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_7219757
_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         'C18 H22 Cl N4 Pd, F6 P'
_chemical_formula_sum            'C18 H22 Cl F6 N4 P Pd'
_chemical_formula_weight         581.22
_chemical_name_systematic
;
 ? 
;
_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             2014-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_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                   7.8169(4)
_cell_length_b                   12.9702(6)
_cell_length_c                   22.3383(10)
_cell_measurement_reflns_used    2876
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.8030
_cell_measurement_theta_min      3.2680
_cell_volume                     2264.81(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -23.00    6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -120.0000 29

  2 omega   -3.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   37.0000 -120.0000 84

  3 omega   36.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000 -150.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0826572000
_diffrn_orient_matrix_UB_12      -0.0042191000
_diffrn_orient_matrix_UB_13      -0.0128659000
_diffrn_orient_matrix_UB_21      -0.0236706000
_diffrn_orient_matrix_UB_22      -0.0357372000
_diffrn_orient_matrix_UB_23      0.0225695000
_diffrn_orient_matrix_UB_31      -0.0289072000
_diffrn_orient_matrix_UB_32      0.0412148000
_diffrn_orient_matrix_UB_33      0.0182472000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6519
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98578
_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_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0541P)^2^+0.8150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                3684
_reflns_number_total             4214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra01706h3.cif
_cod_data_source_block           201408162
_cod_original_cell_volume        2264.82(18)
_cod_database_code               7219757
_chemical_oxdiff_formula         C20H20N4O4Cl1Pd1
_reflns_odcompleteness_completeness 99.70
_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:
 C2(H2A,H2B), C4(H4A,H4B), C7(H7A,H7B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'