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_4323664
_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            'C0 H49 Na6 O67 V19'
_chemical_formula_weight         2227.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 97.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.488(9)
_cell_length_b                   15.073(7)
_cell_length_c                   18.936(8)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     5796(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5433
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.553
_exptl_crystal_F_000             4352
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.380
_refine_ls_goodness_of_fit_obs   1.462
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5413
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.458
_refine_ls_restrained_S_obs      1.462
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_obs          0.0747
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.001
_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         0.2147
_refine_ls_wR_factor_obs         0.1927
_reflns_number_observed          4395
_reflns_number_total             6320
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9703641_17.cif
_cod_data_source_block           sovt_8
_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        5795.6(44)
_cod_database_code               4323664