Synthesis and Characterization of Racemic Mixture and Meso Isomers of Bis(trans-2-aminocyclohexyl)aminepentaacetic Acid and the Stabilities of Their Gd(III) Complexes
Yizhen Sun; Arthur E. Martell; Joseph H. Reibenspies; David E. Reichert; Michael J. Welch; Inorganic Chemistry 39 (2000) 1480–1486; doi:10.1021/ic991189m

data_4320836
_publ_section_title
;
 Synthesis and Characterization of Racemic Mixture and Meso Isomers of
 Bis(trans-2-aminocyclohexyl)aminepentaacetic Acid and the Stabilities of
 Their Gd(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1480
_journal_page_last               1486
_journal_paper_doi               10.1021/ic991189m
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C42 H75 N3 O10'
_chemical_formula_weight         782.05
_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                91.41(3)
_cell_angle_beta                 98.23(3)
_cell_angle_gamma                113.88(3)
_cell_formula_units_Z            2
_cell_length_a                   10.805(2)
_cell_length_b                   11.384(2)
_cell_length_c                   20.999(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2327.8(10)
_computing_cell_refinement       'P3VAX (SIEMENS, 1990)'
_computing_data_collection       'P3VAX (SIEMENS, 1990)'
_computing_data_reduction        'XDISK (SIEMENS, 1990)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Siemens R3M'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0008(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1386P)^2^+1.5009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2336
_refine_ls_wR_factor_ref         0.2800
_reflns_number_gt                4540
_reflns_number_total             7968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991189m.cif
_cod_data_source_block           am99
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        2327.8(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4320836