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_4340048
_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
;
 Dy2Zn9(C10H8N2O2)10(C5H5N)10(C6H6)4.25(H2O)4.75(OH)2(NO3)1.25(Cl)0.7
;
_chemical_formula_sum            'C175.5 H167 Cl0.75 Dy2 N31.25 O30.5 Zn9'
_chemical_formula_weight         4141.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.512(5)
_cell_angle_beta                 102.150(5)
_cell_angle_gamma                113.693(5)
_cell_formula_units_Z            2
_cell_length_a                   20.445(5)
_cell_length_b                   21.830(5)
_cell_length_c                   22.271(5)
_cell_measurement_reflns_used    122620
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.10
_cell_volume                     8779(4)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0936
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            235204
_diffrn_reflns_theta_full        68.30
_diffrn_reflns_theta_max         68.30
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    6.544
_exptl_absorpt_correction_T_max  0.8279
_exptl_absorpt_correction_T_min  0.2915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4195
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.514
_refine_diff_density_min         -3.124
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2596
_refine_ls_number_reflns         31589
_refine_ls_number_restraints     1952
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                26961
_reflns_number_total             31589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500832u_si_001.cif
_cod_data_source_block           Dy2Zn9(quinHA)10
_cod_depositor_comments
'Adding full bibliography for 4340046--4340049.cif.'
_cod_original_formula_sum        'C175.50 H167 Cl0.75 Dy2 N31.25 O30.50 Zn9'
_cod_database_code               4340048