Tuning of Magnetic Properties of Polynuclear Lanthanide(III)−Octacyanotungstate(V) Systems: Determination of Ligand-Field Parameters and Exchange Interaction
Przychodzeń, Paweł; Pełka, Robert; Lewiński, Krzysztof; Supel, Justyna; Rams, Michał; Tomala, Krzysztof; Sieklucka, Barbara; Inorganic Chemistry 46 (2007) 8924–8938; doi:10.1021/ic700795q

data_4333371
_publ_section_title
;
 Tuning of Magnetic Properties of Polynuclear
 Lanthanide(III)&#x2212;Octacyanotungstate(V) Systems:&#x00A0;
 Determination of Ligand-Field Parameters and Exchange Interaction
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8924
_journal_page_last               8938
_journal_paper_doi               10.1021/ic700795q
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'(C21 H31 N5 O5 Tm), (C8 N8 W), (C3 H7 N O), 4(H2 O)'
_chemical_formula_sum            'C32 H46 N14 O10 Tm W'
_chemical_formula_weight         1139.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.48
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.9810(2)
_cell_length_b                   20.2360(1)
_cell_length_c                   26.1510(2)
_cell_measurement_temperature    100(1)
_cell_volume                     17341.77(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with the \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            37243
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.751
_exptl_absorpt_correction_T_max  0.7636
_exptl_absorpt_correction_T_min  0.3298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN; Otwinowski & Minor, 1997'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8944
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.423
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.000065(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         19732
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+41.1327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                16377
_reflns_number_total             19732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700795qsup1.cif
_cod_data_source_block           pp31
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        17341.83(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4333371