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_4346773
_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         'C47 H37 Cl2 N3 P2 Pd'
_chemical_formula_sum            'C47 H37 Cl2 N3 P2 Pd'
_chemical_formula_weight         883.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                80.675(5)
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_cell_angle_gamma                89.627(5)
_cell_formula_units_Z            2
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_cell_length_b                   12.002(5)
_cell_length_c                   16.139(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2021.9(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.781
_diffrn_measured_fraction_theta_max 0.990
_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  0.0828
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.781
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16587
_diffrn_reflns_point_group_measured_fraction_full 0.781
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.223
_diffrn_reflns_theta_min         1.290
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       plate
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+1.6338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3785
_reflns_number_total             5724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02110_si_002.cif
_cod_data_source_block           Pd-I
_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_cell_volume        2022.0(14)
_cod_database_code               4346773
_shelxl_version_number           2014-1
_shelx_res_checksum              37300
_shelx_hkl_checksum              82838