Facile base-free in situ generation and palladation of mesoionic and normal N-heterocyclic carbenes at ambient conditions.
Sureshbabu, Bemineni; Ramkumar, Venkatachalam; Sankararaman, Sethuraman; Dalton transactions (Cambridge, England : 2003) 43 (2014) 10710–10712; doi:10.1039/c4dt01112k

data_7031196
_publ_section_title
;
 Facile base-free in situ generation and palladation of mesoionic and
 normal N-heterocyclic carbenes at ambient conditions.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10710
_journal_page_last               10712
_journal_paper_doi               10.1039/c4dt01112k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C32 H28 Br2 N4 Pd '
_chemical_formula_sum            'C32 H28 Br2 N4 Pd'
_chemical_formula_weight         734.80
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 100.0162(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   20.2336(10)
_cell_length_c                   9.0739(4)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.49
_cell_volume                     1441.50(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
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_diffrn_reflns_limit_l_min       -10
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_diffrn_reflns_point_group_measured_fraction_full 0.974
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_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.013
_exptl_absorpt_coefficient_mu    3.444
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            green
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_exptl_crystal_description       rectangular
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_exptl_crystal_size_max          0.350
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_refine_diff_density_max         0.290
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_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2286
_reflns_number_total             2544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01112k2.cif
_cod_data_source_block           211
_cod_depositor_comments
'Adding full bibliography for 7031193--7031196.cif.'
_cod_database_code               7031196
_shelx_estimated_absorpt_t_min   0.379
_shelx_estimated_absorpt_t_max   0.626
_shelxl_version_number           2013-3
_shelx_res_checksum              66279