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_4323653
_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            'Br H48 K9 N8 O56 V18'
_chemical_formula_weight         2405.19
_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                   13.201(2)
_cell_length_b                   13.201(2)
_cell_length_c                   36.491(7)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      14.38
_cell_measurement_theta_min      5.72
_cell_volume                     6359.2(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(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  0.1489
_diffrn_reflns_av_sigmaI/netI    0.1228
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7011
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.841
_exptl_absorpt_correction_T_max  0.104
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.512
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_goodness_of_fit_obs   1.198
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_restrained_S_obs      1.198
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_obs          0.0751
_refine_ls_shift/esd_max         0.040
_refine_ls_shift/esd_mean        0.006
_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         0.2461
_refine_ls_wR_factor_obs         0.1919
_reflns_number_observed          2075
_reflns_number_total             3505
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9703641_06.cif
_cod_data_source_block           vabro_2b
_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_sg_symbol_H-M      'P 4/n c c'
_cod_original_formula_sum        'H48 Br K9 N8 O56 V18'
_cod_database_code               4323653