Triazolyl-phosphole and triazolyl-azaphosphole: synthesis, transition metal complexes and catalytic studies.
Radhakrishna, Latchupatula; Kote, Basvaraj S.; Gourkhede, Rani; Pandey, Ankit; Kaur, Bhupinder; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2599–2608; doi:10.1039/d4dt03213f

data_7717711
_publ_section_title
;
 Triazolyl-phosphole and triazolyl-azaphosphole: synthesis, transition
 metal complexes and catalytic studies.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2599
_journal_page_last               2608
_journal_paper_doi               10.1039/d4dt03213f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H14 N3 P'
_chemical_formula_sum            'C20 H14 N3 P'
_chemical_formula_weight         327.31
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-05
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                112.436(4)
_cell_angle_beta                 95.007(3)
_cell_angle_gamma                109.940(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1297(3)
_cell_length_b                   9.3832(4)
_cell_length_c                   11.0431(4)
_cell_measurement_reflns_used    10574
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.9420
_cell_measurement_theta_min      2.0420
_cell_volume                     795.84(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  25.00   0.50   12.00    --  -20.00   0.00-108.00  270
  2  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00-108.00  258
  3  \w    -69.00  19.00   0.50   12.00    --  -20.00 -72.00  36.00  176
  4  \w    -75.50 -12.00   0.50   12.00    --  -20.00 -72.00-180.00  127
  5  \w    -35.00  -5.00   0.50   12.00    --  -20.00 -72.00 -36.00   60
  6  \w   -110.00  70.00   0.50   12.00    --  -20.00   0.00 -36.00  360
  7  \w    -58.50  19.00   0.50   12.00    --  -20.00 -72.00 108.00  155
  8  \w    -59.00  22.00   0.50   12.00    --  -20.00  72.00 -36.00  162
  9  \w    -58.50   4.00   0.50   12.00    --  -20.00  72.00  36.00  125
 10  \w    -44.00 -13.00   0.50   12.00    --  -20.00  72.00-108.00   62
 11  \w    -59.00 -28.50   0.50   12.00    --  -20.00  72.00 108.00   61
 12  \w    -94.00  11.50   0.50   12.00    --  -20.00   0.00  36.00  211
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21476
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.128
_diffrn_reflns_theta_min         2.061
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74727
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.4008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3741
_reflns_number_total             4719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03213f2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 7717710--7717712.cif.'
_cod_original_cell_volume        795.83(6)
_cod_database_code               7717711
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C17(H17), C18(H18), C16(H16), C19(H19), C14(H14), C13(H13), C4(H4),
 C7(H7), C5(H5), C10(H10), C6(H6), C12(H12), C11(H11)
;
_shelx_res_checksum              69619
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;