Influencing the Size and Anion Selectivity of Dimeric Ln3+[15-Metallacrown-5] Compartments through Systematic Variation of the Host Side Chains and Central Metal
Joseph Jankolovits; Choong-Sun Lim; Gellert Mezei; Jeff W. Kampf; Vincent L. Pecoraro; Inorganic Chemistry 51 (2012) 4527–4538; doi:10.1021/ic202347j

data_4328888
_publ_contact_author             vlpec@umich.edu
_publ_section_title
;
 Influencing the Size and Anion Selectivity of Dimeric
 Ln3+[15-Metallacrown-5] Compartments through Systematic Variation of the
 Host Side Chains and Central Metal
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4527
_journal_page_last               4538
_journal_paper_doi               10.1021/ic202347j
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
 (GdCu5C50H60N10O10)2(C10H4O4S2)3(C3H7NO)8(H2O)18(CH4O)0.25 
;
_chemical_formula_sum            'C154.25 H225 Cu10 Gd2 N28 O58.25 S6'
_chemical_formula_weight         4545.88
_chemical_name_systematic
; 
 Gd[15-MC Cu(II), L-homopheHA-5](btDC)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.7120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7609(9)
_cell_length_b                   35.759(2)
_cell_length_c                   17.9482(10)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.25
_cell_volume                     10247.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            409925
_diffrn_reflns_theta_full        29.59
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  0.7383
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       multi-faceted
_exptl_crystal_F_000             4653
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.127
_refine_diff_density_min         -1.933
_refine_diff_density_rms         0.243
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2741
_refine_ls_number_reflns         57566
_refine_ls_number_restraints     2500
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+48.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                54661
_reflns_number_total             57566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202347j_si_002_3.cif
_cod_data_source_block           Gd3+[15-MCCu(II),hpheHA-5](btDC)
_cod_database_code               4328888