Design and Synthesis of a New Binucleating Ligand via Cobalt-Promoted C-N Bond Fusion Reaction. Ligand Isolation and Its Coordination to Nickel, Palladium, and Platinum
Kunal K. Kamar; Srijit Das; Chen-Hsiung Hung; Alfonso Castiñeiras; Michael D. Kuz'min; Conrado Rillo; Juan Bartolomé; Sreebrata Goswami; Inorganic Chemistry 42 (2003) 5367–5375; doi:10.1021/ic034313h

data_4314079
_publ_section_title
;
 Design and Synthesis of a New Binucleating Ligand via Cobalt-Promoted C-N
 Bond Fusion Reaction. Ligand Isolation and Its Coordination to Nickel,
 Palladium, and Platinum
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5367
_journal_page_last               5375
_journal_paper_doi               10.1021/ic034313h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C32 H26 Cl2 N10 O9 Pd2'
_chemical_formula_weight         978.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.919(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5546(9)
_cell_length_b                   14.4884(11)
_cell_length_c                   21.2438(15)
_cell_measurement_temperature    293(2)
_cell_volume                     3766.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.1860
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23768
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2634
_reflns_number_total             8654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034313hsi20030630_015107.cif
_cod_data_source_block           c:\xray\h204\work\h204m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3766.3(5)
_cod_database_code               4314079