Structural and NMR Characterization of Sm(III), Eu(III), and Yb(III) Complexes of an Amide Based Polydentate Ligand Exhibiting Paramagnetic Chemical Exchange Saturation Transfer Abilities
Jason D. Dorweiler; Victor N. Nemykin; Amanda N. Ley; Robert D. Pike; Steven M. Berry; Inorganic Chemistry 48 (2009) 9365–9376; doi:10.1021/ic901191a

data_4303296
_publ_contact_author_address
; 
 Department of Chemistry and Biochemistry
 University of Minnesota Duluth
 1039 University Drive
 Duluth, MN 55812, USA  
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_publ_contact_author_email       vnemykin@d.umn.edu
_publ_contact_author_fax         '+1 218 7266729'
_publ_contact_author_name        'Victor Nemykin'
_publ_contact_author_phone       '+1 218 7266729'
_publ_section_title
;
Structural and NMR Characterization of Sm(III), Eu(III), and Yb(III)
Complexes of an Amide Based Polydentate Ligand Exhibiting Paramagnetic
Chemical Exchange Saturation Transfer Abilities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9365
_journal_page_last               9376
_journal_paper_doi               10.1021/ic901191a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C32 H64 N6 O7 Yb, 3(N O3), C2 H6 O'
_chemical_formula_sum            'C34 H70 N9 O17 Yb'
_chemical_formula_weight         1050.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.331(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.436(5)
_cell_length_b                   14.1718(18)
_cell_length_c                   20.786(3)
_cell_measurement_temperature    100(2)
_cell_volume                     10082(2)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'XSHELL (Bruker, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w and \y'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53564
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.033
_exptl_absorpt_correction_T_max  0.4482
_exptl_absorpt_correction_T_min  0.2717
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.179
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0605P)^2^+56.1010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                8198
_reflns_number_total             8630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901191a_si_002_3.cif
_cod_data_source_block           Yb(III)L
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4303296