Self-Assembly of Anionic Polyoxometalate-Organic Architectures Based on Lacunary Phosphomolybdates and Pyridyl Ligands.
Li, Chifeng; Mizuno, Noritaka; Yamaguchi, Kazuya; Suzuki, Kosuke; Journal of the American Chemical Society 141 (2019) 7687–7692; doi:10.1021/jacs.9b02541

data_4128235
_publ_section_title
;
 Self-Assembly of Anionic Polyoxometalate-Organic Architectures Based on
 Lacunary Phosphomolybdates and Pyridyl Ligands.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7687
_journal_page_last               7692
_journal_paper_doi               10.1021/jacs.9b02541
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C63 H15 Mo9 N6 O31 P'
_chemical_formula_weight         2246.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4306(2)
_cell_length_b                   21.7192(2)
_cell_length_c                   26.7317(3)
_cell_measurement_reflns_used    15828
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.460
_cell_measurement_theta_min      1.208
_cell_volume                     10700.64(19)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.133
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            15078
_diffrn_reflns_point_group_measured_fraction_full 0.511
_diffrn_reflns_point_group_measured_fraction_max 0.508
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.460
_diffrn_reflns_theta_min         1.208
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.323
_refine_diff_density_min         -2.240
_refine_diff_density_rms         0.422
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         15078
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1281P)^2^+15.9308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                14344
_reflns_number_total             15078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02541_si_002.cif
_cod_data_source_block           TBA-I
_cod_database_code               4128235
_shelxl_version_number           2014/6
_shelx_res_checksum              44599
_shelx_hkl_checksum              96163
_shelx_fab_checksum              4137