HP-MoO2: A High-Pressure Polymorph of Molybdenum Dioxide.
Lüdtke, Tobias; Wiedemann, Dennis; Efthimiopoulos, Ilias; Becker, Nils; Seidel, Stefan; Janka, Oliver; Pöttgen, Rainer; Dronskowski, Richard; Koch-Müller, Monika; Lerch, Martin; Inorganic chemistry 56 (2017) 2321–2327; doi:10.1021/acs.inorgchem.6b03067

data_4345369
_publ_section_title
;
 HP-MoO2: A High-Pressure Polymorph of Molybdenum Dioxide.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2321
_journal_page_last               2327
_journal_paper_doi               10.1021/acs.inorgchem.6b03067
_journal_volume                  56
_journal_year                    2017
_chemical_formula_iupac          'Mo O2(oP36)'
_chemical_formula_sum            'Mo O2'
_chemical_formula_weight         127.94
_chemical_name_common            'molydenum(IV) oxide - Hp'
_chemical_name_systematic        'molybdenum dioxide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-13
_audit_creation_method           'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   9.6921(3)
_cell_length_b                   8.4322(3)
_cell_length_c                   4.7188(2)
_cell_measurement_reflns_used    1627
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.366
_cell_measurement_theta_min      9.142
_cell_volume                     385.65(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond 3.2 (Brandenburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            'Agilent Atlas'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -112.00 -24.00   1.00   15.00    --  -41.43 -38.00 -60.00   88
  2  \w    -93.00  -2.00   1.00   15.00    --  -41.43 125.00-180.00   91
  3  \w    -66.00  24.00   1.00   15.00    --  -41.43  38.00 120.00   90
  4  \w     16.00  41.00   1.00   15.00    --   41.43-125.00-180.00   25
  5  \w     79.00 104.00   1.00   20.00    --  106.44  30.00 -90.00   25
  6  \w    113.00 138.00   1.00   20.00    --  106.44  30.00 -90.00   25
  7  \w     45.00 119.00   1.00   20.00    --  106.44 -61.00-150.00   74
  8  \w     77.00 157.00   1.00   20.00    --  106.44 125.00-120.00   80
  9  \w     93.00 118.00   1.00   20.00    --  106.44-125.00  60.00   25
 10  \w     74.00 138.00   1.00   20.00    --  106.44 -77.00 -90.00   64
 11  \w     79.00 115.00   1.00   20.00    --  106.44  61.00-150.00   36
 12  \w    128.00 154.00   1.00   20.00    --  106.44  61.00-150.00   26
 13  \w     34.00  79.00   1.00   20.00    --  106.44 -30.00 -90.00   45
 14  \w     86.00 123.00   1.00   20.00    --  106.44 -30.00 -90.00   37
 15  \w     34.00 108.00   1.00   20.00    --  106.44 -94.00-180.00   74
 16  \w     38.00 113.00   1.00   20.00    --  106.44-125.00 120.00   75
 17  \w     46.00 116.00   1.00   20.00    --  106.44 -15.00  60.00   70
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (Single Source)'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type
'CrysAlisPro convention (Paciorek et al., 1999)'
_diffrn_orient_matrix_UB_11      0.0292060000
_diffrn_orient_matrix_UB_12      -0.1585148000
_diffrn_orient_matrix_UB_13      -0.1508201000
_diffrn_orient_matrix_UB_21      0.0109184000
_diffrn_orient_matrix_UB_22      -0.0835461000
_diffrn_orient_matrix_UB_23      0.2894922000
_diffrn_orient_matrix_UB_31      -0.1558336000
_diffrn_orient_matrix_UB_32      -0.0356571000
_diffrn_orient_matrix_UB_33      -0.0077902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1931
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.263
_diffrn_reflns_theta_min         9.154
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Agilent Nova'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    78.438
_exptl_absorpt_correction_T_max  0.162
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)

Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid
 (Clark & Reid, 1995).

Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    6.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.402
_refine_ls_extinction_coef       0.0038(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                393
_reflns_number_total             403
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic6b03067_si_002.cif
_cod_data_source_block           MoO2
_cod_database_code               4345369
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              85270
_shelx_hkl_checksum              60758