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_7131926
_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_absolute_configuration unk
_chemical_formula_moiety         'C9 H10 B F3 N3 P'
_chemical_formula_sum            'C9 H10 B F3 N3 P'
_chemical_formula_weight         258.993
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_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                 99.5596(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.80174(8)
_cell_length_b                   8.60271(12)
_cell_length_c                   11.79661(16)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    168.00
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.94
_cell_volume                     580.601(14)
_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)'
_diffrn_ambient_temperature      168.00
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.9947
_diffrn_reflns_Laue_measured_fraction_max 0.9953
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14658
_diffrn_reflns_point_group_measured_fraction_full 0.9943
_diffrn_reflns_point_group_measured_fraction_max 0.9950
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8598
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1231 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.9127.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       rod
_exptl_crystal_F_000             264.421
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.5100
_refine_diff_density_min         -0.3190
_refine_diff_density_rms         0.1158
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.00(2)
_refine_ls_d_res_high            0.7997
_refine_ls_d_res_low             6.9168
_refine_ls_goodness_of_fit_ref   1.1590
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2376
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.1590
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.995
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                2354
_reflns_number_total             2376
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc03268j2.cif
_cod_data_source_block           LD023
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7131926
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
1.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c)
;
_olex2_submission_special_instructions 'No special instructions were received'