Phosphinoborinium cation: a synthon for cationic B-P bond systems
Kaniewska-Laskowska, Kinga; Klimsiak, Katarzyna; Szynkiewicz, Natalia; Chojnacki, Jarosław; Grubba, Rafał; Chemical Communications  (2022) –; doi:10.1039/D2CC02933B

data_7130520
_publ_section_title
;
 Phosphinoborinium cation: a synthon for cationic B-P bond systems
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02933B
_journal_year                    2022
_chemical_formula_moiety
'C16 Al F36 O4, 0.5(C44 H72 B2 N2 P2), 2(C H2 Cl2)'
_chemical_formula_sum            'C40 H40 Al B Cl4 F36 N O4 P'
_chemical_formula_weight         1493.29
_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             2022-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.268(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6428(8)
_cell_length_b                   15.3495(10)
_cell_length_c                   25.7474(14)
_cell_measurement_reflns_used    15011
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.00
_cell_volume                     5582.7(6)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.72.0.0 (STOE, 2018) X-Area X-Red32 1.63.4.0 (STOE, 2017)'
_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 0.999
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34189
_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         25.999
_diffrn_reflns_theta_min         2.299
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.680
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1626P)^2^+19.7087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2461
_refine_ls_wR_factor_ref         0.2717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8075
_reflns_number_total             10939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02933b2.cif
_cod_data_source_block           A
_cod_database_code               7130520
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-F2 \\sim F2-F3 \\sim F3-F1
 with sigma of 0.02
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.02
 F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.02
 C26A-F7A \\sim C26A-F8A \\sim C26A-F9A
 with sigma of 0.02
 C25A-F4A \\sim C25A-F5A \\sim C25A-F6A
 with sigma of 0.02
 C24A-F1A \\sim C24A-F2A \\sim C24A-F3A
 with sigma of 0.02
3. Others
 Sof(F9A)=Sof(C26A)=Sof(F7A)=Sof(F8A)=Sof(C25A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=
 Sof(C24A)=Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(C24)=Sof(C25)=Sof(C26)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C17(H17)
4.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              14030
_shelx_hkl_checksum              97132
_olex2_submission_special_instructions 'No special instructions were received'