Isolation of Elusive Tetranuclear and Pentanuclear M(II)-Hydroximate Intermediates in the Assembly of Lanthanide [15-Metallacrown-5] Complexes
Joseph Jankolovits; Jeff W. Kampf; Vincent L. Pecoraro; Inorganic Chemistry 52 (2013) 5063–5076; doi:10.1021/ic302831u

data_4334638
_publ_contact_author             vlpec@umich.edu
_publ_section_title
;
 Isolation of Elusive Tetranuclear and Pentanuclear M(II)-Hydroximate
 Intermediates in the Assembly of Lanthanide [15-Metallacrown-5] Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5063
_journal_page_last               5076
_journal_paper_doi               10.1021/ic302831u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C26 H34 N6 O14 Zn4'
_chemical_formula_weight         916.15
_chemical_name_systematic
; 
 Zn4(picHA)2(acetate)4(dimethylformamide)2
;
_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                80.6810(10)
_cell_angle_beta                 77.5350(10)
_cell_angle_gamma                79.5470(10)
_cell_formula_units_Z            1
_cell_length_a                   7.9774(2)
_cell_length_b                   10.4943(3)
_cell_length_c                   10.6971(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.65
_cell_volume                     852.85(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34139
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.5992
_exptl_absorpt_correction_T_min  0.4438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0346P)^2^+0.3814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                4720
_reflns_number_total             5208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302831u_si_001_4.cif
_cod_data_source_block           Zn4(picHA)2(OAc)4
_cod_database_code               4334638