Rational Design of a Ternary Supramolecular System: Self-Assembly of Pentanuclear Lanthanide Helicates
Badr El Aroussi; Soumaila Zebret; Céline Besnard; Philippe Perrottet; Josef Hamacek; Journal of the American Chemical Society 133 (2011) 10764–10767; doi:10.1021/ja204474v

data_4106424
_publ_contact_author_address
;
Departement of Inorganic Analytical Chemistry
University of Geneva
30 quai E. Ansermet
Geneva 4
CH-1211
SWITZERLAND
;
_publ_contact_author_email       Josef.Hamacek@unige.ch
_publ_contact_author_name        'Dr Josef Hamacek'
_publ_section_title
;
 Rational Design of a Ternary Supramolecular System: Self-Assembly of
 Pentanuclear Lanthanide Helicates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10764
_journal_page_last               10767
_journal_paper_doi               10.1021/ja204474v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C105 H114 Lu2 N18 O12, 6(Cl O4), C5 O, 5.54(C2 H3 N) '
_chemical_formula_sum            'C121.08 H130.62 Cl6 Lu2 N23.54 O37'
_chemical_formula_weight         3069.94
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.88(2)
_cell_length_b                   24.28(2)
_cell_length_c                   25.540(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    220
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     14188(18)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      220
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            119882
_diffrn_reflns_theta_full        28.282
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         4.857
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.579
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6246.760
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9870
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         17514
_refine_ls_number_restraints     338
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.0205982
_refine_ls_shift/su_mean         0.8272135
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +38.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1186
_reflns_limit_h_max              30
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                13048
_reflns_number_total             17514
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0645
_oxford_refine_ls_scale          1.219(3)
_oxford_reflns_number_all        17514
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ja204474v_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        14192(18)
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C121.08 H130.62 Cl6 Lu2 N23.54 O37 '
_cod_database_code               4106424