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_4334637
_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         'C80 H80 N20 Ni6 O26'
_chemical_formula_sum            'C98.75 H85.25 N10.88 Ni5 O19.25'
_chemical_formula_weight         2025.83
_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                85.346(6)
_cell_angle_beta                 85.445(6)
_cell_angle_gamma                85.262(6)
_cell_formula_units_Z            2
_cell_length_a                   13.1078(2)
_cell_length_b                   15.7214(3)
_cell_length_c                   21.3430(15)
_cell_measurement_reflns_used    48929
_cell_measurement_temperature    358(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.10
_cell_volume                     4357.0(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      358(2)
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            127732
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.7310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       needle
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.940
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         15677
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0715
_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^)+(0.1249P)^2^+0.9506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                11958
_reflns_number_total             15677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302831u_si_001_3.cif
_cod_data_source_block           Ni5(quinHA)4
_cod_database_code               4334637