Use of 13C-1H NMR Coupling Constants To Assess the Binding of Imidazole Ring Ligands to Metals
Scott J. Moore; Rene J. Lachicotte; Sharon T. Sullivan; Luigi G. Marzilli; Inorganic Chemistry 38 (1999) 383–390; doi:10.1021/ic980519k

data_4321739
_publ_section_title
;
 Use of 13C-1H NMR Coupling Constants To Assess the Binding of Imidazole
 Ring Ligands to Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              383
_journal_page_last               390
_journal_paper_doi               10.1021/ic980519k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H20 Cl Co N6 O4'
_chemical_formula_weight         406.72
_chemical_name_common            1-methylimidazole-chlorocobaloxime
_chemical_name_systematic
; 
 trans-bis(Dimethylglyoximato)-chloro-1-methylimidazole-cobalt(iii) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.059(18)
_cell_angle_beta                 84.022(17)
_cell_angle_gamma                68.483(12)
_cell_formula_units_Z            2
_cell_length_a                   8.9783(15)
_cell_length_b                   9.0136(15)
_cell_length_c                   11.480(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      2.41
_cell_volume                     859.1(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2760
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        4.40
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.184
_exptl_crystal_colour            'amber             '
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate             '
_exptl_crystal_F_000             420
_exptl_crystal_size_max          .16
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .4
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0454
_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
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2019
_reflns_number_total             2241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980519k_4.cif
_cod_data_source_block           NMeImdCo(DH)2Cl
_cod_database_code               4321739