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_7717712
_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         'C30 H28 Cl2 N3 P Ru, C H2 Cl2'
_chemical_formula_sum            'C31 H30 Cl4 N3 P Ru'
_chemical_formula_weight         718.42
_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                88.026(6)
_cell_angle_beta                 82.589(6)
_cell_angle_gamma                77.993(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3109(7)
_cell_length_b                   10.3812(8)
_cell_length_c                   16.2248(10)
_cell_measurement_reflns_used    6907
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.4360
_cell_measurement_theta_min      2.0440
_cell_volume                     1521.09(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -349.73  10.27   0.50    3.00   9.41 -12.98 -31.50    --   720
  2  \w    -68.96   0.04   0.50    3.00    --  -19.47  94.56 -34.84  138
  3  \w    -65.46   0.04   0.50    3.00    --  -15.96  94.56 145.16  131
  4  \w   -108.63  15.87   0.50    3.00    --  -12.98 -59.25 173.08  249
  5  \f    -10.27 349.73   0.50    3.00  77.88 -12.98  31.50    --   720
  6  \w    -65.46   0.04   0.50    3.00    --  -15.96  94.56  73.16  131
  7  \w    -26.98   0.02   0.50    3.00    --   -6.49  94.56 -34.84   54
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58324
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.810
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39755
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.155
_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     391
_refine_ls_number_reflns         11099
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0623P)^2^+1.4623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7191
_reflns_number_total             11099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03213f2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
'Adding full bibliography for 7717710--7717712.cif.'
_cod_database_code               7717712
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.878
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl3A) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31A) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: Cl4(0.75) Cl3(0.75) C31(0.75) H31a(0.75) H31b(0.75) Cl4A(0.25)
 C31A(0.25) H31c(0.25) H31d(0.25) Cl3A(0.25)
4.a Ternary CH refined with riding coordinates:
 C28(H28)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b), C31A(H31c,H31d)
4.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C20(H20), C14(H14), C22(H22), C19(H19), C7(H7), C10(H10), C16(H16),
 C25(H25), C26(H26), C6(H6), C12(H12), C4(H4), C13(H13), C11(H11), C5(H5),
 C17(H17), C18(H18)
4.d Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c)
;
_shelx_res_checksum              80721
_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
;