Phosphorus Derivatives of Mesoionic Carbenes: Synthesis and Characterization of Triazaphosphole-5-ylidene→ BF3 Adducts
Dettling, Lea; Limberg, Niklas; Küppers, Raphaela; Frost, Daniel Sebastian; Weber, Manuela; Coles, Nathan Thomas; Andrada, Diego M.; Muller, Christian; Chemical Communications  (2023) –; doi:10.1039/D3CC03268J

data_7131930
_publ_section_title
;
 Phosphorus Derivatives of Mesoionic Carbenes: Synthesis and
 Characterization of Triazaphosphole-5-ylidene\\rightarrow BF3 Adducts
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03268J
_journal_year                    2023
_chemical_formula_moiety         'C21 H37 B N3 P'
_chemical_formula_sum            'C21 H37 B N3 P'
_chemical_formula_weight         373.346
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-06 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7284(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.06027(9)
_cell_length_b                   23.24206(15)
_cell_length_c                   14.36186(9)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    102.60
_cell_measurement_theta_max      74.56
_cell_measurement_theta_min      3.22
_cell_volume                     4577.97(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      102.60
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            78829
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9975
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         74.66
_diffrn_reflns_theta_min         3.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  0.8406
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1199 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8440.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       plate
_exptl_crystal_F_000             1638.560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.3528
_refine_diff_density_min         -0.2408
_refine_diff_density_rms         0.0381
_refine_ls_d_res_high            0.7994
_refine_ls_d_res_low             13.7147
_refine_ls_goodness_of_fit_ref   1.0328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    108
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0328
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+1.4546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                8729
_reflns_number_total             9356
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc03268j2.cif
_cod_data_source_block           NL1078
_cod_database_code               7131930
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C8B(H8B), C11B(H11B)
1.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C16(H16a,H16b), C18(H18a,H18b), C20(H20a,H20b), C14B(H14c,
 H14d), C16B(H16c,H16d), C18B(H18c,H18d), C20B(H20c,H20d)
1.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C4B(H4B), C5B(H5B), C6B(H6B)
1.d 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), C17(H17a,H17b,H17c), C19(H19a,H19b,H19c), C21(H21a,
 H21b,H21c), C9B(H9Ba,H9Bb,H9Bc), C10B(H10d,H10e,H10f), C12B(H12d,H12e,H12f),
 C13B(H13d,H13e,H13f), C15B(H15d,H15e,H15f), C17B(H17d,H17e,H17f), C19B(H19d,
 H19e,H19f), C21B(H21d,H21e,H21f)
;
_olex2_submission_special_instructions 'No special instructions were received'