data_shelx

_audit_update_record
;
2020-03-03 # Formatted by publCIF

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# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents

 section 
;
Introduction
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;

;
 section 
;
Experimental
; 
;

;
 subsection 
;
Synthesis and crystallization
; 
;

;
 subsection 
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;

 section 
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Results and discussion
; 
;

;
# publcif _publ_body_element loop end
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Mo0.55 O2 V0.45' 
_chemical_formula_weight          107.79

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'V'  'V'   0.3005   0.5294
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo'  'Mo'  -1.6832   0.6857
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            69
_space_group_name_H-M_alt         'F m m m'
_space_group_name_Hall            '-F 2 2'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'x, y+1/2, z+1/2'
 '-x, -y+1/2, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x, -y+1/2, -z+1/2'
 'x+1/2, y, z+1/2'
 '-x+1/2, -y, z+1/2'
 '-x+1/2, y, -z+1/2'
 'x+1/2, -y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x, y, -z'
 'x, -y, z'
 '-x, y, z'
 '-x, -y+1/2, -z+1/2'
 'x, y+1/2, -z+1/2'
 'x, -y+1/2, z+1/2'
 '-x, y+1/2, z+1/2'
 '-x+1/2, -y, -z+1/2'
 'x+1/2, y, -z+1/2'
 'x+1/2, -y, z+1/2'
 '-x+1/2, y, z+1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 
_cell_length_a                    13.3365(9)
_cell_length_b                    13.3352(10)
_cell_length_c                    5.6785(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1009.89(12)
_cell_formula_units_Z             32
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     29677
_cell_measurement_theta_min       41.97
_cell_measurement_theta_max       42.59
 
_exptl_crystal_description        plate
_exptl_crystal_colour             metallic-blusih-black
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     5.671          
_exptl_crystal_F_000              1584
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.16
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     8.577
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.7247
_exptl_absorpt_correction_T_max   1.3270
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Rigaku XtaLAB Syngergy-R'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             29677
_diffrn_reflns_av_unetI/netI      0.0179
_diffrn_reflns_av_R_equivalents   0.0931
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        26
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.055
_diffrn_reflns_theta_max          44.976
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              1186
_reflns_number_gt                 954
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0932P)²+7.7390P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_number_reflns          1186
_refine_ls_number_parameters      47
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0678
_refine_ls_R_factor_gt            0.0643
_refine_ls_wR_factor_ref          0.2011
_refine_ls_wR_factor_gt           0.1970
_refine_ls_goodness_of_fit_ref    1.248
_refine_ls_restrained_S_all       1.248
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
V1 V 0.000000 0.000000 0.72902(13) 0.0175(2) Uani 0.48(2) 4 d S T P . .
V2 V 0.250000 -0.250000 0.750000 0.0230(3) Uani 0.48(2) 4 d S T P . .
V3 V 0.000000 -0.24464(6) 1.000000 0.0208(2) Uani 0.43(2) 4 d S T P . .
V4 V 0.24884(7) 0.000000 1.000000 0.0247(2) Uani 0.40(2) 4 d S T P . .
Mo1 Mo 0.000000 0.000000 0.72902(13) 0.0175(2) Uani 0.52(2) 4 d S T P . .
Mo2 Mo 0.250000 -0.250000 0.750000 0.0230(3) Uani 0.52(2) 4 d S T P . .
Mo3 Mo 0.000000 -0.24464(6) 1.000000 0.0208(2) Uani 0.57(2) 4 d S T P . .
Mo4 Mo 0.24884(7) 0.000000 1.000000 0.0247(2) Uani 0.60(2) 4 d S T P . .
O1 O 0.000000 -0.0970(3) 1.000000 0.0183(7) Uani 1 4 d S T P . .
O2 O 0.2494(3) 0.1484(3) 1.000000 0.0218(6) Uani 1 2 d S T P . .
O3 O -0.1451(2) 0.000000 0.7470(6) 0.0157(5) Uani 1 2 d S T P . .
O4 O 0.1050(2) -0.250000 0.750000 0.0160(5) Uani 1 2 d S T P . .
O5 O 0.000000 -0.3930(4) 1.000000 0.0226(8) Uani 1 4 d S T P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
V1 O5 1.931(4) 21_546 ?
V1 O5 1.931(4) 5_554 ?
V1 O3 1.937(3) 2 ?
V1 O3 1.937(3) . ?
V1 O1 2.010(3) . ?
V1 O1 2.011(3) 17_557 ?
V1 V1 2.6010(15) 17_556 ?
V1 V1 3.0775(15) 17_557 ?
V2 O4 1.934(3) . ?
V2 O4 1.934(3) 14_545 ?
V2 O2 1.962(3) 19 ?
V2 O2 1.962(3) 5_544 ?
V2 O2 1.962(3) 15_547 ?
V2 O2 1.962(3) 25_556 ?
V2 V2 2.83925(16) 29_546 ?
V2 V2 2.83925(14) 29_547 ?
V3 O1 1.968(5) . ?
V3 O5 1.978(6) . ?
V3 O4 1.995(2) 21_546 ?
V3 O4 1.995(2) 18_557 ?
V3 O4 1.995(2) 6_545 ?
V3 O4 1.995(2) . ?
V3 V3 2.84285(17) 21_546 ?
V3 V3 2.84285(18) 21_547 ?
V4 O2 1.979(4) 19 ?
V4 O2 1.979(4) . ?
V4 O3 1.992(3) 9 ?
V4 O3 1.992(3) 26_556 ?
V4 O3 1.995(3) 2 ?
V4 O3 1.995(3) 17_557 ?
V4 V4 2.83942(15) 25_556 ?
V4 V4 2.83942(16) 25_557 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O5 V1 O5 95.3(2) 21_546 5_554 ?
O5 V1 O3 92.03(7) 21_546 2 ?
O5 V1 O3 92.03(7) 5_554 2 ?
O5 V1 O3 92.03(7) 21_546 . ?
O5 V1 O3 92.03(7) 5_554 . ?
O3 V1 O3 173.97(19) 2 . ?
O5 V1 O1 92.28(15) 21_546 . ?
O5 V1 O1 172.41(16) 5_554 . ?
O3 V1 O1 87.69(7) 2 . ?
O3 V1 O1 87.69(7) . . ?
O5 V1 O1 172.41(16) 21_546 17_557 ?
O5 V1 O1 92.28(15) 5_554 17_557 ?
O3 V1 O1 87.69(7) 2 17_557 ?
O3 V1 O1 87.69(7) . 17_557 ?
O1 V1 O1 80.1(2) . 17_557 ?
O5 V1 V1 47.66(12) 21_546 17_556 ?
O5 V1 V1 47.66(12) 5_554 17_556 ?
O3 V1 V1 93.02(10) 2 17_556 ?
O3 V1 V1 93.02(10) . 17_556 ?
O1 V1 V1 139.94(10) . 17_556 ?
O1 V1 V1 139.94(10) 17_557 17_556 ?
O5 V1 V1 132.34(12) 21_546 17_557 ?
O5 V1 V1 132.34(12) 5_554 17_557 ?
O3 V1 V1 86.98(10) 2 17_557 ?
O3 V1 V1 86.98(10) . 17_557 ?
O1 V1 V1 40.06(10) . 17_557 ?
O1 V1 V1 40.06(10) 17_557 17_557 ?
V1 V1 V1 180.0 17_556 17_557 ?
O4 V2 O4 180.0 . 14_545 ?
O4 V2 O2 89.76(12) . 19 ?
O4 V2 O2 90.24(12) 14_545 19 ?
O4 V2 O2 89.76(12) . 5_544 ?
O4 V2 O2 90.24(12) 14_545 5_544 ?
O2 V2 O2 179.5(2) 19 5_544 ?
O4 V2 O2 90.24(12) . 15_547 ?
O4 V2 O2 89.76(12) 14_545 15_547 ?
O2 V2 O2 87.31(17) 19 15_547 ?
O2 V2 O2 92.69(17) 5_544 15_547 ?
O4 V2 O2 90.24(12) . 25_556 ?
O4 V2 O2 89.76(12) 14_545 25_556 ?
O2 V2 O2 92.69(17) 19 25_556 ?
O2 V2 O2 87.31(17) 5_544 25_556 ?
O2 V2 O2 179.5(2) 15_547 25_556 ?
O4 V2 V2 90.0 . 29_546 ?
O4 V2 V2 90.0 14_545 29_546 ?
O2 V2 V2 136.35(8) 19 29_546 ?
O2 V2 V2 43.65(8) 5_544 29_546 ?
O2 V2 V2 136.35(8) 15_547 29_546 ?
O2 V2 V2 43.65(8) 25_556 29_546 ?
O4 V2 V2 90.0 . 29_547 ?
O4 V2 V2 90.0 14_545 29_547 ?
O2 V2 V2 43.65(8) 19 29_547 ?
O2 V2 V2 136.35(8) 5_544 29_547 ?
O2 V2 V2 43.65(8) 15_547 29_547 ?
O2 V2 V2 136.35(8) 25_556 29_547 ?
V2 V2 V2 180.0 29_546 29_547 ?
O1 V3 O5 180.0 . . ?
O1 V3 O4 92.05(2) . 21_546 ?
O5 V3 O4 87.95(2) . 21_546 ?
O1 V3 O4 92.05(2) . 18_557 ?
O5 V3 O4 87.95(2) . 18_557 ?
O4 V3 O4 175.89(5) 21_546 18_557 ?
O1 V3 O4 92.05(2) . 6_545 ?
O5 V3 O4 87.95(2) . 6_545 ?
O4 V3 O4 90.72(12) 21_546 6_545 ?
O4 V3 O4 89.13(12) 18_557 6_545 ?
O1 V3 O4 92.05(2) . . ?
O5 V3 O4 87.95(2) . . ?
O4 V3 O4 89.13(12) 21_546 . ?
O4 V3 O4 90.72(12) 18_557 . ?
O4 V3 O4 175.89(5) 6_545 . ?
O1 V3 V3 92.88(3) . 21_546 ?
O5 V3 V3 87.12(3) . 21_546 ?
O4 V3 V3 44.57(6) 21_546 21_546 ?
O4 V3 V3 135.14(6) 18_557 21_546 ?
O4 V3 V3 135.14(6) 6_545 21_546 ?
O4 V3 V3 44.57(6) . 21_546 ?
O1 V3 V3 92.88(3) . 21_547 ?
O5 V3 V3 87.12(3) . 21_547 ?
O4 V3 V3 135.14(6) 21_546 21_547 ?
O4 V3 V3 44.57(6) 18_557 21_547 ?
O4 V3 V3 44.57(6) 6_545 21_547 ?
O4 V3 V3 135.14(6) . 21_547 ?
V3 V3 V3 174.23(6) 21_546 21_547 ?
O2 V4 O2 179.6(2) 19 . ?
O2 V4 O3 89.85(9) 19 9 ?
O2 V4 O3 89.85(9) . 9 ?
O2 V4 O3 89.85(9) 19 26_556 ?
O2 V4 O3 89.85(9) . 26_556 ?
O3 V4 O3 89.50(18) 9 26_556 ?
O2 V4 O3 90.14(8) 19 2 ?
O2 V4 O3 90.14(8) . 2 ?
O3 V4 O3 178.67(14) 9 2 ?
O3 V4 O3 89.18(12) 26_556 2 ?
O2 V4 O3 90.14(8) 19 17_557 ?
O2 V4 O3 90.14(8) . 17_557 ?
O3 V4 O3 89.18(12) 9 17_557 ?
O3 V4 O3 178.67(14) 26_556 17_557 ?
O3 V4 O3 92.15(18) 2 17_557 ?
O2 V4 V4 89.998(1) 19 25_556 ?
O2 V4 V4 89.998(1) . 25_556 ?
O3 V4 V4 134.12(10) 9 25_556 ?
O3 V4 V4 44.63(9) 26_556 25_556 ?
O3 V4 V4 44.55(9) 2 25_556 ?
O3 V4 V4 136.70(11) 17_557 25_556 ?
O2 V4 V4 89.998(1) 19 25_557 ?
O2 V4 V4 89.998(1) . 25_557 ?
O3 V4 V4 44.63(9) 9 25_557 ?
O3 V4 V4 134.12(10) 26_556 25_557 ?
O3 V4 V4 136.70(11) 2 25_557 ?
O3 V4 V4 44.55(9) 17_557 25_557 ?
V4 V4 V4 178.75(7) 25_556 25_557 ?
V3 O1 V1 130.06(10) . . ?
V3 O1 V1 130.06(10) . 17_557 ?
V1 O1 V1 99.9(2) . 17_557 ?
V2 O2 V2 92.69(17) 5 25_556 ?
V2 O2 V4 133.65(8) 5 . ?
V2 O2 V4 133.65(8) 25_556 . ?
V1 O3 V4 132.24(17) . 9_454 ?
V1 O3 V4 136.94(18) . 17_557 ?
V4 O3 V4 90.82(12) 9_454 17_557 ?
V2 O4 V3 134.57(6) . 21_546 ?
V2 O4 V3 134.57(6) . . ?
V3 O4 V3 90.87(12) 21_546 . ?
V1 O5 V1 84.7(2) 21_546 5_545 ?
V1 O5 V3 137.66(12) 21_546 . ?
V1 O5 V3 137.66(12) 5_545 . ?
 
_refine_diff_density_max    2.339
_refine_diff_density_min   -3.147
_refine_diff_density_rms    0.402


loop_
_publcif_info_cif.paper_type
 ?



_publcif_funding_html
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