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_4328887
_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
;
 [LaCu5(C8H8N2O2)5]4(C10H4O4S2)6(C3H7N2O2)5(CH4O)2(H2O)27.5
;
_chemical_formula_sum            'C237 H282 Cu20 La4 N50 O103.5 S12'
_chemical_formula_weight         7698.29
_chemical_name_systematic
; 
 La[15-MC Cu(II), L-phenylglycineHA-5](bithiophene dicarboxylate) 
;
_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                 100.620(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5616(14)
_cell_length_b                   30.839(3)
_cell_length_c                   30.729(3)
_cell_measurement_temperature    150(2)
_cell_volume                     14494(2)
_computing_cell_refinement       'Bruker SAINT v7.60A'
_computing_data_collection       'Bruker APEX2 v2009.11.0'
_computing_data_reduction        'Bruker SAINT v7.60A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            252123
_diffrn_reflns_theta_full        29.08
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         0.74
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.7945
_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            grey-purple
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       blade
_exptl_crystal_F_000             7764
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.750
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.277
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.089(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3775
_refine_ls_number_reflns         59688
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                39751
_reflns_number_total             59688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202347j_si_002_2.cif
_cod_data_source_block           La3+[15-MCCu(II),pgHA-5](btDC)
_cod_original_formula_sum        'C237 H282 Cu20 La4 N50 O103.50 S12'
_cod_database_code               4328887