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_4334636
_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            'C87.5 H75.9 B2 F8 N17.5 O10.2 Zn5'
_chemical_formula_weight         2036.23
_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                 93.190(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.048(4)
_cell_length_b                   23.873(3)
_cell_length_c                   18.784(3)
_cell_measurement_reflns_used    104052
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      1.75
_cell_volume                     8976(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX-II'
_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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18365
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.8068
_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            yellow
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       needle
_exptl_crystal_F_000             4148
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         18365
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0958P)^2^+11.0024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                12758
_reflns_number_total             18365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302831u_si_001_2.cif
_cod_data_source_block           Zn5(quinHA)4
_cod_original_formula_sum        'C87.50 H75.90 B2 F8 N17.50 O10.20 Zn5'
_cod_database_code               4334636