Canopied trans-chelating bis(N-heterocyclic carbene) ligand: synthesis, structure and catalysis
Morgan, Brad P.; Galdamez, Gabriela A.; Gilliard, Jr., Robert J.; Smith, Rhett C.; Dalton Transactions  (2009) 2020–2028; doi:10.1039/b815739a

data_7000715
_publ_section_title
;
 Canopied trans-chelating bis(N-heterocyclic carbene) ligand:
 synthesis, structure and catalysis
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2020
_journal_page_last               2028
_journal_paper_doi               10.1039/b815739a
_journal_year                    2009
_chemical_formula_moiety         'C34 H38 Br0.57 Cl1.43 N4 Pd, C7 H8'
_chemical_formula_sum            'C41 H46 Br0.57 Cl1.43 N4 Pd'
_chemical_formula_weight         797.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.66(3)
_cell_angle_beta                 91.31(3)
_cell_angle_gamma                111.21(3)
_cell_formula_units_Z            2
_cell_length_a                   10.392(2)
_cell_length_b                   13.675(3)
_cell_length_c                   15.092(3)
_cell_measurement_reflns_used    4694
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.3732
_cell_measurement_theta_min      2.1313
_cell_volume                     1857.2(9)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC,2001)'
_computing_data_collection       'CrystalClear (Rigaku/MSC,2001)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC,2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS,2000)'
_computing_publication_material  'SHELXTL 6.10 (Bruker AXS,2000)'
_computing_structure_refinement  'SHELXTL 6.10 (Bruker AXS,2000)'
_computing_structure_solution    'SHELXTL 6.10 (Bruker AXS,2000)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
scan:
Number of images: 260
Slice: -40.0000 - 90.0000
Image width: 0.5000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 27.6329
2theta: -0.3627
scan:
Number of images: 220
Slice: -40.0000 - 90.0000
Image width: 0.5000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 27.6329
2theta: -0.3627

;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3 circle
;
_diffrn_measurement_method       omega
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13822
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.8852
_exptl_absorpt_correction_T_min  0.7705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'REQAB, Rigaku/MSC, The Woodlands, TX, USA, 1999.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             821
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0010P)^2^+9.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                4343
_reflns_number_total             6539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815739a.txt
_cod_data_source_block           {X2Pd{1}}CH3Ph
_cod_original_cell_volume        1857.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000715