Regioselective ortho Amination of Coordinated 2-(Arylazo)pyridine. Isolation of Monoradical Palladium Complexes of a New Series of Azo-Aromatic Pincer Ligands.
Sengupta, Debabrata; Chowdhury, Nabanita Saha; Samanta, Subhas; Ghosh, Pradip; Seth, Saikat Kumar; Demeshko, Serhiy; Meyer, Franc; Goswami, Sreebrata; Inorganic chemistry 54 (2015) 11465–11476; doi:10.1021/acs.inorgchem.5b02110

data_4346769
_publ_section_title
;
 Regioselective ortho Amination of Coordinated 2-(Arylazo)pyridine.
 Isolation of Monoradical Palladium Complexes of a New Series of
 Azo-Aromatic Pincer Ligands.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11465
_journal_page_last               11476
_journal_paper_doi               10.1021/acs.inorgchem.5b02110
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C15 H17 Cl2 N4 Pd'
_chemical_formula_sum            'C15 H17 Cl2 N4 Pd'
_chemical_formula_weight         430.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.398(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6921(17)
_cell_length_b                   11.836(3)
_cell_length_c                   18.457(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1672.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi SCANS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14342
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.047
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       Square
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0478P)^2^+0.9156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3023
_reflns_number_total             3715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02110_si_002.cif
_cod_data_source_block           1e
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4346769
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.861
_shelxl_version_number           2013-4
_shelx_res_checksum              92689
_shelx_hkl_checksum              84821