Insight into the reactivity of in situ formed {(NbO2)3SiW9}: synthesis, structure, and solution properties of a trimeric polytungstosilicate trapping a {MnNb9} core.
Wang, Haiying; Liang, Zhijie; Wang, Yaya; Zhang, Dongdi; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15236–15241; doi:10.1039/c6dt02252a

data_7040323
_publ_section_title
;
 Insight into the reactivity of in situ formed {(NbO2)3SiW9}: synthesis,
 structure, and solution properties of a trimeric polytungstosilicate
 trapping a {MnNb9} core.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15236
_journal_page_last               15241
_journal_paper_doi               10.1039/c6dt02252a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.33(Cs30 Mn3 Na9 Nb27 O387 Si9 W81), 9(O)'
_chemical_formula_sum            'Cs10 H42 Mn Na3 Nb9 O138 Si3 W27'
_chemical_formula_weight         9587.75
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_audit_creation_date             2015-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.722(2)
_cell_length_b                   30.722
_cell_length_c                   16.0353(12)
_cell_measurement_reflns_used    4202
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.609
_cell_measurement_theta_min      2.30
_cell_volume                     13107.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22609
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.296
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.494
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1764 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.4483.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    3.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12489
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.313
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.304
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.669(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0654P)^2^+124.8428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4357
_reflns_number_total             5265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02252a1.cif
_cod_data_source_block           njy1
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-04

 Adding full bibliography for 7040323.cif.
;
_cod_original_cell_volume        13107(2)
_cod_database_code               7040323
_shelx_estimated_absorpt_t_max   0.149
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.331(18) 0.669(18)
2. Uiso/Uaniso restraints and constraints
Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
;
_shelx_res_checksum              51918
_shelx_hkl_checksum              61069
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'