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_7130521
_publ_section_title
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 Phosphinoborinium cation: a synthon for cationic B-P bond systems
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02933B
_journal_year                    2022
_chemical_formula_moiety         'C16 Al F36 O4, C40 H63 B2 N2 P2, C H Cl3'
_chemical_formula_sum            'C57 H64 Al B2 Cl3 F36 N2 O4 P2'
_chemical_formula_weight         1741.99
_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
_audit_creation_date             2022-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2022-03-30 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                89.963(2)
_cell_angle_beta                 74.734(2)
_cell_angle_gamma                73.552(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7391(3)
_cell_length_b                   15.3673(4)
_cell_length_c                   20.1094(5)
_cell_measurement_reflns_used    53953
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.26
_cell_volume                     3630.76(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.229
_diffrn_reflns_theta_min         2.262
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         19572
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0580P)^2^+0.8306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14862
_reflns_number_total             19572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02933b2.cif
_cod_data_source_block           B
_cod_original_cell_volume        3630.76(16)
_cod_database_code               7130521
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.933
_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
 C41-C42 \\sim C41-C43 \\sim C41-C44 \\sim C41A-C42A \\sim C41A-C43A \\sim
C41A-C44A
 with sigma of 0.02
 O1-C41 \\sim O1A-C41A
 with sigma of 0.02
 O4-C53 \\sim O4A-C53A
 with sigma of 0.02
 C57-Cl1 \\sim C57-Cl2 \\sim C57-Cl3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C56) = Uanis(C56A)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=
 Sof(F9A)=Sof(O1A)=Sof(C41A)=Sof(C42A)=Sof(C43A)=Sof(C44A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(O1)=Sof(C41)=Sof(C42)=Sof(C43)=Sof(C44)=FVAR(1)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=Sof(F35A)=Sof(F36A)=Sof(F37A)=
 Sof(F38A)=Sof(F39A)=Sof(O4A)=Sof(C53A)=Sof(C54A)=Sof(C55A)=Sof(C56A)=1-FVAR(2)
 Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=Sof(F37)=Sof(F38)=
 Sof(F39)=Sof(O4)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=FVAR(2)
 Sof(C49A)=Sof(C50A)=Sof(C51A)=Sof(C52A)=Sof(F19A)=Sof(F20A)=Sof(F21A)=
 Sof(F22A)=Sof(F24A)=Sof(F23A)=Sof(F25A)=Sof(F26A)=Sof(F27A)=1-FVAR(3)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(F25)=Sof(F26)=
 Sof(F27)=Sof(C49)=Sof(C50)=Sof(C51)=Sof(C52)=FVAR(3)
 Sof(C58A)=Sof(H58A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=1-FVAR(4)
 Sof(C57)=Sof(H57)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C57(H57), C7(H7), C13(H13), C29(H29), C35(H35), C58A(H58A)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
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_shelx_res_checksum              48486
_shelx_hkl_checksum              3028
_olex2_submission_special_instructions 'No special instructions were received'