Polyoxovanadates: High-Nuclearity Spin Clusters with Interesting Host-Guest Systems and Different Electron Populations. Synthesis, Spin Organization, Magnetochemistry, and Spectroscopic Studies
Achim Müller; Roberta Sessoli; Erich Krickemeyer; Hartmut Bögge; Jochen Meyer; Dante Gatteschi; Luca Pardi; Jörg Westphal; Kai Hovemeier; Ralf Rohlfing; Joachim Döring; Frank Hellweg; Christian Beugholt; Marc Schmidtmann; Inorganic Chemistry 36 (1997) 5239–5250; doi:10.1021/ic9703641

data_4323651
_publ_section_title
;
 Polyoxovanadates: High-Nuclearity Spin Clusters with Interesting
 Host-Guest Systems and Different Electron Populations. Synthesis, Spin
 Organization, Magnetochemistry, and Spectroscopic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5239
_journal_page_last               5250
_journal_paper_doi               10.1021/ic9703641
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'H49 K9 N8 O57 V18'
_chemical_formula_weight         2342.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.317(2)
_cell_length_b                   13.317(2)
_cell_length_c                   36.435(10)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14.26
_cell_measurement_theta_min      3.79
_cell_volume                     6461(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       R3m/V
_diffrn_measurement_method       omega-scan
_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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6861
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  0.149
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown-black
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             4584
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.142
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.403
_refine_ls_goodness_of_fit_obs   1.467
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.512
_refine_ls_restrained_S_obs      1.467
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         0.045
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2196
_refine_ls_wR_factor_obs         0.1846
_reflns_number_observed          2702
_reflns_number_total             3560
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9703641_04.cif
_cod_data_source_block           jonny_1d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6461.5(22)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4323651