Effects of the Central Lanthanide Ion Crystal Radius on the 15-MCCuII(N)pheHA-5 Structure
Curtis M. Zaleski; Choong-Sun Lim; Annabel D. Cutland-Van Noord; Jeff W. Kampf; Vincent L. Pecoraro; Inorganic Chemistry 50 (2011) 7707–7717; doi:10.1021/ic200740h

data_4325899
_publ_section_title
;
 Effects of the Central Lanthanide Ion Crystal Radius on the
 15-MCCuII(N)pheHA-5 Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7707
_journal_page_last               7717
_journal_paper_doi               10.1021/ic200740h
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H76 Ce Cu5 N13 O32'
_chemical_formula_structural
;
Ce1 Cu5 (C9 H10 N2 O2)5 (N1 O3)3 (H2 O1)13
;
_chemical_formula_sum            'C45 H76 Ce Cu5 N13 O32'
_chemical_formula_weight         1769.01
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.251(3)
_cell_length_b                   15.251(3)
_cell_length_c                   48.494(19)
_cell_measurement_reflns_used    2043
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      3.40
_cell_volume                     9768(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            80928
_diffrn_reflns_theta_full        29.67
_diffrn_reflns_theta_max         29.67
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    2.387
_exptl_absorpt_correction_T_max  0.5155
_exptl_absorpt_correction_T_min  0.3285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         17947
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0000P)^2^+71.0058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                17029
_reflns_number_total             17947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200740h_si_001_03.cif
_cod_data_source_block           Ce-1
_cod_original_cell_volume        9769(5)
_cod_database_code               4325899