Redox Treatment of Orthorhombic Mo29V11O112and Relationships between Crystal Structure, Microporosity and Catalytic Performance for Selective Oxidation of Ethane
Ishikawa, Satoshi; Kobayashi, Daichi; Konya, Takeshi; Ohmura, Shunpei; Murayama, Toru; Yasuda, Nobuhiro; Sadakane, Masahiro; Ueda, Wataru; The Journal of Physical Chemistry C 119 (2015) 7195–; doi:10.1021/jp512848w

data_1518890
_publ_section_title
;
 Redox Treatment of Orthorhombic Mo29V11O112and Relationships between
 Crystal Structure, Microporosity and Catalytic Performance for Selective
 Oxidation of Ethane
;
_journal_issue                   13
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              7195
_journal_paper_doi               10.1021/jp512848w
_journal_volume                  119
_journal_year                    2015
_chemical_formula_moiety         'Mo7.62 O28 V2.38, 1.23(O)'
_chemical_formula_sum            'Mo7.62 O29.23 V2.38'
_chemical_formula_weight         1320.25
_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'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/4
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9864(5)
_cell_length_b                   26.4023(6)
_cell_length_c                   3.98755(9)
_cell_measurement_reflns_used    38157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.027
_cell_measurement_theta_min      1.449
_cell_volume                     2209.46(9)
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_refinement  'SHELXL-2014/4 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0828
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            38157
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        29.898
_diffrn_reflns_theta_max         30.027
_diffrn_reflns_theta_min         1.449
_exptl_absorpt_coefficient_mu    7.986
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.969
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2435
_exptl_crystal_size_max          0.0944
_exptl_crystal_size_mid          0.0008
_exptl_crystal_size_min          0.0008
_refine_diff_density_max         1.615
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details
;
 Flack x determined using 1407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4016
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0296P)^2^+24.6648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3714
_reflns_number_total             4016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp512848w_si_001.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 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 1518890.cif.
;
_cod_database_code               1518890
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014/4
_shelx_res_checksum              98549
_shelx_hkl_checksum              56551