Synthesis and characterization of multinuclear manganese-containing tungstosilicates.
Al-Oweini, Rami; Bassil, Bassem S.; Friedl, Jochen; Kottisch, Veronika; Ibrahim, Masooma; Asano, Marie; Keita, Bineta; Novitchi, Ghenadie; Lan, Yanhua; Powell, Annie; Stimming, Ulrich; Kortz, Ulrich; Inorganic chemistry 53 (2014) 5663–5673; doi:10.1021/ic500425c

data_4338449
_publ_section_title
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 Synthesis and characterization of multinuclear manganese-containing
 tungstosilicates.
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_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5663
_journal_page_last               5673
_journal_paper_doi               10.1021/ic500425c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H39 K4.5 Mn3 Na2.5 O55 Si W9'
_chemical_formula_weight         3000.29
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.3104(4)
_cell_length_b                   12.3104(4)
_cell_length_c                   52.317(2)
_cell_measurement_reflns_used    9150
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.46
_cell_volume                     6866.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.792
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.792
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            66070
_diffrn_reflns_point_group_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.254
_diffrn_reflns_theta_min         3.505
_exptl_absorpt_coefficient_mu    23.908
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.354
_exptl_crystal_description       plate
_exptl_crystal_F_000             8082
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.646
_exptl_transmission_factor_min   0.064
_refine_diff_density_max         2.123
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+850.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1690
_reflns_number_total             2197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500425c_si_002.cif
_cod_data_source_block           r-3
_cod_depositor_comments
'Adding full bibliography for 4338445--4338449.cif.'
_cod_original_cell_volume        6866.2(5)
_cod_original_formula_sum        'H39 K4.50 Mn3 Na2.50 O55 Si W9'
_cod_database_code               4338449
_shelx_estimated_absorpt_t_min   0.064
_shelx_estimated_absorpt_t_max   0.646
_plat015_alert_5_a
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PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF 
RESPONSE: The new SHELX package (2011 and after) includes
the hkl file in the cif file. For our compounds however, 
due to the very large number of reflections, 
the size of the cif file would become too large. 
Therefore, we usually delete the hkl part.
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