Experimental and Theoretical Studies of 45Sc NMR Interactions in Solids
Aaron J. Rossini; Robert W. Schurko; Journal of the American Chemical Society 128 (2006) 10391–10402; doi:10.1021/ja060477w

data_4110800
_publ_section_title
;
 Experimental and Theoretical Studies of 45Sc NMR Interactions in Solids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10391
_journal_page_last               10402
_journal_paper_doi               10.1021/ja060477w
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'H10 N3 O14 Sc'
_chemical_formula_weight         321.07
_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                84.179(5)
_cell_angle_beta                 70.033(5)
_cell_angle_gamma                66.679(5)
_cell_formula_units_Z            2
_cell_length_a                   8.075(5)
_cell_length_b                   8.821(5)
_cell_length_c                   9.267(5)
_cell_measurement_reflns_used    3651
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.52
_cell_volume                     569.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6491
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0333P)^2^+0.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                2250
_reflns_number_total             2579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060477wsi20060407_043921_ScNO33_5H2O.cif
_cod_data_source_block           p1b
_cod_database_code               4110800