Activation of small molecules by ambiphilic NHC-stabilized phosphinoborenium cation: formation of boreniums with B-O-C, B-O-B, and B-O-P structural motifs.
Wojnowski, Tomasz; Ordyszewska, Anna; Halenka, Hanna; Anusiewicz, Iwona; Chojnacki, Jarosław; Kaniewska-Laskowska, Kinga; Grubba, Rafał; Dalton transactions (Cambridge, England : 2003) 54 (2024) 290–297; doi:10.1039/d4dt02656j

data_7717447
_publ_section_title
;
 Activation of small molecules by ambiphilic NHC-stabilized
 phosphinoborenium cation: formation of boreniums with B-O-C, B-O-B, and
 B-O-P structural motifs.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              290
_journal_page_last               297
_journal_paper_doi               10.1039/d4dt02656j
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C16 Al F36 O4 -, C17 H26 B F9 N3 O +'
_chemical_formula_sum            'C33 H26 Al B F45 N3 O5'
_chemical_formula_weight         1437.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                75.250(17)
_cell_angle_beta                 81.060(17)
_cell_angle_gamma                84.851(15)
_cell_formula_units_Z            2
_cell_length_a                   10.7476(19)
_cell_length_b                   15.641(3)
_cell_length_c                   15.787(4)
_cell_measurement_reflns_used    7384
_cell_measurement_temperature    120
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.51
_cell_volume                     2531.7(9)
_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
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.363
_diffrn_reflns_theta_min         1.921
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         13620
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0257P)^2^+3.2582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8449
_reflns_number_total             13620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02656j2.cif
_cod_data_source_block           6_WCA
_cod_depositor_comments
'Adding full bibliography for 7717444--7717448.cif.'
_cod_original_cell_volume        2531.6(9)
_cod_database_code               7717447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.952
_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
 F30-C24 \\sim F31-C24 \\sim F32-C24
 with sigma of 0.02
 F30A-C24A \\sim F31A-C24A \\sim F32A-C24A
 with sigma of 0.02
 C24-C22 \\sim C24A-C22
 with sigma of 0.02
3. Others
 Sof(C25A)=Sof(F29A)=Sof(F28A)=Sof(F27A)=1-FVAR(1)
 Sof(F27)=Sof(F28)=Sof(F29)=Sof(C25)=FVAR(1)
 Sof(C23A)=Sof(F35A)=Sof(F33A)=Sof(F34A)=1-FVAR(2)
 Sof(F33)=Sof(F34)=Sof(F35)=Sof(C23)=FVAR(2)
 Sof(C24A)=Sof(F31A)=Sof(F32A)=Sof(F30A)=1-FVAR(3)
 Sof(F30)=Sof(F31)=Sof(F32)=Sof(C24)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              2294
_shelx_hkl_checksum              75973
_olex2_submission_special_instructions 'No special instructions were received'