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_4328890
_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(C45H50N10O10)]2(C6H4NO2)4(NO3)2(H2O)14(CH4O)
;
_chemical_formula_sum            'C115 H148 Cu10 La2 N26 O49'
_chemical_formula_weight         3591.81
_chemical_name_systematic
; 
 La[15-MC Cu(II), L-phenylalanineHA-5](isonicotinate)
;
_space_group_IT_number           1
_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                74.492(4)
_cell_angle_beta                 67.296(7)
_cell_angle_gamma                71.961(5)
_cell_formula_units_Z            1
_cell_length_a                   15.082(5)
_cell_length_b                   15.242(5)
_cell_length_c                   17.234(8)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.463
_cell_measurement_theta_min      2.295
_cell_volume                     3425(2)
_computing_cell_refinement       CELL_NOW
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37707
_diffrn_reflns_theta_full        29.71
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.222
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Sheldrick, G.M. TWINABS, v. 2008/2.  Program for empirical 
 Absorption Correction of Area Detector Data, University of 
 Gottingen: Gottingen, Germany, 2008.  
;
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       blue
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.389
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1829
_refine_ls_number_reflns         37707
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.738
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1952P)^2^+20.1674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                34495
_reflns_number_total             37707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202347j_si_002_5.cif
_cod_data_source_block           La3+[15-MCCu(II),pheHA-5](isonicotinate)
_cod_database_code               4328890