Chelating Bis-N-heterocyclic Carbene‒Palladium(II) Complexes for Oxidative Arene C‒H Functionalization
Desai, Sai Puneet; Mondal, Moumita; Choudhury, Joyanta; Organometallics 34 (2015) 2731–; doi:10.1021/om501163m

data_4089707
_publ_section_title
;
 Chelating Bis-N-heterocyclic Carbene--Palladium(II) Complexes for
 Oxidative Arene C--H Functionalization
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2731
_journal_paper_doi               10.1021/om501163m
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C20 H28 Cl4 I3 N5 Pd'
_chemical_formula_weight         967.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.9849(15)
_cell_length_b                   12.9449(7)
_cell_length_c                   7.9074(5)
_cell_measurement_reflns_used    2861
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      26.031
_cell_measurement_theta_min      2.677
_cell_volume                     2864.5(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      109(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8106
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.031
_diffrn_reflns_theta_min         2.677
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.274
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0300P)^2^+114.3094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2183
_reflns_number_total             2861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501163m_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4089707
_shelx_estimated_absorpt_t_min   0.467
_shelx_estimated_absorpt_t_max   0.784
_shelxl_version_number           2014-3
_shelx_res_checksum              97925
_shelx_hkl_checksum              88605