Synthesis, structure and magnetism of a S-shaped multi-iron substituted arsenotungstate containing a trivacant Keggin [B-α-AsVW9O34]9− and a hexavacant Keggin [α-AsVW6O26]11− fragments
Zhao, Junwei; Han, Qiuxia; Shi, Dongying; Chen, Lijuan; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Journal of Solid State Chemistry 184 (2011) 2756–2761; doi:10.1016/j.jssc.2011.08.016

data_1563178
_publ_section_title
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 Synthesis, structure and magnetism of a S-shaped multi-iron substituted
 arsenotungstate containing a trivacant Keggin [B-\a-AsVW9O34]9&#x2212;
 and a hexavacant Keggin [\a-AsVW6O26]11&#x2212; fragments
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_journal_issue                   10
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              2756
_journal_page_last               2761
_journal_paper_doi               10.1016/j.jssc.2011.08.016
_journal_volume                  184
_journal_year                    2011
_chemical_formula_sum            'C4 H52 As4 Fe8 N4 O130 W30'
_chemical_formula_weight         8498.48
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 113.05
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   30.369(11)
_cell_length_b                   21.530(10)
_cell_length_c                   11.891(5)
_cell_measurement_reflns_used    2553
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.38
_cell_volume                     7154(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1478
_diffrn_reflns_av_sigmaI/netI    0.2262
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17387
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    25.809
_exptl_absorpt_correction_T_max  0.0742
_exptl_absorpt_correction_T_min  0.0461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    3.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7408
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.356
_refine_diff_density_min         -4.705
_refine_diff_density_rms         0.582
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                2950
_reflns_number_total             6290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2011-184-2756.CIF
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

data item '_refine_ls_hydrogen_treatment' value 'CONSTR' was changed
to 'constr' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               1563178