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_4328889
_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_formula_moiety
;
 (LaCu5C50H60N10O10)(C6H4NO2)2(NO3)(H2O)13.25
;
_chemical_formula_sum            'C63 H94.5 Cu5 La N13 O29.25'
_chemical_formula_weight         1958.63
_chemical_name_systematic
; 
 La[15-MC Cu(II), L-homopheHA-5](isonicotinate) 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            8
_cell_length_a                   16.4964(3)
_cell_length_b                   16.4964(3)
_cell_length_c                   61.5156(18)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      45.438
_cell_measurement_theta_min      4.383
_cell_volume                     16740.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1020
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            314012
_diffrn_reflns_theta_full        25.81
_diffrn_reflns_theta_max         25.81
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.6999
_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            purple
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             7996
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         16062
_refine_ls_number_restraints     820
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0948
_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^)+(0.0224P)^2^+279.5247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                14367
_reflns_number_total             16062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202347j_si_002_4.cif
_cod_data_source_block           La3+[15-MCCu(II),hpheHA-5](isonicotinate)
_cod_original_formula_sum        'C63 H94.50 Cu5 La N13 O29.25'
_cod_database_code               4328889