Synthesis, Characterization, and X-ray Crystal Structure of In(DOTA-AA) (AA = p-Aminoanilide): A Model for 111In-Labeled DOTA-Biomolecule Conjugates
Shuang Liu; Zhengjie He; Wen-Yuan Hsieh; Phillip E. Fanwick; Inorganic Chemistry 42 (2003) 8831–8837; doi:10.1021/ic0349914

data_4312822
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@.purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Phillip E. Fanwick'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Synthesis, Characterization, and X-ray Crystal Structure of In(DOTA-AA)
 (AA = p-Aminoanilide): A Model for 111In-Labeled DOTA-Biomolecule
 Conjugates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8831
_journal_page_last               8837
_journal_paper_doi               10.1021/ic0349914
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C22 H31 In1 N6 O7,4(H2 O1)'
_chemical_formula_sum            'C22 H39 In N6 O11'
_chemical_formula_weight         678.41
_chemical_name_systematic        ' ?'
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             5-05-03
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.5963(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3412(2)
_cell_length_b                   23.4757(7)
_cell_length_c                   13.0486(4)
_cell_measurement_reflns_used    17859
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     2712.04(13)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF99,_Beurskins,_1999)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.8411
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17859
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.7408
_exptl_absorpt_correction_T_min  0.5403
_exptl_absorpt_correction_type   multi-scan_(Otwinowski_&_Minor,_
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.66
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment
;
Chemically significant hydrogens refined isotropically
Others riding
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6091
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.3352P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.072
_reflns_number_gt                5196
_reflns_number_total             6101
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic0349914si20030821_115226.cif
_cod_data_source_block           SL001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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_original_formula_sum        'C22 H39 In1 N6 O11'
_cod_database_code               4312822