Catalytically active nanosized Pd9Te4 (telluropalladinite) and PdTe (kotulskite) alloys: first precursor-architecture controlled synthesis using palladium complexes of organotellurium compounds as single source precursors
Arora, Aayushi; Oswal, Preeti; Rao, Gyandshwar K.; Kumar, Sushil; Singh, Ajai K.; Kumar, Arun; RSC Advances 11 (2021) 7214–7224; doi:10.1039/D0RA08732G

data_7242266
_publ_section_title
;
 Catalytically active nanosized Pd9Te4 (telluropalladinite) and PdTe
 (kotulskite) alloys: first precursor-architecture controlled synthesis
 using palladium complexes of organotellurium compounds as single source
 precursors
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              7214
_journal_page_last               7224
_journal_paper_doi               10.1039/D0RA08732G
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         '4(C16 H16 Cl N O Pd Te)'
_chemical_formula_sum            'C16 H16 Cl N O Pd Te'
_chemical_formula_weight         507.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-03 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.7218(2)
_cell_length_b                   19.2440(3)
_cell_length_c                   20.2510(3)
_cell_measurement_reflns_used    11703
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0940
_cell_measurement_theta_min      2.0240
_cell_volume                     6424.28(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9896
_diffrn_measured_fraction_theta_max 0.8722
_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    -20.00  56.00   1.00   14.06    --   26.84 -99.00-120.00   76
  2  \w     -5.00  92.00   1.00   14.06    --   26.84  57.00  30.00   97
  3  \w    -20.00  28.00   1.00   14.06    --   26.84 -99.00-180.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038691000
_diffrn_orient_matrix_UB_12      0.0283248000
_diffrn_orient_matrix_UB_13      -0.0227497000
_diffrn_orient_matrix_UB_21      0.0180031000
_diffrn_orient_matrix_UB_22      -0.0202357000
_diffrn_orient_matrix_UB_23      -0.0228404000
_diffrn_orient_matrix_UB_31      -0.0388942000
_diffrn_orient_matrix_UB_32      -0.0121623000
_diffrn_orient_matrix_UB_33      -0.0148816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21641
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.0999
_exptl_crystal_description       Orange
_exptl_crystal_F_000             3872
_refine_diff_density_max         2.1093
_refine_diff_density_min         -0.9230
_refine_diff_density_rms         0.1935
_refine_ls_d_res_high            0.7493
_refine_ls_d_res_low             11.7781
_refine_ls_goodness_of_fit_ref   1.0431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    112
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0431
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0057
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+4.7752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -15
_reflns_number_gt                11578
_reflns_number_total             15978
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra08732g2.cif
_cod_data_source_block           Pd_HA_Lt_Mo
_cod_original_sg_symbol_Hall     '-P 2yn (x-z,y,z)'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7242266
_chemical_oxdiff_formula         'c h n o'
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C55(H55a,H55b), C2(H2a,H2b), C3(H3a,H3b), C65(H65a,H65b), C33(H33a,H33b),
 C66(H66a,H66b), C34(H34a,H34b), C54(H54a,H54b)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C47(H47), C27(H27), C82(H82), C50(H50), C48(H48), C10(H10),
 C29(H29), C36(H36), C40(H40), C73(H73), C78(H78), C7(H7), C49(H49), C8(H8),
 C57(H57), C28(H28), C81(H81), C9(H9), C61(H61), C80(H80), C60(H60), C19(H19),
 C39(H39), C15(H15), C79(H79), C70(H70), C37(H37), C59(H59), C72(H72), C18(H18),
  C71(H71), C38(H38), C17(H17), C58(H58), C16(H16)
2.c Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C63(H63a,H63b,H63c), C84(H84a,H84b,H84c), C42(H42a,H42b,
 H42c)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.907