Synthesis and Characterization of Palladium(II) and Platinum(II) Adducts and Cyclometalated Complexes of 6,6′-Dimethoxy-2,2′-bipyridine: C(sp3)‒H and C(sp2)‒H Bond Activations
Cocco, Fabio; Zucca, Antonio; Stoccoro, Sergio; Serratrice, Maria; Guerri, Annalisa; Cinellu, Maria A.; Organometallics  (2014) 140624160931008–; doi:10.1021/om5003057

data_4083737
_publ_section_title
;
 Synthesis and Characterization of Palladium(II) and Platinum(II)
 Adducts and Cyclometalated Complexes of
 6,6&#x2032;-Dimethoxy-2,2&#x2032;-bipyridine: C(sp3)--H and C(sp2)--H
 Bond Activations
;
_journal_name_full               Organometallics
_journal_page_first              140624160931008
_journal_paper_doi               10.1021/om5003057
_journal_year                    2014
_chemical_formula_sum            'C14 H18 Cl3 N2 O3 Pt1.5 S'
_chemical_formula_weight         693.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
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_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'
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_cell_angle_beta                 103.920(4)
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_cell_measurement_reflns_used    4515
_cell_measurement_temperature    150(2)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'Sir97 (Altomare,1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         32.728
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    11.435
_exptl_absorpt_correction_T_max  0.63292
_exptl_absorpt_correction_T_min  0.42417
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.391
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0064P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4590
_reflns_number_total             6324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5003057_si_002.cif
_cod_data_source_block           9
_cod_original_formula_sum        'C14 H18 Cl3 N2 O3 Pt1.50 S'
_cod_database_code               4083737
_shelxl_version_number           2012-9
_shelx_res_checksum              26338
_shelx_hkl_checksum              92805