Crystal structure of chlorido (2-(4-ethylphenyl)pyrimidine-k2 C,N)(triphenylphosphane-kP) palladium(II), C30H26ClN2PPd
Liu, Hui; Lou, Xin-Hua; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 659–661; doi:10.1515/ncrs-2019-0886

data_8105249
_publ_section_title
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 Crystal structure of chlorido (2-(4-ethylphenyl)pyrimidine-k2
 C,N)(triphenylphosphane-kP) palladium(II), C30H26ClN2PPd
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              659
_journal_page_last               661
_journal_paper_doi               10.1515/ncrs-2019-0886
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C30 H26 Cl N2 P Pd'
_chemical_formula_sum            'C30 H26 Cl N2 P Pd'
_chemical_formula_weight         587.35
_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                79.827(6)
_cell_angle_beta                 89.131(5)
_cell_angle_gamma                78.358(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1278(5)
_cell_length_b                   9.5892(7)
_cell_length_c                   15.5255(10)
_cell_measurement_reflns_used    3641
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.6240
_cell_measurement_theta_min      3.4610
_cell_volume                     1309.74(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -80.00  -39.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104    0.0000  -90.0000 41

  2 omega  -44.00    4.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104   19.0000    0.0000 48

  3 omega  -24.00    6.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000  120.0000 30

  4 omega  -16.00   10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104    0.0000  -90.0000 26

  5 omega  -35.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104   57.0000   90.0000 71

  6 omega  -25.00   60.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -99.0000 -120.0000 85

  7 omega   -7.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   77.0000    0.0000 97

  8 omega   -2.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   57.0000 -150.0000 47
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0172380000
_diffrn_orient_matrix_UB_12      0.0186628000
_diffrn_orient_matrix_UB_13      0.0417377000
_diffrn_orient_matrix_UB_21      -0.0067616000
_diffrn_orient_matrix_UB_22      -0.0721910000
_diffrn_orient_matrix_UB_23      0.0165755000
_diffrn_orient_matrix_UB_31      0.0771779000
_diffrn_orient_matrix_UB_32      -0.0181019000
_diffrn_orient_matrix_UB_33      0.0117748000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10890
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0239P)^2^+0.1743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                4548
_reflns_number_total             5353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2019-0886_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        1309.74(14)
_cod_database_code               8105249
_chemical_oxdiff_formula         C1H1O1N1Pd1
_reflns_odcompleteness_completeness 99.83
_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:
 C29(H29A,H29B)
2.b 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), C23(H23), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'