Two nanoscale Nb containing polyoxometalates based on the {P2W15Nb3O62} clusters and Chromium Cations
Huang, Peng; Wang, Xinlong; He, De-Qing; Wu, Hai-Yang; Qin, Chao; Du, Meng; Lai, chao; Su, Zhong-Min; Dalton Trans.  (2017) –; doi:10.1039/C7DT02737K

data_7044082
_publ_section_title
;
 Two nanoscale Nb containing polyoxometalates based on the {P2W15Nb3O62}
 clusters and Chromium Cations
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02737K
_journal_year                    2017
_chemical_formula_moiety
'0.25(Cr12 Cs20 K16 Nb24 O588 P16 W120), 5(O)'
_chemical_formula_sum            'Cr3 Cs5 K4 Nb6 O196 P4 W30'
_chemical_formula_weight         10309.79
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2017-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2017-08-25 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.632(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.856(5)
_cell_length_b                   23.354(5)
_cell_length_c                   21.811(5)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     19066(6)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54424
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    19.705
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             18068
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.506
_refine_diff_density_min         -2.836
_refine_diff_density_rms         0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         16706
_refine_ls_number_restraints     1836
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+847.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8915
_reflns_number_total             16706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02737k2.cif
_cod_data_source_block           mm
_cod_database_code               7044082
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.110
_shelx_estimated_absorpt_t_min   0.088
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
O1 \\sim O1W \\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O4W \\sim O5
\\sim O5W \\sim O6 \\sim O6W \\sim O7 \\sim O8 \\sim O8W \\sim O9 \\sim O9W
\\sim O10 \\sim O10W \\sim O11 \\sim O12 \\sim O13 \\sim O13W \\sim O14 \\sim
O14W \\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21
\\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29
\\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37
\\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45
\\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim O50 \\sim O51 \\sim O52 \\sim O53
\\sim O54 \\sim O55 \\sim O56 \\sim O57 \\sim O58 \\sim O59 \\sim O60 \\sim O61
\\sim O62 \\sim O7W \\sim O11W \\sim O15W \\sim O12W: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03
Cs3B \\sim Cs3A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O8W) \\sim Ueq, Uanis(O14W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.004
Uanis(Cs1) \\sim Ueq, Uanis(K1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(K2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(Cs3A) \\sim Ueq, Uanis(Cs3B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
2. Others
 Fixed Sof: O13W(0.5) Cs3B(0.25) Cs3A(0.25)
;
_shelx_res_checksum              64103
_olex2_submission_special_instructions 'No special instructions were received'