Solid-State Crystal-to-Crystal Phase Transitions and Reversible Structure-Temperature Behavior of Phosphovanadomolybdic Acid, H5PV2Mo10O40.
Barats-Damatov, Delina; Shimon, Linda J. W.; Feldman, Yishay; Bendikov, Tatyana; Neumann, Ronny; Inorganic chemistry 54 (2015) 628–634; doi:10.1021/ic502541b

data_4342101
_publ_section_title
;
 Solid-State Crystal-to-Crystal Phase Transitions and Reversible
 Structure-Temperature Behavior of Phosphovanadomolybdic Acid,
 H5PV2Mo10O40.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              628
_journal_page_last               634
_journal_paper_doi               10.1021/ic502541b
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'H5 Mo10 O40 P V2, 14 (H2O)'
_chemical_formula_sum            'H33 Mo10 O54 P V2'
_chemical_formula_weight         1989.51
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                60.8204(8)
_cell_angle_beta                 67.8345(8)
_cell_angle_gamma                70.3150(7)
_cell_formula_units_Z            2
_cell_length_a                   13.4705(2)
_cell_length_b                   13.9620(2)
_cell_length_c                   13.99670(10)
_cell_measurement_reflns_used    11602
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     2090.11(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor (1997)'
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor (1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18248
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.065
_diffrn_source                   sealed-tube
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_T_max  0.8445
_exptl_absorpt_correction_T_min  0.7211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor (1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.161
_exptl_crystal_description       piece
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.123
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1234P)^2^+5.6902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7024
_reflns_number_total             9538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502541b_si_003.cif
_cod_data_source_block           n489h
_cod_depositor_comments
'Adding full bibliography for 4342097--4342101.cif.'
_cod_database_code               4342101
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.844
_shelxl_version_number           2013-4
_shelx_res_checksum              9549
_shelx_hkl_checksum              43048