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_7055817
_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     Pb3[P2W18O62]*14.5HCON(CH3)2*1.3H2O
_chemical_formula_sum            'C43.5 H104.1 N14.5 O77.8 P2 Pb3 W18'
_chemical_formula_weight         6068.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.4927(6)
_cell_length_b                   17.8801(6)
_cell_length_c                   25.0895(6)
_cell_measurement_reflns_used    14838
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.3170
_cell_measurement_theta_min      3.5690
_cell_volume                     12333.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40347
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    20.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             10788
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.469
_refine_diff_density_min         -2.962
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         12988
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0307P)^2^+280.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10172
_reflns_number_total             12988
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6nj02155g2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7055816--7055817.cif.'
_cod_original_formula_sum        'C43.50 H104.10 N14.50 O77.80 P2 Pb3 W18'
_cod_database_code               7055817
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.188
_shelx_estimated_absorpt_t_max   0.488
_shelx_res_checksum              23952