 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_common             'kingsgateite'
_chemical_formula_sum
 'H0 Mo2 O11 Zr' 
_chemical_formula_weight          427.73

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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zr'  'Zr'  -2.9673   0.5597
 '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       tetragonal
_space_group_IT_number            110
_space_group_name_H-M_alt         'I 41 c d'
_space_group_name_Hall            'I 4bw -2c'
 
_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+1/2, -y+1/2, z+1/2'
 '-y, x+1/2, z+1/4'
 'y+1/2, -x, z+3/4'
 'x, -y, z+1/2'
 '-x+1/2, y+1/2, z'
 '-y, -x+1/2, z+3/4'
 'y+1/2, x, z+1/4'
 'x+1/2, y+1/2, z+1/2'
 '-x+1, -y+1, z+1'
 '-y+1/2, x+1, z+3/4'
 'y+1, -x+1/2, z+5/4'
 'x+1/2, -y+1/2, z+1'
 '-x+1, y+1, z+1/2'
 '-y+1/2, -x+1, z+5/4'
 'y+1, x+1/2, z+3/4'
 
_cell_length_a                    11.4626(16)
_cell_length_b                    11.4626(16)
_cell_length_c                    12.584(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1653.4(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     11769
_cell_measurement_theta_min       3.5460
_cell_measurement_theta_max       28.7520

_exptl_crystal_description        tablet
_exptl_crystal_colour             grey
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.689          
_exptl_crystal_F_000              1696
_exptl_transmission_factor_min    0.389
_exptl_transmission_factor_max    0.434
_exptl_crystal_size_max           0.035
_exptl_crystal_size_mid           0.030
_exptl_crystal_size_min           0.005
_exptl_absorpt_coefficient_mu     4.271
_shelx_estimated_absorpt_T_min    0.389
_shelx_estimated_absorpt_T_max    0.434
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.389
_exptl_absorpt_correction_T_max   0.434
_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   Dectris
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             13501
_diffrn_reflns_av_unetI/netI      0.0244
_diffrn_reflns_av_R_equivalents   0.0404
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.555
_diffrn_reflns_theta_max          29.571
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.987
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.987
_diffrn_reflns_point_group_measured_fraction_max   0.986
_diffrn_reflns_point_group_measured_fraction_full  0.980
_reflns_number_total              1159
_reflns_number_gt                 1159
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.903
_reflns_Friedel_fraction_max      0.980
_reflns_Friedel_fraction_full     0.972
 
_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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0911P)²+4.2024P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.0018(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 550 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.00(6)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1159
_refine_ls_number_parameters      68
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0453
_refine_ls_R_factor_gt            0.0453
_refine_ls_wR_factor_ref          0.1067
_refine_ls_wR_factor_gt           0.1067
_refine_ls_goodness_of_fit_ref    1.103
_refine_ls_restrained_S_all       1.103
_refine_ls_shift/su_max           0.000
_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
Zr Zr 0.500000 0.500000 0.28159(16) 0.0108(3) Uani 1 2 d S T P . .
Mo Mo 0.66375(5) 0.52379(6) 0.54984(9) 0.0124(3) Uani 1 1 d . . P . .
O1 O 0.6608(13) 0.6749(7) 0.5534(9) 0.020(2) Uani 1 1 d . . . . .
O2 O 0.6141(5) 0.4954(5) 0.4185(5) 0.0183(15) Uani 1 1 d . . . . .
O3 O 0.8194(6) 0.4944(8) 0.5399(9) 0.0190(16) Uani 1 1 d . . . . .
O4 O 0.500000 0.500000 0.6094(12) 0.013(3) Uani 1 2 d S T P . .
OH5 O 0.6786(5) 0.5072(7) 0.7176(8) 0.0182(17) Uani 1 1 d . . . . .
OW6 O 0.6590(12) 0.3249(7) 0.5740(9) 0.022(2) Uani 1 1 d . . . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Zr 0.0086(4) 0.0081(4) 0.0155(6) 0.000 0.000 0.0007(2)
Mo 0.0070(4) 0.0133(4) 0.0168(4) 0.0003(4) 0.0005(2) -0.00018(16)
O1 0.012(4) 0.009(3) 0.039(5) 0.003(4) -0.001(3) -0.005(2)
O2 0.012(3) 0.026(3) 0.017(2) -0.0045(19) -0.0016(19) -0.001(2)
O3 0.015(2) 0.018(3) 0.023(4) 0.002(3) -0.001(3) 0.001(3)
O4 0.005(3) 0.020(5) 0.014(7) 0.000 0.000 0.000(3)
OH5 0.010(3) 0.020(3) 0.025(5) -0.001(3) 0.000(3) -0.0027(19)
OW6 0.019(4) 0.007(3) 0.039(5) -0.003(3) -0.005(5) 0.002(2)
 
_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
Zr O3 2.074(7) 7_664 ?
Zr O3 2.074(7) 16_444 ?
Zr O2 2.164(6) . ?
Zr O2 2.164(6) 10_554 ?
Zr O4 2.167(14) 5_564 ?
Zr OH5 2.202(7) 14_544 ?
Zr OH5 2.202(7) 5_564 ?
Mo O1 1.733(8) . ?
Mo O2 1.778(7) . ?
Mo O3 1.820(7) . ?
Mo O4 2.040(5) . ?
Mo OH5 2.127(10) . ?
Mo OW6 2.301(9) . ?
 
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
O3 Zr O3 174.2(7) 7_664 16_444 ?
O3 Zr O2 88.0(3) 7_664 . ?
O3 Zr O2 87.4(4) 16_444 . ?
O3 Zr O2 87.4(4) 7_664 10_554 ?
O3 Zr O2 88.0(3) 16_444 10_554 ?
O2 Zr O2 74.5(3) . 10_554 ?
O3 Zr O4 92.9(3) 7_664 5_564 ?
O3 Zr O4 92.9(3) 16_444 5_564 ?
O2 Zr O4 142.76(17) . 5_564 ?
O2 Zr O4 142.76(17) 10_554 5_564 ?
O3 Zr OH5 90.6(3) 7_664 14_544 ?
O3 Zr OH5 91.6(3) 16_444 14_544 ?
O2 Zr OH5 148.7(3) . 14_544 ?
O2 Zr OH5 74.2(3) 10_554 14_544 ?
O4 Zr OH5 68.6(2) 5_564 14_544 ?
O3 Zr OH5 91.6(3) 7_664 5_564 ?
O3 Zr OH5 90.6(3) 16_444 5_564 ?
O2 Zr OH5 74.2(3) . 5_564 ?
O2 Zr OH5 148.7(3) 10_554 5_564 ?
O4 Zr OH5 68.6(2) 5_564 5_564 ?
OH5 Zr OH5 137.1(5) 14_544 5_564 ?
O1 Mo O2 101.6(4) . . ?
O1 Mo O3 101.9(5) . . ?
O2 Mo O3 102.5(4) . . ?
O1 Mo O4 96.1(5) . . ?
O2 Mo O4 91.3(4) . . ?
O3 Mo O4 154.5(4) . . ?
O1 Mo OH5 93.7(4) . . ?
O2 Mo OH5 158.8(3) . . ?
O3 Mo OH5 88.4(4) . . ?
O4 Mo OH5 72.4(4) . . ?
O1 Mo OW6 170.6(5) . . ?
O2 Mo OW6 86.2(4) . . ?
O3 Mo OW6 81.3(4) . . ?
O4 Mo OW6 78.3(4) . . ?
OH5 Mo OW6 77.4(4) . . ?
Mo O2 Zr 158.3(3) . . ?
Mo O3 Zr 167.5(5) . 15_654 ?
Mo O4 Mo 136.9(8) 10_554 . ?
Mo O4 Zr 111.6(4) 10_554 5_565 ?
Mo O4 Zr 111.6(4) . 5_565 ?
Mo OH5 Zr 107.0(3) . 5_565 ?
 
_refine_diff_density_max    5.495
_refine_diff_density_min   -2.132
_refine_diff_density_rms    0.526

