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_4340047
_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         Dy2Zn16(picHA)16(py)4(OH)6(THF)1.25(H2O)21.25
_chemical_formula_sum            'C60.5 H71.25 Dy N18 O30.25 Zn8'
_chemical_formula_weight         2220.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.143(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.7224(5)
_cell_length_b                   22.7796(4)
_cell_length_c                   29.467(2)
_cell_measurement_reflns_used    51595
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      2.50
_cell_volume                     15579.8(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1454
_diffrn_reflns_av_sigmaI/netI    0.1095
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            170675
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    8.514
_exptl_absorpt_correction_T_max  0.9197
_exptl_absorpt_correction_T_min  0.4544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8866
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.667
_refine_diff_density_min         -2.304
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2206
_refine_ls_number_reflns         28505
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2605
_reflns_number_gt                16387
_reflns_number_total             28505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500832u_si_001.cif
_cod_data_source_block           DyZn8(picHA)8
_cod_depositor_comments
'Adding full bibliography for 4340046--4340049.cif.'
_cod_original_cell_volume        15579.6(12)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_original_formula_sum        'C60.50 H71.25 Dy N18 O30.25 Zn8'
_cod_database_code               4340047