Palladium pincer-type complexes and zwitterionic sulfur adducts of pyridine-bridged bis(1,2,3-triazolin-5-ylidenes): syntheses, characterizations and catalytic applications.
Wang, Haiying; Zhang, Bo; Yan, Xuechao; Guo, Shuai; Dalton transactions (Cambridge, England : 2003) 47 (2018) 528–537; doi:10.1039/c7dt03687f

data_7045048
_publ_section_title
;
 Palladium pincer-type complexes and zwitterionic sulfur adducts of
 pyridine-bridged bis(1,2,3-triazolin-5-ylidenes): syntheses,
 characterizations and catalytic applications.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              528
_journal_page_last               537
_journal_paper_doi               10.1039/c7dt03687f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'B F4, C25 H23 Cl N7 Pd'
_chemical_formula_sum            'C25 H23 B Cl F4 N7 Pd'
_chemical_formula_weight         650.16
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-14 deposited with the CCDC.
2017-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.715(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8856(10)
_cell_length_b                   5.7367(3)
_cell_length_c                   25.7084(15)
_cell_measurement_reflns_used    4478
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      72.9790
_cell_measurement_theta_min      4.6800
_cell_volume                     2582.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    -12.00  63.00   1.00    1.00    --   39.74 -37.00  30.00   75
  2  \w     26.00 109.00   1.00    3.00    --  108.77 -94.00  30.00   83
  3  \w     75.00 123.00   1.00    3.00    --  108.77 -45.00  30.00   48
  4  \w     85.00 177.00   1.00    3.00    --  108.77  30.00  60.00   92
  5  \w    125.00 178.00   1.00    3.00    --  108.77  45.00  90.00   53
  6  \w     96.00 172.00   1.00    3.00    --  108.77 125.00 -60.00   76
  7  \w     85.00 174.00   1.00    3.00    --  108.77  45.00   0.00   89
  8  \w     96.00 130.00   1.00    3.00    --  108.77 -61.00-150.00   34
  9  \w     93.00 120.00   1.00    3.00    --  108.77 -77.00 -90.00   27
 10  \w     76.00 109.00   1.00    3.00    --  108.77 -94.00 -90.00   33
 11  \w     60.00  98.00   1.00    3.00    --  108.77 -94.00-120.00   38
 12  \w     42.00  69.00   1.00    3.00    --  108.77 -61.00-150.00   27
 13  \w     30.00  55.00   1.00    3.00    --  108.77 -94.00-120.00   25
 14  \w     33.00  65.00   1.00    3.00    --  108.77 -77.00 -90.00   32
 15  \w     38.00 122.00   1.00    3.00    --  108.77-125.00-180.00   84
 16  \w     46.00 104.00   1.00    3.00    --  108.77 -45.00   0.00   58
 17  \w     90.00 129.00   1.00    1.00    --   39.74 178.00 150.00   39
 18  \w    -68.00  18.00   1.00    1.00    --  -39.74  57.00 -30.00   86
 19  \w    -82.00 -15.00   1.00    1.00    --  -39.74 -37.00   0.00   67
 20  \w   -114.00  -9.00   1.00    1.00    --  -39.74 -77.00-180.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0266861000
_diffrn_orient_matrix_UB_12      -0.2158019000
_diffrn_orient_matrix_UB_13      0.0343808000
_diffrn_orient_matrix_UB_21      0.0533961000
_diffrn_orient_matrix_UB_22      0.1549147000
_diffrn_orient_matrix_UB_23      0.0403514000
_diffrn_orient_matrix_UB_31      -0.0646045000
_diffrn_orient_matrix_UB_32      0.0384598000
_diffrn_orient_matrix_UB_33      0.0306416000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15824
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.964
_diffrn_reflns_theta_min         3.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.208
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.1111
_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^)+(0.0832P)^2^+54.0405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2589
_refine_ls_wR_factor_ref         0.2683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4252
_reflns_number_total             5117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03687f2.cif
_cod_data_source_block           20170721c
_cod_depositor_comments          'Adding full bibliography for 7045048.cif.'
_cod_database_code               7045048
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c1h1n1o1Cl1Pd1
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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:
 C1(H1A,H1B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              62665
_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 2.991
_oxdiff_exptl_absorpt_empirical_full_min 0.474