1,2,3-Triazole based ligands with phosphine and pyridine functionalities: Synthesis, PdII, PtII chemistry and catalytic studies
Radhakrishna, Latchupatula; Kote, Basvaraj S.; Kunchur, Harish S.; Pandey, Madhusudan Kumar; Mondal, Dipanjan; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2022) –; doi:10.1039/D2DT00112H

data_7709671
_publ_section_title
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 1,2,3-Triazole based ligands with phosphine and pyridine functionalities:
 Synthesis, PdII, PtII chemistry and catalytic studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00112H
_journal_year                    2022
_chemical_formula_moiety         'C37 H28 Cl2 N4 P2 Pd, C H Cl3'
_chemical_formula_sum            'C38 H29 Cl5 N4 P2 Pd'
_chemical_formula_weight         887.24
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-09-26 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.185(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0885(5)
_cell_length_b                   19.5981(10)
_cell_length_c                   17.1297(8)
_cell_measurement_reflns_used    6944
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.9650
_cell_measurement_theta_min      2.7730
_cell_volume                     3663.9(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.861
_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  66.50   0.50   16.00    --  -20.00   0.00-108.00  353
;
_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_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17053
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.124
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85067
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.806
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.5965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7027
_reflns_number_total             10159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00112h2.cif
_cod_data_source_block           compound-11
_cod_database_code               7709671
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C38 \\sim Cl3A-C38
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl3A, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H19, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H38A)=Sof(Cl3A)=1-FVAR(1)
 Sof(Cl3)=Sof(H38)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C38(H38), C38(H38A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C25(H25), C4(H4), C23(H23), C21(H21), C37(H37),
 C24(H24), C15(H15), C31(H31), C11(H11), C36(H36), C13(H13), C22(H22), C10(H10),
  C19(H19), C33(H33), C12(H12), C16(H16), C28(H28), C27(H27), C30(H30),
 C35(H35), C34(H34), C17(H17), C29(H29), C18(H18)
;
_shelx_res_checksum              90039
_shelx_hkl_checksum              35483
_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
;