Variable-Temperature Nuclear Magnetic Resonance Spectroscopy Allows Direct Observation of Carboxylate Shift in Zinc Carboxylate Complexes
Alojz Demšar; Janez Košmrlj; Saša Petriček; Journal of the American Chemical Society 124 (2002) 3951–3958; doi:10.1021/ja016534x

data_4114731
_publ_section_title
;
 Variable-Temperature Nuclear Magnetic Resonance Spectroscopy Allows
 Direct Observation of Carboxylate Shift in Zinc Carboxylate Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3951
_journal_page_last               3958
_journal_paper_doi               10.1021/ja016534x
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C14 H26 Cl2 D2 N2 O7 Zn2'
_chemical_formula_weight         540.04
_chemical_name_systematic
;
 catena tetrakis(\m-acetato-O,O')(\m-acetato-O,O)(\m-1,3-bis
(dimethylamino)N,N'-2-propoxo-O) di-zinc(II)
;
_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     SIR92
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7671(2)
_cell_length_b                   13.4855(3)
_cell_length_c                   15.5292(4)
_cell_measurement_temperature    200(2)
_cell_volume                     2254.64(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9663
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.399
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+2.5944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                3879
_reflns_number_total             5130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016534x_s2_3.cif
_cod_data_source_block           k149
_cod_database_code               4114731