Nickel(II) and Palladium(II) Complexes with Chelating N-Heterocyclic Carbene Amidate Ligands: Interplay between Normal and Abnormal Coordination Modes
Tan, Kel Vin; Dutton, Jason L.; Skelton, Brian W.; Wilson, David J. D.; Barnard, Peter J.; Organometallics 32 (2013) 1913–; doi:10.1021/om4000133

data_4080469
_publ_section_title
;
 Nickel(II) and Palladium(II) Complexes with Chelating N-Heterocyclic
 Carbene Amidate Ligands: Interplay between Normal and Abnormal
 Coordination Modes
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_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1913
_journal_paper_doi               10.1021/om4000133
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C28 H22 N6 O2 Pd, C H4 O, C0.5 H1.5 O0.25'
_chemical_formula_sum            'C29.5 H27.5 N6 O3.25 Pd'
_chemical_formula_weight         624.48
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-08
_audit_creation_method
;
  Olex2 1.2
  (compiled Oct 26 2012 17:06:22, GUI svn.r4371)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.648(4)
_cell_length_b                   19.386(4)
_cell_length_c                   14.289(3)
_cell_measurement_reflns_used    5432
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.4362
_cell_measurement_theta_min      2.4294
_cell_volume                     5271(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      173
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14425
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0416P)^2^+8.0861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                4106
_reflns_number_total             5195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4000133_si_002.cif
_cod_data_source_block           6a,a
_cod_original_cell_volume        5271.5(18)
_cod_original_formula_sum        'C29.50 H27.50 N6 O3.25 Pd'
_cod_database_code               4080469
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H12' of C12', H13' of C13', H13 of C13, H7' of C7', H1' of C1', H11 of C11,
  H3' of C3', H8' of C8', H7 of C7, H10' of C10', H14' of C14', H12 of C12, H8
  of C8, H11' of C11', {H4A,H4B} of C4, H1 of C1, H3 of C3, {H4'A,H4'B} of C4',
  H10 of C10, H14 of C14
 At 1.5 times of:
  {H15A,H15B,H15C} of C15, {H16A,H16B,H16C} of C16, H2 of O2
2. Others
 Fixed Sof: C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) O3(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C4'(H4'A,H4'B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C10(H10), C14(H14), C7(H7), C8'(H8'), C13(H13), C8(H8),
 C12(H12), C11(H11), C3'(H3'), C1'(H1'), C7'(H7'), C14'(H14'), C10'(H10'),
 C11'(H11'), C12'(H12'), C13'(H13')
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
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