Complexes of non-lacunary Keggin- and Dawson-type polyoxometalates with Pb(ii): formation of 1D coordination polymers with different bonding modes
Udalova, Liubov I.; Adonin, Sergey A.; Abramov, Pavel A.; Korolkov, Ilya V.; Yunoshev, Alexander S.; Plyusnin, Pavel E.; Sokolov, Maxim N.; New J. Chem. 40 (2016) 9981–; doi:10.1039/C6NJ02155G

data_7055816
_publ_section_title
;
 Complexes of non-lacunary Keggin- and Dawson-type polyoxometalates with
 Pb(ii): formation of 1D coordination polymers with different bonding
 modes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              9981
_journal_paper_doi               10.1039/C6NJ02155G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_structural     Pb2[SiW12O40]*11HOCN(CH3)2
_chemical_formula_sum            'C33 H77 N11 O51 Pb2 Si W12'
_chemical_formula_weight         4092.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                94.2851(11)
_cell_angle_beta                 103.2466(10)
_cell_angle_gamma                102.5634(12)
_cell_formula_units_Z            2
_cell_length_a                   13.0771(7)
_cell_length_b                   14.1413(7)
_cell_length_c                   22.4997(9)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.42
_cell_volume                     3919.0(3)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
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_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
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_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.987
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_diffrn_source                   'sealed X-ray tube'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             3652
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_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.019
_refine_diff_density_min         -2.492
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0684
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_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^)+(0.0207P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13173
_reflns_number_total             17949
_reflns_threshold_expression     >2\s(I)
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_cod_data_source_block           lu
_cod_depositor_comments
'Adding full bibliography for 7055816--7055817.cif.'
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_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.353
_shelx_res_checksum              18701