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_7131929
_publ_section_title
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 Phosphorus Derivatives of Mesoionic Carbenes: Synthesis and
 Characterization of Triazaphosphole-5-ylidene\\rightarrow BF3 Adducts
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03268J
_journal_year                    2023
_chemical_formula_moiety         'C9 H11 N3 P, B F4'
_chemical_formula_sum            'C9 H11 B F4 N3 P'
_chemical_formula_weight         278.999
_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                 111.9100(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.71411(7)
_cell_length_b                   8.96879(6)
_cell_length_c                   13.55016(9)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      3.52
_cell_volume                     1208.023(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.00
_diffrn_measured_fraction_theta_full 0.9835
_diffrn_measured_fraction_theta_max 0.9824
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.9835
_diffrn_reflns_Laue_measured_fraction_max 0.9824
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18430
_diffrn_reflns_point_group_measured_fraction_full 0.9835
_diffrn_reflns_point_group_measured_fraction_max 0.9824
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         68.28
_diffrn_reflns_theta_min         4.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.400
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1569 before and 0.1064 after correction.
The Ratio of minimum to maximum transmission is 0.6156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       rod
_exptl_crystal_F_000             571.568
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.2943
_refine_diff_density_min         -0.3051
_refine_diff_density_rms         0.0535
_refine_ls_d_res_high            0.8298
_refine_ls_d_res_low             9.9402
_refine_ls_goodness_of_fit_ref   1.0617
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    19
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0617
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.7898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2081
_reflns_number_total             2174
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc03268j2.cif
_cod_data_source_block           LB1050
_cod_database_code               7131929
_audit_contact_author
;
      Prof. Dr.Christian M\"uller
      Freie Universit\"at Berlin
      Institut f\"ur Chemie und Biochemie
      Anorganische Chemie      
      Fabeckstr. 34-36
      14195 Berlin
      Germany
;
_audit_contact_letter
;

;
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b)
1.b Aromatic/amide H refined with riding coordinates:
 C1(H1), 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'