Gd(III)[15-Metallacrown-5] Recognition of Chiral α-Amino Acid Analogues
Choong-Sun Lim; Joseph Jankolovits; Peng Zhao; Jeff W. Kampf; Vincent L. Pecoraro; Inorganic Chemistry 50 (2011) 4832–4841; doi:10.1021/ic102579t

data_4325178
_publ_contact_author             vlpec@umich.edu
_publ_section_title
;
 Gd(III)[15-Metallacrown-5] Recognition of Chiral \a-Amino Acid Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4832
_journal_page_last               4841
_journal_paper_doi               10.1021/ic102579t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C54 H61 Cu5 Gd N12 O19 , 2(N O3), 6(H2O) '
_chemical_formula_sum            'C54 H79 Cu5 Gd N14 O30'
_chemical_formula_weight         1879.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.092(3)
_cell_length_b                   16.734(3)
_cell_length_c                   28.419(5)
_cell_measurement_reflns_used    6902
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.79
_cell_volume                     7177(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      118(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            66765
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.8665
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Blessing, R. Acta Cryst. (1995) A51 33-38'
 Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
 detector absorption and other corrections, University of
 Gottingen, Germany 2003.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       plate
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.921
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(11)
_refine_ls_extinction_coef       0.00260(8)
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         14649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0572P)^2^+11.7390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                12496
_reflns_number_total             14649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102579t_si_001_1.cif
_cod_data_source_block           1-S-2
_cod_database_code               4325178