1H NMR spectroscopic identification of binding modes of 2,2′-bipyridine ligands in complexes of square-planar d8 metal ions
Shen, Wei-Zheng; Trötscher-Kaus, Gabriele; Lippert, Bernhard; Dalton Transactions  (2009) 8203–8214; doi:10.1039/b904173g

data_7002362
_publ_section_title
;
 1H NMR spectroscopic identification of binding modes of
 2,2&#x2032;-bipyridine ligands in complexes of square-planar d8 metal
 ions
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8203
_journal_page_last               8214
_journal_paper_doi               10.1039/b904173g
_journal_year                    2009
_chemical_formula_moiety         'C30 H32 N10 O9 Pd2'
_chemical_formula_sum            'C30 H32 N10 O9 Pd2'
_chemical_formula_weight         889.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2009-05-25
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 119.03(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.188(3)
_cell_length_b                   16.115(3)
_cell_length_c                   17.888(7)
_cell_measurement_reflns_used    5239
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     3576.1(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1302
_diffrn_reflns_av_unetI/netI     0.2021
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10021
_diffrn_reflns_theta_full        23.74
_diffrn_reflns_theta_max         23.74
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5239
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.1795
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.154
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                1846
_reflns_number_total             5239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904173g.txt
_cod_data_source_block           1_729008_shen
_cod_original_cell_volume        3576.1(17)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7002362