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_4334635
_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_moiety
; 
 2(C49 H41 N13 O8 Zn5), 2.5(C F3 S O3), (C5 H5 N)
 1.5(O H), (C H4 O)2.25, (H2 O)7.5
;
_chemical_formula_sum            'C107.75 H112 F7.5 N27 O34.75 S2.5 Zn10'
_chemical_formula_weight         3217.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_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                83.760(6)
_cell_angle_beta                 89.320(6)
_cell_angle_gamma                74.143(5)
_cell_formula_units_Z            1
_cell_length_a                   13.9392(3)
_cell_length_b                   14.4645(3)
_cell_length_c                   19.5726(14)
_cell_measurement_reflns_used    37722
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      2.30
_cell_volume                     3773.0(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80841
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.7332
_exptl_absorpt_correction_T_min  0.6085
_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    1.416
_exptl_crystal_description       needle
_exptl_crystal_F_000             1633
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.258(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2147
_refine_ls_number_reflns         24956
_refine_ls_number_restraints     2719
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1704P)^2^+3.9857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2144
_reflns_number_gt                23643
_reflns_number_total             24956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302831u_si_001_1.cif
_cod_data_source_block           Zn5(picHA)4
_cod_original_formula_sum        'C107.75 H112 F7.50 N27 O34.75 S2.50 Zn10'
_cod_database_code               4334635