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_7709674
_publ_section_title
;
 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, 1[CHCl3]'
_chemical_formula_sum            'C38 H30 Cl4 N4 P2 Pd'
_chemical_formula_weight         852.80
_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             2021-09-23
_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                 100.667(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9552(3)
_cell_length_b                   19.8167(5)
_cell_length_c                   17.0756(6)
_cell_measurement_reflns_used    11731
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.8020
_cell_measurement_theta_min      2.1570
_cell_volume                     3642.98(19)
_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      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.904
_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  19.00   0.50    8.00    --  -20.00 -72.00 108.00  258
  2  \w    -92.50  19.00   0.50    8.00    --  -20.00 -72.00 -36.00  223
  3  \w    -34.50  70.00   0.50    8.00    --  -20.00   0.00-108.00  209
  4  \w    -34.50 -13.50   0.50    8.00    --  -20.00 -72.00-180.00   42
;
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33975
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.242
_diffrn_reflns_theta_min         2.153
_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    0.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66095
_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    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.089
_refine_diff_density_max         2.546
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         10695
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0713P)^2^+5.8234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7416
_reflns_number_total             10695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00112h2.cif
_cod_data_source_block           compound-13
_cod_original_cell_volume        3643.0(2)
_cod_database_code               7709674
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl3-C38 \\sim Cl3A-C38
 with sigma of 0.02
 C8-C13 \\sim C8-C13A
 with sigma of 0.02
 C11-C12 \\sim C11-C12A
 with sigma of 0.02
 C13-C12 \\sim C13A-C12A
 with sigma of 0.02
 C8-C12 \\sim C8-C12A
 with sigma of 0.04
 C11-C13 \\sim C11-C13A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 Cl3, Cl3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H38C)=Sof(H38D)=Sof(Cl3A)=1-FVAR(1)
 Sof(Cl3)=Sof(H38B)=Sof(H38A)=FVAR(1)
 Sof(H11A)=Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(H12A)=1-FVAR(2)
 Sof(H11)=Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38B,H38A), C38(H38C,H38D)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C15(H15), C37(H37), C22(H22), C31(H31), C24(H24),
 C19(H19), C33(H33), C27(H27), C5(H5), C16(H16), C23(H23), C17(H17), C4(H4),
 C30(H30), C36(H36), C18(H18), C29(H29), C34(H34), C35(H35), C3(H3), C28(H28),
 C9(H9), C10(H10), C11(H11), C11(H11A), C13(H13), C12(H12), C13A(H13A),
 C12A(H12A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94767
_shelx_hkl_checksum              32909
_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
;