The first heterometallic examples of 3d-4f heptanuclear [Mn(II)(3)Ln(III)(4)] complexes with planar disc-like cores and diverse magnetic properties.
Liu, Jinying; Ma, Chengbing; Chen, Hui; Hu, Mingqiang; Wen, Huimin; Cui, Honghua; Chen, Changneng; Dalton transactions (Cambridge, England : 2003) 42 (2013) 3787–3790; doi:10.1039/c3dt32985b

data_7021043
_publ_section_title
;
 The first heterometallic examples of 3d-4f heptanuclear
 [Mn(II)(3)Ln(III)(4)] complexes with planar disc-like cores and diverse
 magnetic properties.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3787
_journal_page_last               3790
_journal_paper_doi               10.1039/c3dt32985b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C72 H138 Mn3 N2 Nd4 O33'
_chemical_formula_sum            'C72 H138 Mn3 N2 Nd4 O33'
_chemical_formula_weight         2301.62
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

The two tert-butyl groups were each disordered into two positions
with occupancies of 71/29,52/48, respectively,
and the temperature factors of all atoms were restrained by using
the command DELU/SIMU/ISOR. The subsequent refinement gave good ellipsoid plot.
The bond lengths and bond angles of those two tert-butyl groups
were restrained by using DFIX.
All the hydrogens were added geometrically. The terminal H2O ligand
were confirmed by the charge consideration and bond-valence-sum (BVS) calculations,
but O6 atoms lies in a special location (O(6)on threefold axis),
and may involve in some form of disorde,we failed to added the hydrogens on them,
and these six hydrogens were calculated in the reported formula.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.9410(6)
_cell_length_b                   17.9410(6)
_cell_length_c                   57.790(5)
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.1960
_cell_volume                     16109.3(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            32266
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6942
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
;
_refine_diff_density_max         2.256
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+101.3595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                2816
_reflns_number_total             3150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32985b.txt
_cod_data_source_block           1
_cod_original_cell_volume        16109.2(17)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7021043