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_7020877
_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 Dy2 Mn4 N2 O28'
_chemical_formula_sum            'C62 H118 Dy2 Mn4 N2 O28'
_chemical_formula_weight         1884.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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 disordered into two positions
with occupancies of 60/40,70/30,64/36,54/46 respectively,
and the temperature factors of all atoms were restrained by using
command DELU/SIMU. The following refinement gave good ellipsoid plot.

The bond lengths and bond angles of those four tert. butyl cations
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
different diffraction density was found suitable for the definition
of the proton of H2tea- cations , and these protons were calculated
in the reported formula.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.085(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.5402(11)
_cell_length_b                   11.4633(4)
_cell_length_c                   22.0523(13)
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5244
_cell_measurement_theta_min      2.3224
_cell_volume                     4079.0(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43364
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  0.6367
_exptl_absorpt_correction_T_min  0.3422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         9330
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0413
_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^+4.9692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                8405
_reflns_number_total             9330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32269b.txt
_cod_data_source_block           compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_H-M      P2(1)/n
_cod_database_code               7020877