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_7713087
_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 H37 B N2 O P +'
_chemical_formula_sum            'C37 H37 Al B F36 N2 O5 P'
_chemical_formula_weight         1342.44
_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             2023-02-02
_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                 118.9290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0561(3)
_cell_length_b                   40.9364(7)
_cell_length_c                   17.3489(3)
_cell_measurement_reflns_used    89710
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.33
_cell_volume                     10601.8(3)
_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 0.984
_diffrn_measured_fraction_theta_max 0.986
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54894
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             5360
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1788
_refine_ls_number_reflns         21431
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0524P)^2^+29.8971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16051
_reflns_number_total             21431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01433a2.cif
_cod_data_source_block           3
_cod_database_code               7713087
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.945
_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
 C66A-F52A = C66A-F53A = C66A-F54A
 1.332 with sigma of 0.02
 C44-F1 \\sim C44-F2 \\sim C44-F3
 with sigma of 0.02
 C44A-F1A \\sim C44A-F2A \\sim C44A-F3A
 with sigma of 0.02
 C45-F4 \\sim C45-F5 \\sim C45-F6
 with sigma of 0.02
 C45A-F4A \\sim C45A-F5A \\sim C45A-F6A
 with sigma of 0.02
 C63-C64 \\sim C63-C65 \\sim C63-C66 \\sim C63A-C64A \\sim C63A-C65A \\sim
C63A-C66A
 with sigma of 0.02
 C71-C72 \\sim C71-C73 \\sim C71-C74 \\sim C71A-C72A \\sim C71A-C73A \\sim
C71A-C74A
 with sigma of 0.02
 O10-C71 \\sim O10A-C71A
 with sigma of 0.02
 F52A-F53A \\sim F53A-F54A \\sim F54A-F52A
 with sigma of 0.02
 F64A-F65A \\sim F65A-F66A \\sim F66A-F64A \\sim F67A-F68A \\sim F68A-F69A
\\sim F69A-F67A
 with sigma of 0.02
 C73-F67 \\sim C73-F68 \\sim C73-F69
 with sigma of 0.02
 C60A-F37A \\sim C60A-F38A \\sim C60A-F39A
 with sigma of 0.02
 C61A-F40A \\sim C61A-F41A \\sim C61A-F42A
 with sigma of 0.02
 C62A-F43A \\sim C62A-F44A \\sim C62A-F45A
 with sigma of 0.02
 C68A-F55A \\sim C68A-F56A \\sim C68A-F57A
 with sigma of 0.02
 C69A-F58A \\sim C69A-F59A \\sim C69A-F60A
 with sigma of 0.02
 C70A-F61A \\sim C70A-F62A \\sim C70A-F63A
 with sigma of 0.02
 C67A-C68A \\sim C67A-C69A \\sim C67A-C70A
 with sigma of 0.02
3. Others
 Sof(F46A)=Sof(F47A)=Sof(F48A)=Sof(F49A)=Sof(F50A)=Sof(F51A)=Sof(F52A)=
 Sof(F53A)=Sof(F54A)=Sof(C63A)=Sof(C64A)=Sof(C65A)=Sof(C66A)=1-FVAR(1)
 Sof(F46)=Sof(F47)=Sof(F48)=Sof(F49)=Sof(F50)=Sof(F51)=Sof(F52)=Sof(F53)=
 Sof(F54)=Sof(C63)=Sof(C64)=Sof(C65)=Sof(C66)=FVAR(1)
 Sof(F64A)=Sof(F65A)=Sof(F66A)=Sof(F67A)=Sof(F68A)=Sof(F69A)=Sof(F70A)=
 Sof(F71A)=Sof(F72A)=Sof(O10A)=Sof(C71A)=Sof(C72A)=Sof(C73A)=Sof(C74A)=1-FVAR(2)
 Sof(F64)=Sof(F65)=Sof(F66)=Sof(F67)=Sof(F68)=Sof(F69)=Sof(F70)=Sof(F71)=
 Sof(F72)=Sof(O10)=Sof(C71)=Sof(C72)=Sof(C73)=Sof(C74)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=
 Sof(F9A)=Sof(C44A)=Sof(C45A)=Sof(C46A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(C44)=Sof(C45)=Sof(C46)=FVAR(3)
 Sof(F37A)=Sof(F38A)=Sof(F39A)=Sof(F40A)=Sof(F41A)=Sof(F42A)=Sof(F43A)=
 Sof(F44A)=Sof(F45A)=Sof(O7A)=Sof(C59A)=Sof(C60A)=Sof(C61A)=Sof(C62A)=1-FVAR(4)
 Sof(F37)=Sof(F38)=Sof(F39)=Sof(F40)=Sof(F41)=Sof(F42)=Sof(F43)=Sof(F44)=
 Sof(F45)=Sof(O7)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=FVAR(4)
 Sof(O9A)=Sof(C67A)=Sof(C68A)=Sof(C70A)=Sof(C69A)=Sof(F55A)=Sof(F56A)=
 Sof(F57A)=Sof(F58A)=Sof(F59A)=Sof(F60A)=Sof(F63A)=Sof(F61A)=Sof(F62A)=1-FVAR(5)
 Sof(F55)=Sof(F56)=Sof(F57)=Sof(F58)=Sof(F59)=Sof(F60)=Sof(F61)=Sof(F62)=
 Sof(F63)=Sof(O9)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=FVAR(5)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C29(H29), C32(H32)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 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), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C)
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_shelx_res_checksum              18623
_olex2_submission_special_instructions 'No special instructions were received'