Sterically Demanding Multidentate Ligand Tris[(2-(6-methylpyridyl))methyl]amine Slows Exchange and Enhances Solution State Ligand Proton NMR Coupling to 199Hg(II)
Deborah C. Bebout; James F. Bush; Kathleen K. Crahan; Edith V. Bowers; Raymond J. Butcher; Inorganic Chemistry 41 (2002) 2529–2536; doi:10.1021/ic011209w

data_4317947
_publ_section_title
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 Sterically Demanding Multidentate Ligand
 Tris[(2-(6-methylpyridyl))methyl]amine Slows Exchange and Enhances
 Solution State Ligand Proton NMR Coupling to 199Hg(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2529
_journal_page_last               2536
_journal_paper_doi               10.1021/ic011209w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H30 Cl2 Hg N4 O9'
_chemical_formula_weight         790.01
_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                115.458(10)
_cell_angle_beta                 90.286(11)
_cell_angle_gamma                108.445(11)
_cell_formula_units_Z            2
_cell_length_a                   9.3525(16)
_cell_length_b                   12.956(2)
_cell_length_c                   14.199(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.30
_cell_measurement_theta_min      5.25
_cell_volume                     1453.5(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7961
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.60
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.534
_exptl_absorpt_correction_T_max  0.7885
_exptl_absorpt_correction_T_min  0.3865
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0029(3)
_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   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+1.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                6013
_reflns_number_total             7516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011209w.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4317947