NCN Pincer Palladium Complexes Based on 1,3-dipicolyl-3,4,5,6-tetrahydropyrimidin-2-ylidenes: Synthesis, Characterization and Catalytic Activities
Yang, Liangru; Zhang, Xinchi; Mao, Pu; Xiao, Yong-Mei; Bian, Huanyu; Yuan, Jinwei; Mai, Wen-Peng; Qu, Lingbo; RSC Adv.  (2015) –; doi:10.1039/C5RA01706H

data_7219756
_publ_section_title
;
 NCN Pincer Palladium Complexes Based on
 1,3-dipicolyl-3,4,5,6-tetrahydropyrimidin-2-ylidenes: Synthesis,
 Characterization and Catalytic Activities
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA01706H
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'F6 P, C18 H23 N4'
_chemical_formula_sum            'C18 H23 F6 N4 P'
_chemical_formula_weight         440.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-23
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_audit_update_record
;
2014-12-12 deposited with the CCDC.
2015-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6098(2)
_cell_length_b                   11.4528(4)
_cell_length_c                   18.8441(5)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.6450
_cell_measurement_theta_min      4.5140
_cell_volume                     2073.97(10)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -71.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 33

  2 omega  -95.00  -69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -60.0000 26

  3 omega -113.00  -18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -37.0000   60.0000 95

  4 omega  -61.00  -34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -60.0000 27

  5 omega -112.00  -65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -143.0000 -160.0000 47

  6 omega   68.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  -60.0000 36

  7 omega   34.00   59.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  -60.0000 25

  8 omega   47.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 35

  9 omega   48.00  112.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 64

 10 omega   41.00   84.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 43

 11 omega   42.00   98.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 56

 12 omega   94.00  174.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 80

 13 omega  -49.00  -23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000   60.0000 26

 14 omega  -18.00   18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000   60.0000 36

 15 omega  -31.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000  150.0000 57

 16 omega   58.00   87.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4066  -37.0000  -90.0000 29

 17 omega   94.00  157.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4066   63.0000   90.0000 63

 18 omega   39.00   64.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4066  -37.0000 -180.0000 25

 19 omega   39.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4066  -37.0000  -30.0000 43

 20 omega   88.00  130.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      111.4066  -91.0000    0.0000 42
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0975149000
_diffrn_orient_matrix_UB_12      0.0566383000
_diffrn_orient_matrix_UB_13      -0.0549873000
_diffrn_orient_matrix_UB_21      0.0810700000
_diffrn_orient_matrix_UB_22      -0.0602247000
_diffrn_orient_matrix_UB_23      -0.0602654000
_diffrn_orient_matrix_UB_31      -0.0980524000
_diffrn_orient_matrix_UB_32      -0.1061064000
_diffrn_orient_matrix_UB_33      0.0048939000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7994
_diffrn_reflns_theta_full        72.38
_diffrn_reflns_theta_max         72.38
_diffrn_reflns_theta_min         4.52
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75941
_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_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_coef       0.0020(3)
_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   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.2565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1494
_reflns_number_gt                3502
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra01706h3.cif
_cod_data_source_block           201309151
_cod_original_cell_volume        2073.98(10)
_cod_database_code               7219756
_chemical_oxdiff_formula         C20H20P1F6
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97