Pd‒PEPPSI-Type Expanded Ring N-Heterocyclic Carbene Complexes: Synthesis, Characterization, and Catalytic Activity in Suzuki‒Miyaura Cross Coupling
Dunsford, Jay J.; Cavell, Kingsley J.; Organometallics 33 (2014) 2902–; doi:10.1021/om5003107

data_4083335
_publ_section_title
;
 Pd--PEPPSI-Type Expanded Ring N-Heterocyclic Carbene Complexes:
 Synthesis, Characterization, and Catalytic Activity in Suzuki--Miyaura
 Cross Coupling
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2902
_journal_paper_doi               10.1021/om5003107
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C28 H34 Cl3 N3 Pd'
_chemical_formula_sum            'C28 H34 Cl3 N3 Pd'
_chemical_formula_weight         625.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-02-08
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4260(2)
_cell_length_b                   18.7561(3)
_cell_length_c                   22.6164(3)
_cell_measurement_reflns_used    11529
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.2480
_cell_measurement_theta_min      3.6830
_cell_volume                     5695.25(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
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_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9969
_diffrn_measurement_details
;
  1 omega  -20.00    5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555  -99.0000  120.0000 25

  2 omega  -50.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   19.0000  150.0000 118

  3 omega  -45.00  -17.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   77.0000  -60.0000 28
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0451557000
_diffrn_orient_matrix_UB_12      -0.0085630000
_diffrn_orient_matrix_UB_13      0.0146409000
_diffrn_orient_matrix_UB_21      0.0258088000
_diffrn_orient_matrix_UB_22      -0.0248309000
_diffrn_orient_matrix_UB_23      0.0180402000
_diffrn_orient_matrix_UB_31      0.0092961000
_diffrn_orient_matrix_UB_32      0.0271978000
_diffrn_orient_matrix_UB_33      0.0210702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25402
_diffrn_reflns_theta_full        29.4010
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4586
_exptl_crystal_description       block
_exptl_crystal_F_000             2260.0
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.5954
_refine_diff_density_min         -0.7201
_refine_diff_density_rms         0.1475
_refine_ls_d_res_high            0.7239
_refine_ls_d_res_low             7.2791
_refine_ls_goodness_of_fit_ref   1.1052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1052
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+6.3372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                5464
_reflns_number_total             6969
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om5003107_si_002.cif
_cod_data_source_block           amji74
_cod_depositor_comments
'Adding full bibliography for 4083335--4083336.cif.'
_cod_database_code               4083335
_chemical_oxdiff_formula         'C27 H32 N3 Pd Cl3'
_reflns_odcompleteness_completeness 99.69
_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:
 C5(H5a,H5b), C2(H2a,H2b), C4(H4a,H4b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C25(H25), C28(H28), C12(H12), C24(H24), C27(H27), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C23(H23a,H23b,H23c), C16(H16a,H16b,H16c), C17(H17a,H17b,
 H17c), C10(H10a,H10b,H10c), C14(H14a,H14b,H14c)
;