Crystal structure of [2-(4-methoxyphenyl)pyrazine-κ2 C,N) chlorido[N,N′-bis-(2,6-diisopropyl-phenyl)imidazol-2-ylidene-κC)] palladium(II), C38H45ClN4OPd
Wang, Xin-Ling; Li, Hong-Mei; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 145–147; doi:10.1515/ncrs-2015-0063

data_8106809
_publ_section_title
;
 Crystal structure of [2-(4-methoxyphenyl)pyrazine-\k2 C,N)
 chlorido[N,N&#x2032;-bis-(2,6-diisopropyl-phenyl)imidazol-2-ylidene-\kC)]
 palladium(II), C38H45ClN4OPd
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              145
_journal_page_last               147
_journal_paper_doi               10.1515/ncrs-2015-0063
_journal_volume                  231
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H45 Cl N4 O Pd'
_chemical_formula_sum            'C38 H45 Cl N4 O Pd'
_chemical_formula_weight         715.63
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   30.1968(8)
_cell_length_b                   30.1968(8)
_cell_length_c                   11.4611(3)
_cell_measurement_reflns_used    3261
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.4200
_cell_measurement_theta_min      3.5600
_cell_volume                     9050.6(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0165944000
_diffrn_orient_matrix_UB_12      0.0064152000
_diffrn_orient_matrix_UB_13      0.0486440000
_diffrn_orient_matrix_UB_21      0.0132371000
_diffrn_orient_matrix_UB_22      -0.0108723000
_diffrn_orient_matrix_UB_23      -0.0282417000
_diffrn_orient_matrix_UB_31      0.0168900000
_diffrn_orient_matrix_UB_32      0.0239988000
_diffrn_orient_matrix_UB_33      -0.0258401000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8267
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97567
_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
;
;
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3895
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3362
_reflns_number_total             3895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2015-0063_supp.cif
_cod_data_source_block           1
_cod_original_cell_volume        9050.7(4)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               8106809
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C9(H9), C10(H10), C13(H13), C16(H16),
 C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;