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_4303294
_publ_contact_author_address
; 
 Department of Chemistry and Biochemistry
 University of Minnesota Duluth
 1039 University Drive
 Duluth, MN 55812, USA  
;
_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         'C40 H75 N10 O17 Sm1'
_chemical_formula_sum            'C40 H75 N10 O17 Sm'
_chemical_formula_weight         1118.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-01-30
_audit_creation_method           CRYSTALS_ver_12.85
_audit_update_record
;
2009-02-02 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 102.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.198(4)
_cell_length_b                   16.070(3)
_cell_length_c                   16.119(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      18
_cell_measurement_theta_min      15
_cell_volume                     5363.1(18)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12746
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.189
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.56
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.005762
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 29.9 39.6 22.5 4.98 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1530
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1312
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7649
_reflns_number_total             12305
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0599
_oxford_refine_ls_scale          0.18366(10)
_oxford_reflns_number_all        12265
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'Amid in P2(1)/n'
_cod_data_source_file            ic901191a_si_002_1.cif
_cod_data_source_block           Sm(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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C40 H75 N10 O17 Sm1'
_cod_database_code               4303294