Crystal structure of (2-p-tolylpyrimidine-κ2 C,N)(triphenylphosphane-κ P) palladium(II), C29H24ClN2PPd
Liu, Hui; Lou, Xin-Hua; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 713–715; doi:10.1515/ncrs-2019-0913

data_8105265
_publ_section_title
;
 Crystal structure of (2-p-tolylpyrimidine-\k2 C,N)(triphenylphosphane-\k
 P) palladium(II), C29H24ClN2PPd
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              713
_journal_page_last               715
_journal_paper_doi               10.1515/ncrs-2019-0913
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C29 H24 Cl N2 P Pd'
_chemical_formula_sum            'C29 H24 Cl N2 P Pd'
_chemical_formula_weight         573.32
_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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                76.342(6)
_cell_angle_beta                 89.821(6)
_cell_angle_gamma                71.435(7)
_cell_formula_units_Z            2
_cell_length_a                   9.9885(8)
_cell_length_b                   11.5836(8)
_cell_length_c                   11.6133(9)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.0620
_cell_measurement_theta_min      4.1520
_cell_volume                     1233.96(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    2.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -150.0000 39

  2 omega  -14.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 41

  3 omega  -77.00  -52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -120.0000 25

  4 omega   35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 31

  5 omega  -68.00  -37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 31

  6 omega   27.00   58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -60.0000 31

  7 omega   30.00   58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000   30.0000 28

  8 omega   96.00  125.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -30.0000 29

  9 omega   18.00  110.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -180.0000 92

 10 omega   86.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -60.0000 29

 11 omega   71.00  125.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -90.0000 54

 12 omega   22.00   73.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -90.0000 51

 13 omega  -13.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -180.0000 77

 14 omega   31.00  113.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   30.0000 82

 15 omega   41.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 57

 16 omega   91.00  160.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 69

 17 omega   45.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  150.0000 29

 18 omega   76.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 40

 19 omega   58.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   30.0000 26

 20 omega   74.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000    0.0000 52

 21 omega   52.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -60.0000 55

 22 omega   40.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 48

 23 omega   89.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -150.0000 26

 24 omega   42.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 55

 25 omega   51.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 39

 26 omega  145.00  177.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -90.0000 32

 27 omega   89.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -90.0000 30

 28 omega   41.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -90.0000 55

 29 omega   41.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 37

 30 omega   52.00   99.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 47

 31 omega   40.00  156.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000 -120.0000 116

 32 omega  -70.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000   30.0000 100

 33 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 90

 34 omega  -77.00  -32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 45

 35 omega   26.00  126.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   90.0000 100

 36 omega   26.00  126.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -180.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0933471000
_diffrn_orient_matrix_UB_12      0.0182824000
_diffrn_orient_matrix_UB_13      -0.1125058000
_diffrn_orient_matrix_UB_21      -0.1037762000
_diffrn_orient_matrix_UB_22      0.1210082000
_diffrn_orient_matrix_UB_23      0.0239347000
_diffrn_orient_matrix_UB_31      0.0846355000
_diffrn_orient_matrix_UB_32      0.0774277000
_diffrn_orient_matrix_UB_33      -0.0741446000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8906
_diffrn_reflns_theta_full        67.11
_diffrn_reflns_theta_max         67.11
_diffrn_reflns_theta_min         3.93
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00103(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.3457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                3959
_reflns_number_total             4400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2019-0913_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        1233.96(16)
_cod_database_code               8105265
_chemical_oxdiff_formula         C20H20N4O4Cl1Pd1
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C25(H25), C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'