Supramolecular interaction-induced assemblies of polyanions and 2-aminopyridinium in two polyoxometalate-based hybrids
Duan, Fengxue; Liu, Xiaoting; Xu, Wei; Tao, Yanchun; Li, Bao; Wu, Lixin; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618012548

data_2021272
_publ_section_title
;
 Supramolecular interaction-induced assemblies of polyanions and
 2-aminopyridinium in two polyoxometalate-based hybrids
;
_journal_coeditor_code           JR3004
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618012548
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'(C5 H7 N2)2 [Ni Mo6 O16 (C5 H9 O3)2 (O H)2], 4H2 O'
_chemical_formula_moiety         '2(C5 H7 N2 +), C10 H20 Mo6 Ni O24 2-, 4(H2 O)'
_chemical_formula_sum            'C20 H42 Mo6 N4 Ni O28'
_chemical_formula_weight         1420.92
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                85.653(5)
_cell_angle_beta                 77.403(5)
_cell_angle_gamma                83.439(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1173(11)
_cell_length_b                   10.3631(14)
_cell_length_c                   10.7022(15)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.13
_cell_volume                     979.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32003
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.854
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            light-green
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.444
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0225P)^2^+0.9013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0530
_reflns_number_gt                3785
_reflns_number_total             4483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3004sup1.cif
_cod_data_source_block           compound_II
_cod_database_code               2021272
_cod_database_fobs_code          2021272
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.793
_shelx_hkl_checksum              49660
_shelx_res_checksum              22982