A High-Nuclearity 3d/4f Metal Oxime Cluster: An Unusual Ni8Dy8 "Core-Shell" Complex from the Use of 2-Pyridinealdoxime
Constantina Papatriantafyllopoulou; Theocharis C. Stamatatos; Constantinos G. Efthymiou; Luis Cunha-Silva; Filipe A. Almeida Paz; Spyros P. Perlepes; George Christou; Inorganic Chemistry 49 (2010) 9743–9745; doi:10.1021/ic101581g

data_4316988
_publ_section_title
;
 A High-Nuclearity 3d/4f Metal Oxime Cluster: An Unusual Ni8Dy8
 "Core-Shell" Complex from the Use of 2-Pyridinealdoxime
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9743
_journal_page_last               9745
_journal_paper_doi               10.1021/ic101581g
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C351 H368 Cl10 Dy16 N114 Ni16 O137'
_chemical_formula_weight         12269.45
_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_date             '03 September 2010'
_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.813(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9726(17)
_cell_length_b                   33.018(2)
_cell_length_c                   64.448(5)
_cell_measurement_reflns_used    8190
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.24
_cell_volume                     46700(6)
_computing_cell_refinement       'APEX2 '
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXTL '
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi 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  0.1132
_diffrn_reflns_av_sigmaI/netI    0.1546
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            415585
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         0.69
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.7338
_exptl_absorpt_correction_T_min  0.5305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1997)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             24168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.177
_refine_diff_density_min         -5.761
_refine_diff_density_rms         0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5269
_refine_ls_number_reflns         107009
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1277P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                58432
_reflns_number_total             107009
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101581g_si_001.cif
_cod_data_source_block           Ni8Dy8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316988