Syntheses, structures and magnetic properties of a family of heterometallic [Mn(II)(2)Mn(III)(2)Ln(III)(2)] clusters.
Liu, Jinying; Ma, Chengbing; Chen, Hui; Hu, Mingqiang; Wen, Huimin; Cui, Honghua; Song, Xiaowei; Chen, Changneng; Dalton transactions (Cambridge, England : 2003) 42 (2013) 2423–2430; doi:10.1039/c2dt32269b

data_7020872
_publ_section_title
;
 Syntheses, structures and magnetic properties of a family of
 heterometallic [Mn(II)(2)Mn(III)(2)Ln(III)(2)] clusters.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2423
_journal_page_last               2430
_journal_paper_doi               10.1039/c2dt32269b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C62 H118 Mn4 N2 Nd2 O28'
_chemical_formula_sum            'C62 H118 Mn4 N2 Nd2 O28'
_chemical_formula_weight         1847.82
_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

The four tert-butyl groups were each disordered into two positions
with occupancies of 66/34,60/40,60/40,60/40, 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 four tert-butyl groups
were restrained by using DFIX.

All the hydrogens were added geometrically. The singly-deprotonated
triethanolamine ligands (H2tea C) were confirmed by the charge
consideration and bond-valence-sum (BVS) calculations, but no
difference fourier peak was found to be suitable for the definition
of the proton of H2tea- anions, and these four hydrogens were
calculated in the reported formula.
;
_cell_angle_alpha                93.20
_cell_angle_beta                 109.563(3)
_cell_angle_gamma                108.359(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8240(9)
_cell_length_b                   12.1223(7)
_cell_length_c                   16.2567(11)
_cell_measurement_reflns_used    2786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4934
_cell_measurement_theta_min      3.1149
_cell_volume                     2049.7(2)
_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 14.6306
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14955
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         6925
_refine_ls_number_restraints     479
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0700P)^2^+0.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                6439
_reflns_number_total             6925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32269b.txt
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7020872