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_4340046
_publ_contact_author             vlpec@umich.edu
_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         'C37.50 H45 Dy0.50 Zn2 N9.50 O13.50'
_chemical_formula_sum            'C37.5 H45 Dy0.5 N9.5 O13.5 Zn2'
_chemical_formula_weight         1056.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 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            4
_cell_length_a                   19.5887(5)
_cell_length_b                   22.7717(16)
_cell_length_c                   10.1759(3)
_cell_measurement_reflns_used    7100
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      3.00
_cell_volume                     4539.1(4)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 2.0 r5 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 2.0 r5 
;
_computing_data_reduction
; 
Rigaku 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 22.2222
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Rigaku CrystalClear-SM Expert 2.0 r5 
;
_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  0.0986
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            97529
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    6.220
_exptl_absorpt_correction_T_max  0.6360
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2150
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         8302
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0981P)^2^+14.4620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                7571
_reflns_number_total             8302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500832u_si_001.cif
_cod_data_source_block           DyZn4(quinHA)4
_cod_depositor_comments
'Adding full bibliography for 4340046--4340049.cif.'
_cod_original_formula_sum        'C37.5 H45 Dy0.5 Zn2 N9.5 O13.5'
_cod_database_code               4340046