Thermal Behavior, Crystal Structure, and Solid-State Transformation of Orthorhombic Mo-V Oxide under Nitrogen Flow or in Air.
Sadakane, Masahiro; Kodato, Katsunori; Yasuda, Nobuhiro; Ishikawa, Satoshi; Ueda, Wataru; ACS omega 4 (2019) 13165–13171; doi:10.1021/acsomega.9b01212

data_4514981
_publ_section_title
;
 Thermal Behavior, Crystal Structure, and Solid-State Transformation of
 Orthorhombic Mo-V Oxide under Nitrogen Flow or in Air.
;
_journal_issue                   8
_journal_name_full               'ACS omega'
_journal_page_first              13165
_journal_page_last               13171
_journal_paper_doi               10.1021/acsomega.9b01212
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'Mo7.66 O30.85 V2.82'
_chemical_formula_sum            'Mo7.66 O30.85 V2.82'
_chemical_formula_weight         1372.26
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           32
_space_group_name_Hall           'P 2 -2ab'
_space_group_name_H-M_alt        'P b a 2'
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0912(4)
_cell_length_b                   26.5514(5)
_cell_length_c                   3.97924(7)
_cell_measurement_reflns_used    15426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.026
_cell_measurement_theta_min      1.128
_cell_volume                     2228.38(7)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_radiation_source         'Synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.83077
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            15426
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        29.898
_diffrn_reflns_theta_max         30.026
_diffrn_reflns_theta_min         1.128
_exptl_absorpt_coefficient_mu    8.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.090
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2534
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.0008
_exptl_crystal_size_min          0.0008
_refine_diff_density_max         2.264
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.539
_refine_ls_abs_structure_details
;
 Flack x determined using 932 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3637
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+94.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                2917
_reflns_number_total             3637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01212_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4514981
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              67546
_shelx_hkl_checksum              51759