=
 Sof(F35A)=Sof(F36A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(C32A)=1-FVAR(1)
 Sof(F28)=Sof(F29)=Sof(F30)=Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=
 Sof(F36)=Sof(C31)=Sof(C32)=Sof(C33)=Sof(C34)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=
 Sof(F17A)=Sof(F18A)=Sof(O2A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=
 Sof(F18)=Sof(O2)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(C26)=FVAR(2)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(F25A)=
 Sof(F26A)=Sof(F27A)=Sof(O3A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=Sof(C28A)=1-FVAR(3)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(F25)=Sof(F26)=
 Sof(F27)=Sof(O3)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8)
4.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),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              31930
_olex2_submission_special_instructions 'No special instructions were received'