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_4342097
_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, 36(H2O)'
_chemical_formula_sum            'H41 Mo10 O76 P V2'
_chemical_formula_weight         2349.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.748(3)
_cell_length_b                   12.745(3)
_cell_length_c                   18.027(4)
_cell_measurement_reflns_used    12985
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2928.9(12)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor)'
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21705
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         3.197
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.664
_exptl_crystal_description       piece
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.027
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5848
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1346P)^2^+18.2029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4653
_reflns_number_total             5848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502541b_si_006.cif
_cod_data_source_block           n495h
_cod_depositor_comments
'Adding full bibliography for 4342097--4342101.cif.'
_cod_original_cell_volume        2928.9(10)
_cod_database_code               4342097
_shelx_estimated_absorpt_t_min   0.630
_shelx_estimated_absorpt_t_max   0.701
_shelxl_version_number           2013-4
_shelx_res_checksum              18991
_shelx_hkl_checksum              19054