A Mixed 3d-4f 14-Metallacrown-5 Complex That Displays Slow Magnetic Relaxation through Geometric Control of Magnetoanisotropy
Thaddeus T. Boron; Jeff W. Kampf; Vincent L. Pecoraro; Inorganic Chemistry 49 (2010) 9104–9106; doi:10.1021/ic101121d

data_4316787
_publ_section_title
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 A Mixed 3d-4f 14-Metallacrown-5 Complex That Displays Slow Magnetic
 Relaxation through Geometric Control of Magnetoanisotropy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9104
_journal_page_last               9106
_journal_paper_doi               10.1021/ic101121d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C66 H64 Mn4 N14 O24 Tb2, C3 H7 N O, 2(C5 H5 N), H2 O'
_chemical_formula_sum            'C79 H83 Mn4 N17 O26 Tb2'
_chemical_formula_weight         2224.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.179(2)
_cell_length_b                   16.7785(14)
_cell_length_c                   18.5163(15)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.91
_cell_measurement_theta_min      4.01
_cell_volume                     9065.2(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2 v2009.1.0'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            97123
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.88
_exptl_absorpt_coefficient_mu    2.702
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of 
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.330
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         9679
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0615P)^2^+91.0392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                7579
_reflns_number_total             9679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101121d_si_002_2.cif
_cod_data_source_block           tb14mc5-compound(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        9065.1(13)
_cod_database_code               4316787