Solvent dependent assembly of lanthanide metallacrowns using building blocks with incompatible symmetry preferences.
Jankolovits, Joseph; Kampf, Jeff W.; Pecoraro, Vincent L.; Inorganic chemistry 53 (2014) 7534–7546; doi:10.1021/ic500832u

data_4340049
_publ_section_title
;
 Solvent dependent assembly of lanthanide metallacrowns using building
 blocks with incompatible symmetry preferences.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7534
_journal_page_last               7546
_journal_paper_doi               10.1021/ic500832u
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C100 H80 Eu3 N29 O23 Zn7'
_chemical_formula_sum            'C50 H44 Eu N17 O21 Zn5'
_chemical_formula_weight         1697.83
_chemical_name_systematic
; 
 Eu(III)[15-MC Zn(II),picHA-5](NO3)3(py)4 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            16
_cell_length_a                   45.3648(6)
_cell_length_b                   45.3648(6)
_cell_length_c                   12.0304(9)
_cell_measurement_reflns_used    119997
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.00
_cell_volume                     24758.1(19)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            148290
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    10.036
_exptl_absorpt_correction_T_max  0.2653
_exptl_absorpt_correction_T_min  0.2653
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+75.9379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                10045
_reflns_number_total             11345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500832u_si_001.cif
_cod_data_source_block           EuZn5(quinHA)5
_cod_depositor_comments
'Adding full bibliography for 4340046--4340049.cif.'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4340049