# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ce
_database_code_depnum_ccdc_archive 'CCDC 1886380'
_audit_update_record             
;
2019-01-25 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Cerium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         CeI4MoO15
_chemical_formula_sum            'Ce I4 Mo O15'
_chemical_formula_weight         983.66

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   6.9831(10)
_cell_length_b                   14.1056(19)
_cell_length_c                   7.0752(9)
_cell_angle_alpha                90
_cell_angle_beta                 115.325(4)
_cell_angle_gamma                90
_cell_volume                     629.94(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2890
_cell_measurement_theta_min      2.888
_cell_measurement_theta_max      27.580

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    5.186
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    14.448
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8628
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.888
_diffrn_reflns_theta_max         27.580
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2890
_reflns_number_gt                2871
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.994

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0165P)²+0.8522P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0088(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1336 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.120(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2890
_refine_ls_number_parameters     191
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0618
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.111
_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
Ce1 Ce -0.06725(10) 0.85913(4) 0.08863(9) 0.00592(17) Uani 1 1 d . . . . .
I1 I 0.75286(11) 0.27112(5) 0.34201(10) 0.00747(18) Uani 1 1 d . . . . .
I2 I 0.15673(11) 0.48767(5) 0.45058(11) 0.00595(17) Uani 1 1 d . . . . .
I3 I 0.53141(11) 0.76299(5) 0.26444(10) 0.00552(17) Uani 1 1 d . . . . .
I4 I 0.76355(11) 0.61184(5) 0.80807(10) 0.00585(18) Uani 1 1 d . . . . .
Mo1 Mo 0.59589(15) 0.52074(7) 0.29568(14) 0.0056(2) Uani 1 1 d . . . . .
O1 O 0.7642(14) 0.6182(6) 0.5482(12) 0.0077(16) Uani 1 1 d . . . . .
O2 O 0.2321(14) 0.4238(6) 0.6905(12) 0.0104(18) Uani 1 1 d . . . . .
O3 O 0.5229(14) 0.2580(7) 0.3928(13) 0.0128(17) Uani 1 1 d . . . . .
O4 O 0.7431(13) 0.5646(6) 0.1696(13) 0.0126(18) Uani 1 1 d . . . . .
O5 O 0.3013(15) 0.8348(6) 0.1538(13) 0.0124(17) Uani 1 1 d . . . . .
O6 O 0.3958(14) 0.4544(6) 0.1120(13) 0.0113(17) Uani 1 1 d . . . . .
O7 O 0.9599(14) 0.5196(6) 0.9100(13) 0.0123(17) Uani 1 1 d . U . . .
O8 O 0.7758(13) 0.4294(6) 0.4540(13) 0.0098(17) Uani 1 1 d . . . . .
O9 O 0.9366(14) 0.7103(6) 0.9158(13) 0.0113(18) Uani 1 1 d . U . . .
O10 O 0.3987(14) 0.6473(6) 0.1985(12) 0.0087(17) Uani 1 1 d . U . . .
O11 O 0.7463(14) 0.1399(6) 0.2630(15) 0.0130(18) Uani 1 1 d . . . . .
O12 O 0.4301(13) 0.5127(6) 0.4928(12) 0.0089(17) Uani 1 1 d . . . . .
O13 O 0.6081(13) 0.7677(6) 0.0482(11) 0.0086(16) Uani 1 1 d . . . . .
O14 O 0.9572(13) 0.2506(7) 0.5984(13) 0.0120(18) Uani 1 1 d . . . . .
O15 O 0.0926(14) 0.3885(6) 0.2719(13) 0.0125(18) Uani 1 1 d . . . . .


_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
Ce1 O7 2.382(9) 2_656 ?
Ce1 O9 2.435(9) 1_454 ?
Ce1 O5 2.437(10) . ?
Ce1 O2 2.478(8) 2_556 ?
Ce1 O6 2.510(9) 2 ?
Ce1 O15 2.515(8) 2 ?
Ce1 O13 2.516(8) 1_455 ?
Ce1 O14 2.526(9) 2_656 ?
I1 O14 1.788(8) . ?
I1 O3 1.799(8) . ?
I1 O11 1.929(8) . ?
I1 O8 2.352(9) . ?
I2 O2 1.791(8) . ?
I2 O15 1.808(9) . ?
I2 O12 1.836(8) . ?
I3 O5 1.773(9) . ?
I3 O13 1.826(7) . ?
I3 O10 1.836(9) . ?
I4 O9 1.784(9) . ?
I4 O7 1.802(9) . ?
I4 O1 1.843(7) . ?
Mo1 O6 1.721(9) . ?
Mo1 O4 1.738(9) . ?
Mo1 O8 1.813(8) . ?
Mo1 O1 2.160(8) . ?
Mo1 O12 2.163(8) . ?
Mo1 O10 2.178(9) . ?
O2 Ce1 2.478(8) 2_546 ?
O6 Ce1 2.510(9) 2_545 ?
O7 Ce1 2.382(9) 2_646 ?
O9 Ce1 2.435(9) 1_656 ?
O13 Ce1 2.516(8) 1_655 ?
O14 Ce1 2.526(9) 2_646 ?
O15 Ce1 2.515(8) 2_545 ?

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
O7 Ce1 O9 138.6(3) 2_656 1_454 ?
O7 Ce1 O5 80.1(3) 2_656 . ?
O9 Ce1 O5 74.7(3) 1_454 . ?
O7 Ce1 O2 83.0(3) 2_656 2_556 ?
O9 Ce1 O2 137.9(3) 1_454 2_556 ?
O5 Ce1 O2 132.1(3) . 2_556 ?
O7 Ce1 O6 72.8(3) 2_656 2 ?
O9 Ce1 O6 112.4(3) 1_454 2 ?
O5 Ce1 O6 144.9(3) . 2 ?
O2 Ce1 O6 66.5(3) 2_556 2 ?
O7 Ce1 O15 74.5(3) 2_656 2 ?
O9 Ce1 O15 69.2(3) 1_454 2 ?
O5 Ce1 O15 80.0(3) . 2 ?
O2 Ce1 O15 136.8(3) 2_556 2 ?
O6 Ce1 O15 71.8(3) 2 2 ?
O7 Ce1 O13 138.9(3) 2_656 1_455 ?
O9 Ce1 O13 72.8(3) 1_454 1_455 ?
O5 Ce1 O13 141.0(3) . 1_455 ?
O2 Ce1 O13 67.7(3) 2_556 1_455 ?
O6 Ce1 O13 69.4(3) 2 1_455 ?
O15 Ce1 O13 107.5(3) 2 1_455 ?
O7 Ce1 O14 126.5(3) 2_656 2_656 ?
O9 Ce1 O14 81.6(3) 1_454 2_656 ?
O5 Ce1 O14 81.3(3) . 2_656 ?
O2 Ce1 O14 73.7(3) 2_556 2_656 ?
O6 Ce1 O14 133.0(3) 2 2_656 ?
O15 Ce1 O14 148.5(3) 2 2_656 ?
O13 Ce1 O14 73.2(3) 1_455 2_656 ?
O14 I1 O3 100.0(4) . . ?
O14 I1 O11 92.8(4) . . ?
O3 I1 O11 92.7(4) . . ?
O14 I1 O8 84.4(4) . . ?
O3 I1 O8 88.2(4) . . ?
O11 I1 O8 177.1(4) . . ?
O2 I2 O15 99.1(4) . . ?
O2 I2 O12 94.5(4) . . ?
O15 I2 O12 101.1(4) . . ?
O5 I3 O13 98.3(4) . . ?
O5 I3 O10 97.6(4) . . ?
O13 I3 O10 96.7(4) . . ?
O9 I4 O7 97.5(4) . . ?
O9 I4 O1 95.6(4) . . ?
O7 I4 O1 96.2(4) . . ?
O6 Mo1 O4 105.8(4) . . ?
O6 Mo1 O8 101.8(4) . . ?
O4 Mo1 O8 99.5(4) . . ?
O6 Mo1 O1 161.6(4) . . ?
O4 Mo1 O1 88.1(3) . . ?
O8 Mo1 O1 87.3(3) . . ?
O6 Mo1 O12 88.5(4) . . ?
O4 Mo1 O12 161.2(4) . . ?
O8 Mo1 O12 89.2(4) . . ?
O1 Mo1 O12 75.6(3) . . ?
O6 Mo1 O10 90.4(4) . . ?
O4 Mo1 O10 88.8(4) . . ?
O8 Mo1 O10 162.6(3) . . ?
O1 Mo1 O10 77.7(3) . . ?
O12 Mo1 O10 78.8(3) . . ?
I4 O1 Mo1 124.2(4) . . ?
I2 O2 Ce1 139.1(5) . 2_546 ?
I3 O5 Ce1 148.0(5) . . ?
Mo1 O6 Ce1 165.6(5) . 2_545 ?
I4 O7 Ce1 150.7(5) . 2_646 ?
Mo1 O8 I1 122.5(4) . . ?
I4 O9 Ce1 137.3(5) . 1_656 ?
I3 O10 Mo1 117.8(4) . . ?
I2 O12 Mo1 135.3(4) . . ?
I3 O13 Ce1 119.8(4) . 1_655 ?
I1 O14 Ce1 127.1(5) . 2_646 ?
I2 O15 Ce1 136.5(4) . 2_545 ?

_refine_diff_density_max         1.462
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.286

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pr
_database_code_depnum_ccdc_archive 'CCDC 1886381'
_audit_update_record             
;
2019-01-25 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Praseodymium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         I4MoO15Pr
_chemical_formula_sum            'I4 Mo O15 Pr'
_chemical_formula_weight         984.45

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   6.9871(12)
_cell_length_b                   14.114(2)
_cell_length_c                   7.0873(12)
_cell_angle_alpha                90
_cell_angle_beta                 115.065(4)
_cell_angle_gamma                90
_cell_volume                     633.11(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2901
_cell_measurement_theta_min      2.886
_cell_measurement_theta_max      27.537

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    5.164
_exptl_crystal_F_000             866
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    14.629
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15323
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.886
_diffrn_reflns_theta_max         27.537
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2901
_reflns_number_gt                2879
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.998

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0138P)²] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0225(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1344 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2901
_refine_ls_number_parameters     191
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0413
_refine_ls_wR_factor_gt          0.0412
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.107
_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
Pr1 Pr 1.06767(7) 0.14153(3) 0.91310(7) 0.00554(12) Uani 1 1 d . . . . .
I1 I 0.24647(8) 0.72808(4) 0.65708(8) 0.00584(13) Uani 1 1 d . . . . .
I2 I 0.84499(8) 0.51238(4) 0.54946(8) 0.00550(13) Uani 1 1 d . . . . .
I3 I 0.46924(8) 0.23635(4) 0.73672(8) 0.00529(13) Uani 1 1 d . . . . .
I4 I 0.23641(8) 0.38862(4) 0.19321(8) 0.00550(13) Uani 1 1 d . . . . .
Mo1 Mo 0.40606(11) 0.47900(5) 0.70633(11) 0.00529(16) Uani 1 1 d . . . . .
O1 O 0.2367(9) 0.3816(4) 0.4536(8) 0.0062(12) Uani 1 1 d . . . . .
O2 O 0.7668(9) 0.5775(4) 0.3083(9) 0.0089(13) Uani 1 1 d . . . . .
O3 O 0.4767(9) 0.7422(5) 0.6072(9) 0.0098(12) Uani 1 1 d . . . . .
O4 O 0.2612(9) 0.4353(4) 0.8340(9) 0.0092(13) Uani 1 1 d . . . . .
O5 O 0.7015(10) 0.1646(4) 0.8489(9) 0.0104(13) Uani 1 1 d . . . . .
O6 O 0.6060(10) 0.5456(5) 0.8896(9) 0.0106(12) Uani 1 1 d . . . . .
O7 O 0.0411(10) 0.4810(5) 0.0936(9) 0.0130(13) Uani 1 1 d . . . . .
O8 O 0.2256(10) 0.5713(4) 0.5474(9) 0.0097(13) Uani 1 1 d . . . . .
O9 O 0.0613(10) 0.2903(4) 0.0822(9) 0.0095(13) Uani 1 1 d . . . . .
O10 O 0.6008(10) 0.3527(4) 0.8042(9) 0.0081(12) Uani 1 1 d . . . . .
O11 O 0.2519(10) 0.8608(4) 0.7372(10) 0.0117(13) Uani 1 1 d . . . . .
O12 O 0.5723(9) 0.4865(4) 0.5073(9) 0.0082(13) Uani 1 1 d . U . . .
O13 O 0.3914(9) 0.2324(5) 0.9526(8) 0.0087(12) Uani 1 1 d . U . . .
O14 O 0.0432(9) 0.7484(5) 0.4012(9) 0.0105(13) Uani 1 1 d . U . . .
O15 O 0.9070(10) 0.6111(4) 0.7279(9) 0.0097(13) Uani 1 1 d . . . . .


_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
Pr1 O7 2.384(6) 2_646 ?
Pr1 O9 2.427(6) 1_656 ?
Pr1 O5 2.423(6) . ?
Pr1 O2 2.481(6) 2_746 ?
Pr1 O6 2.508(6) 2_747 ?
Pr1 O13 2.511(6) 1_655 ?
Pr1 O15 2.511(6) 2_747 ?
Pr1 O14 2.525(6) 2_646 ?
I1 O14 1.790(6) . ?
I1 O3 1.799(6) . ?
I1 O11 1.953(6) . ?
I1 O8 2.330(6) . ?
I2 O2 1.809(6) . ?
I2 O15 1.806(6) . ?
I2 O12 1.836(6) . ?
I3 O5 1.789(6) . ?
I3 O13 1.829(5) . ?
I3 O10 1.843(6) . ?
I4 O9 1.796(6) . ?
I4 O7 1.801(6) . ?
I4 O1 1.848(5) . ?
Mo1 O6 1.727(6) . ?
Mo1 O4 1.732(6) . ?
Mo1 O8 1.830(6) . ?
Mo1 O12 2.176(5) . ?
Mo1 O1 2.168(6) . ?
Mo1 O10 2.171(6) . ?
O2 Pr1 2.481(6) 2_756 ?
O6 Pr1 2.508(6) 2_757 ?
O7 Pr1 2.384(6) 2_656 ?
O9 Pr1 2.427(6) 1_454 ?
O13 Pr1 2.511(6) 1_455 ?
O14 Pr1 2.525(6) 2_656 ?
O15 Pr1 2.511(6) 2_757 ?

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
O7 Pr1 O9 139.4(2) 2_646 1_656 ?
O7 Pr1 O5 79.7(2) 2_646 . ?
O9 Pr1 O5 74.8(2) 1_656 . ?
O7 Pr1 O2 82.6(2) 2_646 2_746 ?
O9 Pr1 O2 137.6(2) 1_656 2_746 ?
O5 Pr1 O2 131.9(2) . 2_746 ?
O7 Pr1 O6 72.8(2) 2_646 2_747 ?
O9 Pr1 O6 113.2(2) 1_656 2_747 ?
O5 Pr1 O6 144.6(2) . 2_747 ?
O2 Pr1 O6 66.3(2) 2_746 2_747 ?
O7 Pr1 O13 138.8(2) 2_646 1_655 ?
O9 Pr1 O13 73.0(2) 1_656 1_655 ?
O5 Pr1 O13 141.4(2) . 1_655 ?
O2 Pr1 O13 67.51(19) 2_746 1_655 ?
O6 Pr1 O13 69.5(2) 2_747 1_655 ?
O7 Pr1 O15 75.1(2) 2_646 2_747 ?
O9 Pr1 O15 69.9(2) 1_656 2_747 ?
O5 Pr1 O15 80.15(19) . 2_747 ?
O2 Pr1 O15 136.61(19) 2_746 2_747 ?
O6 Pr1 O15 71.67(19) 2_747 2_747 ?
O13 Pr1 O15 107.52(19) 1_655 2_747 ?
O7 Pr1 O14 125.0(2) 2_646 2_646 ?
O9 Pr1 O14 81.7(2) 1_656 2_646 ?
O5 Pr1 O14 81.32(19) . 2_646 ?
O2 Pr1 O14 73.2(2) 2_746 2_646 ?
O6 Pr1 O14 132.95(19) 2_747 2_646 ?
O13 Pr1 O14 73.65(19) 1_655 2_646 ?
O15 Pr1 O14 149.3(2) 2_747 2_646 ?
O14 I1 O3 100.1(3) . . ?
O14 I1 O11 92.9(3) . . ?
O3 I1 O11 92.4(3) . . ?
O14 I1 O8 84.5(3) . . ?
O3 I1 O8 88.5(3) . . ?
O11 I1 O8 177.3(2) . . ?
O2 I2 O15 99.0(3) . . ?
O2 I2 O12 94.0(3) . . ?
O15 I2 O12 101.1(3) . . ?
O5 I3 O13 98.4(3) . . ?
O5 I3 O10 97.5(3) . . ?
O13 I3 O10 95.9(3) . . ?
O9 I4 O7 97.2(3) . . ?
O9 I4 O1 96.2(3) . . ?
O7 I4 O1 96.3(3) . . ?
O6 Mo1 O4 105.4(3) . . ?
O6 Mo1 O8 101.7(3) . . ?
O4 Mo1 O8 99.9(3) . . ?
O6 Mo1 O12 88.7(3) . . ?
O4 Mo1 O12 161.1(3) . . ?
O8 Mo1 O12 89.1(3) . . ?
O6 Mo1 O1 161.9(3) . . ?
O4 Mo1 O1 88.3(2) . . ?
O8 Mo1 O1 87.1(2) . . ?
O12 Mo1 O1 75.5(2) . . ?
O6 Mo1 O10 90.5(3) . . ?
O4 Mo1 O10 88.1(2) . . ?
O8 Mo1 O10 163.0(2) . . ?
O12 Mo1 O10 79.2(2) . . ?
O1 Mo1 O10 78.0(2) . . ?
I4 O1 Mo1 124.1(3) . . ?
I2 O2 Pr1 138.4(3) . 2_756 ?
I3 O5 Pr1 147.8(3) . . ?
Mo1 O6 Pr1 165.4(3) . 2_757 ?
I4 O7 Pr1 151.4(4) . 2_656 ?
Mo1 O8 I1 122.8(3) . . ?
I4 O9 Pr1 137.1(3) . 1_454 ?
I3 O10 Mo1 118.2(3) . . ?
I2 O12 Mo1 134.9(3) . . ?
I3 O13 Pr1 119.7(3) . 1_455 ?
I1 O14 Pr1 127.8(3) . 2_656 ?
I2 O15 Pr1 137.3(3) . 2_757 ?

_refine_diff_density_max         1.240
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.211

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tb
_database_code_depnum_ccdc_archive 'CCDC 1886383'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Terbium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         IMo2O12Tb
_chemical_formula_sum            'I Mo2 O12 Tb'
_chemical_formula_weight         669.70

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5995(12)
_cell_length_b                   11.3847(18)
_cell_length_c                   11.3300(19)
_cell_angle_alpha                90
_cell_angle_beta                 92.142(4)
_cell_angle_gamma                90
_cell_volume                     979.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2240
_cell_measurement_theta_min      2.537
_cell_measurement_theta_max      27.535

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colerless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.541
_exptl_crystal_F_000             1192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    12.871
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19220
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.537
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2240
_reflns_number_gt                2196
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0629P)²+17.1718P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0124(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2240
_refine_ls_number_parameters     146
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_restrained_S_all      1.220
_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
Tb1 Tb 0.57996(5) 0.25621(3) 0.11526(3) 0.00375(18) Uani 1 1 d . . . . .
I1 I 0.38725(7) 0.10735(4) 0.40035(5) 0.0053(2) Uani 1 1 d . . . . .
Mo1 Mo 0.59803(10) 0.59747(6) 0.20397(6) 0.0046(2) Uani 1 1 d . U . . .
Mo2 Mo 0.63917(10) 0.91179(6) 0.16785(6) 0.0039(2) Uani 1 1 d . U . . .
O1 O 0.7057(9) 0.7511(5) 0.2197(6) 0.0068(12) Uani 1 1 d . U . . .
O2 O 0.6522(8) 0.4372(5) 0.1987(5) 0.0053(11) Uani 1 1 d . . . . .
O3 O 0.6978(8) 1.0719(5) 0.1600(5) 0.0064(12) Uani 1 1 d . . . . .
O4 O 0.4959(9) 0.6216(5) 0.0655(6) 0.0095(12) Uani 1 1 d . . . . .
O5 O 0.5439(9) 0.8727(6) 0.0308(6) 0.0099(12) Uani 1 1 d . . . . .
O6 O 0.3430(8) 0.2113(6) 0.5180(6) 0.0106(13) Uani 1 1 d . U . . .
O7 O 0.6184(8) 0.0736(6) 0.4368(5) 0.0071(12) Uani 1 1 d . U . . .
O8 O 0.4258(10) 0.6044(6) 0.2951(6) 0.0159(15) Uani 1 1 d . . . . .
O9 O 0.4579(9) 0.9244(6) 0.2519(6) 0.0123(13) Uani 1 1 d . . . . .
O10 O 0.4202(9) 0.2133(6) 0.2853(6) 0.0133(13) Uani 1 1 d . U . . .
OW1 O 0.2878(9) 0.3159(8) 0.1081(6) 0.0209(16) Uani 1 1 d . U . . .
OW2 O 0.8984(10) 0.8965(6) 0.0607(6) 0.0152(14) Uani 1 1 d . . . . .


_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
Tb1 O2 2.324(6) . ?
Tb1 O3 2.330(6) 1_545 ?
Tb1 OW1 2.320(7) . ?
Tb1 O6 2.347(6) 4_665 ?
Tb1 O10 2.366(7) . ?
Tb1 O5 2.380(6) 3_665 ?
Tb1 O1 2.434(7) 2_645 ?
Tb1 O4 2.524(6) 3_665 ?
Tb1 Mo1 3.6159(9) 2_645 ?
I1 O10 1.801(7) . ?
I1 O6 1.824(6) . ?
I1 O7 1.830(6) . ?
Mo1 O8 1.699(8) . ?
Mo1 O4 1.746(6) . ?
Mo1 O2 1.872(6) . ?
Mo1 O1 1.937(6) . ?
Mo1 O3 2.166(6) 2_645 ?
Mo1 Tb1 3.6160(9) 2_655 ?
Mo2 O9 1.710(7) . ?
Mo2 O5 1.746(6) . ?
Mo2 O3 1.879(6) . ?
Mo2 O1 1.981(6) . ?
Mo2 O2 2.169(6) 2_655 ?
Mo2 OW2 2.359(7) . ?
O1 Tb1 2.434(7) 2_655 ?
O2 Mo2 2.169(6) 2_645 ?
O3 Mo1 2.166(6) 2_655 ?
O3 Tb1 2.330(6) 1_565 ?
O4 Tb1 2.524(6) 3_665 ?
O5 Tb1 2.380(6) 3_665 ?
O6 Tb1 2.348(6) 4_566 ?

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
O2 Tb1 O3 128.8(2) . 1_545 ?
O2 Tb1 OW1 88.0(3) . . ?
O3 Tb1 OW1 129.1(3) 1_545 . ?
O2 Tb1 O6 81.9(2) . 4_665 ?
O3 Tb1 O6 85.2(2) 1_545 4_665 ?
OW1 Tb1 O6 140.1(2) . 4_665 ?
O2 Tb1 O10 88.4(2) . . ?
O3 Tb1 O10 80.9(2) 1_545 . ?
OW1 Tb1 O10 64.5(2) . . ?
O6 Tb1 O10 152.4(2) 4_665 . ?
O2 Tb1 O5 155.6(2) . 3_665 ?
O3 Tb1 O5 74.6(2) 1_545 3_665 ?
OW1 Tb1 O5 78.7(3) . 3_665 ?
O6 Tb1 O5 95.3(2) 4_665 3_665 ?
O10 Tb1 O5 103.7(2) . 3_665 ?
O2 Tb1 O1 64.39(19) . 2_645 ?
O3 Tb1 O1 64.59(19) 1_545 2_645 ?
OW1 Tb1 O1 130.2(2) . 2_645 ?
O6 Tb1 O1 78.9(2) 4_665 2_645 ?
O10 Tb1 O1 73.7(2) . 2_645 ?
O5 Tb1 O1 139.1(2) 3_665 2_645 ?
O2 Tb1 O4 83.4(2) . 3_665 ?
O3 Tb1 O4 138.3(2) 1_545 3_665 ?
OW1 Tb1 O4 67.7(2) . 3_665 ?
O6 Tb1 O4 72.9(2) 4_665 3_665 ?
O10 Tb1 O4 131.7(2) . 3_665 ?
O5 Tb1 O4 72.7(2) 3_665 3_665 ?
O1 Tb1 O4 139.7(2) 2_645 3_665 ?
O2 Tb1 Mo1 93.92(15) . 2_645 ?
O3 Tb1 Mo1 34.94(15) 1_545 2_645 ?
OW1 Tb1 Mo1 142.45(18) . 2_645 ?
O6 Tb1 Mo1 76.96(16) 4_665 2_645 ?
O10 Tb1 Mo1 78.04(17) . 2_645 ?
O5 Tb1 Mo1 109.11(16) 3_665 2_645 ?
O1 Tb1 Mo1 29.97(13) 2_645 2_645 ?
O4 Tb1 Mo1 149.78(15) 3_665 2_645 ?
O10 I1 O6 97.4(3) . . ?
O10 I1 O7 98.4(3) . . ?
O6 I1 O7 100.0(3) . . ?
O8 Mo1 O4 102.3(3) . . ?
O8 Mo1 O2 103.9(3) . . ?
O4 Mo1 O2 102.4(3) . . ?
O8 Mo1 O1 103.6(3) . . ?
O4 Mo1 O1 96.5(3) . . ?
O2 Mo1 O1 142.3(3) . . ?
O8 Mo1 O3 97.0(3) . 2_645 ?
O4 Mo1 O3 160.6(3) . 2_645 ?
O2 Mo1 O3 74.9(2) . 2_645 ?
O1 Mo1 O3 76.5(3) . 2_645 ?
O8 Mo1 Tb1 98.8(2) . 2_655 ?
O4 Mo1 Tb1 134.3(2) . 2_655 ?
O2 Mo1 Tb1 111.13(18) . 2_655 ?
O1 Mo1 Tb1 38.89(19) . 2_655 ?
O3 Mo1 Tb1 38.03(16) 2_645 2_655 ?
O9 Mo2 O5 101.6(3) . . ?
O9 Mo2 O3 98.2(3) . . ?
O5 Mo2 O3 107.2(3) . . ?
O9 Mo2 O1 96.5(3) . . ?
O5 Mo2 O1 97.0(3) . . ?
O3 Mo2 O1 148.4(3) . . ?
O9 Mo2 O2 100.6(3) . 2_655 ?
O5 Mo2 O2 157.2(3) . 2_655 ?
O3 Mo2 O2 74.7(2) . 2_655 ?
O1 Mo2 O2 75.2(3) . 2_655 ?
O9 Mo2 OW2 177.0(3) . . ?
O5 Mo2 OW2 81.4(3) . . ?
O3 Mo2 OW2 81.0(3) . . ?
O1 Mo2 OW2 82.9(3) . . ?
O2 Mo2 OW2 76.5(2) 2_655 . ?
Mo1 O1 Mo2 134.8(4) . . ?
Mo1 O1 Tb1 111.1(3) . 2_655 ?
Mo2 O1 Tb1 111.2(3) . 2_655 ?
Mo1 O2 Mo2 105.3(3) . 2_645 ?
Mo1 O2 Tb1 145.9(3) . . ?
Mo2 O2 Tb1 108.7(2) 2_645 . ?
Mo2 O3 Mo1 105.2(3) . 2_655 ?
Mo2 O3 Tb1 142.6(3) . 1_565 ?
Mo1 O3 Tb1 107.0(2) 2_655 1_565 ?
Mo1 O4 Tb1 153.6(3) . 3_665 ?
Mo2 O5 Tb1 156.3(4) . 3_665 ?
I1 O6 Tb1 129.0(3) . 4_566 ?
I1 O10 Tb1 144.8(4) . . ?

_refine_diff_density_max         2.165
_refine_diff_density_min         -3.028
_refine_diff_density_rms         0.522

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Dy
_database_code_depnum_ccdc_archive 'CCDC 1886384'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Dysprosium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         DyIMo2O12
_chemical_formula_sum            'Dy I Mo2 O12'
_chemical_formula_weight         673.28

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5804(4)
_cell_length_b                   11.3583(6)
_cell_length_c                   11.2975(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.2852(17)
_cell_angle_gamma                90
_cell_volume                     971.95(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2240
_cell_measurement_theta_min      3.179
_cell_measurement_theta_max      27.569

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.601
_exptl_crystal_F_000             1196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    13.383
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21531
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.179
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2240
_reflns_number_gt                1990
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0203P)²+3.8795P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2240
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0489
_refine_ls_wR_factor_gt          0.0474
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_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
Dy1 Dy 0.58060(3) 0.25560(2) 0.11580(2) 0.00720(7) Uani 1 1 d . . . . .
I1 I 0.38717(4) 0.10851(3) 0.40068(3) 0.01108(9) Uani 1 1 d . . . . .
Mo1 Mo 0.59865(6) 0.59665(4) 0.20227(4) 0.00778(10) Uani 1 1 d . . . . .
Mo2 Mo 0.63734(6) 0.91142(4) 0.16802(4) 0.00760(10) Uani 1 1 d . . . . .
O1 O 0.7063(5) 0.7506(3) 0.2196(3) 0.0093(7) Uani 1 1 d . . . . .
O2 O 0.6522(5) 0.4363(3) 0.1976(3) 0.0102(7) Uani 1 1 d . . . . .
O3 O 0.6968(5) 1.0718(3) 0.1604(3) 0.0105(7) Uani 1 1 d . . . . .
O4 O 0.4961(5) 0.6223(3) 0.0639(3) 0.0132(8) Uani 1 1 d . . . . .
O5 O 0.5444(5) 0.8718(3) 0.0309(3) 0.0148(8) Uani 1 1 d . . . . .
O6 O 0.3416(5) 0.2132(3) 0.5169(3) 0.0155(8) Uani 1 1 d . . . . .
O7 O 0.6182(5) 0.0748(3) 0.4368(3) 0.0149(8) Uani 1 1 d . . . . .
O8 O 0.4255(5) 0.6028(3) 0.2928(3) 0.0186(9) Uani 1 1 d . . . . .
O9 O 0.4557(5) 0.9232(3) 0.2520(3) 0.0181(8) Uani 1 1 d . . . . .
O10 O 0.2865(6) 0.3140(4) 0.1071(4) 0.0324(12) Uani 1 1 d . . . . .
OW1 O 0.4201(5) 0.2129(4) 0.2848(3) 0.0205(9) Uani 1 1 d . . . . .
OW2 O 0.9000(6) 0.8965(3) 0.0594(4) 0.0226(9) Uani 1 1 d . . . . .


_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
Dy1 O2 2.307(3) . ?
Dy1 O3 2.314(3) 1_545 ?
Dy1 O10 2.324(4) . ?
Dy1 O6 2.338(4) 4_665 ?
Dy1 OW1 2.355(4) . ?
Dy1 O5 2.370(3) 3_665 ?
Dy1 O1 2.415(3) 2_645 ?
Dy1 O4 2.508(4) 3_665 ?
Dy1 Mo1 3.6052(5) 2_645 ?
I1 OW1 1.791(4) . ?
I1 O6 1.815(4) . ?
I1 O7 1.823(4) . ?
Mo1 O8 1.697(4) . ?
Mo1 O4 1.742(4) . ?
Mo1 O2 1.867(3) . ?
Mo1 O1 1.937(3) . ?
Mo1 O3 2.168(3) 2_645 ?
Mo1 Mo2 3.2164(6) 2_645 ?
Mo1 Dy1 3.6052(5) 2_655 ?
Mo2 O9 1.709(4) . ?
Mo2 O5 1.735(3) . ?
Mo2 O3 1.879(3) . ?
Mo2 O1 1.980(3) . ?
Mo2 O2 2.177(3) 2_655 ?
Mo2 OW2 2.387(4) . ?
Mo2 Mo1 3.2164(6) 2_655 ?
O1 Dy1 2.415(3) 2_655 ?
O2 Mo2 2.176(3) 2_645 ?
O3 Mo1 2.168(3) 2_655 ?
O3 Dy1 2.314(3) 1_565 ?
O4 Dy1 2.508(4) 3_665 ?
O5 Dy1 2.370(3) 3_665 ?
O6 Dy1 2.338(4) 4_566 ?

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
O2 Dy1 O3 129.37(12) . 1_545 ?
O2 Dy1 O10 88.43(16) . . ?
O3 Dy1 O10 128.53(15) 1_545 . ?
O2 Dy1 O6 82.33(13) . 4_665 ?
O3 Dy1 O6 85.35(13) 1_545 4_665 ?
O10 Dy1 O6 139.91(14) . 4_665 ?
O2 Dy1 OW1 88.82(14) . . ?
O3 Dy1 OW1 80.91(13) 1_545 . ?
O10 Dy1 OW1 64.38(14) . . ?
O6 Dy1 OW1 153.28(14) 4_665 . ?
O2 Dy1 O5 154.80(12) . 3_665 ?
O3 Dy1 O5 74.88(12) 1_545 3_665 ?
O10 Dy1 O5 77.81(16) . 3_665 ?
O6 Dy1 O5 94.62(14) 4_665 3_665 ?
OW1 Dy1 O5 103.67(14) . 3_665 ?
O2 Dy1 O1 64.70(11) . 2_645 ?
O3 Dy1 O1 64.81(11) 1_545 2_645 ?
O10 Dy1 O1 130.56(14) . 2_645 ?
O6 Dy1 O1 79.55(13) 4_665 2_645 ?
OW1 Dy1 O1 73.88(13) . 2_645 ?
O5 Dy1 O1 139.56(11) 3_665 2_645 ?
O2 Dy1 O4 82.84(11) . 3_665 ?
O3 Dy1 O4 138.53(12) 1_545 3_665 ?
O10 Dy1 O4 67.46(13) . 3_665 ?
O6 Dy1 O4 72.70(12) 4_665 3_665 ?
OW1 Dy1 O4 131.27(13) . 3_665 ?
O5 Dy1 O4 72.43(12) 3_665 3_665 ?
O1 Dy1 O4 139.70(11) 2_645 3_665 ?
O2 Dy1 Mo1 94.28(8) . 2_645 ?
O3 Dy1 Mo1 35.10(8) 1_545 2_645 ?
O10 Dy1 Mo1 142.29(10) . 2_645 ?
O6 Dy1 Mo1 77.53(9) 4_665 2_645 ?
OW1 Dy1 Mo1 78.06(10) . 2_645 ?
O5 Dy1 Mo1 109.56(9) 3_665 2_645 ?
O1 Dy1 Mo1 30.01(7) 2_645 2_645 ?
O4 Dy1 Mo1 150.21(9) 3_665 2_645 ?
OW1 I1 O6 97.55(18) . . ?
OW1 I1 O7 98.18(18) . . ?
O6 I1 O7 100.64(17) . . ?
O8 Mo1 O4 101.86(18) . . ?
O8 Mo1 O2 103.36(17) . . ?
O4 Mo1 O2 103.13(16) . . ?
O8 Mo1 O1 103.59(17) . . ?
O4 Mo1 O1 96.36(16) . . ?
O2 Mo1 O1 142.44(15) . . ?
O8 Mo1 O3 97.05(16) . 2_645 ?
O4 Mo1 O3 160.85(16) . 2_645 ?
O2 Mo1 O3 75.10(14) . 2_645 ?
O1 Mo1 O3 76.06(13) . 2_645 ?
O8 Mo1 Mo2 103.57(13) . 2_645 ?
O4 Mo1 Mo2 139.93(12) . 2_645 ?
O2 Mo1 Mo2 40.79(10) . 2_645 ?
O1 Mo1 Mo2 107.03(10) . 2_645 ?
O3 Mo1 Mo2 34.34(9) 2_645 2_645 ?
O8 Mo1 Dy1 98.99(13) . 2_655 ?
O4 Mo1 Dy1 133.99(12) . 2_655 ?
O2 Mo1 Dy1 111.24(10) . 2_655 ?
O1 Mo1 Dy1 38.59(10) . 2_655 ?
O3 Mo1 Dy1 37.85(9) 2_645 2_655 ?
Mo2 Mo1 Dy1 71.008(12) 2_645 2_655 ?
O9 Mo2 O5 102.03(19) . . ?
O9 Mo2 O3 98.61(17) . . ?
O5 Mo2 O3 107.45(16) . . ?
O9 Mo2 O1 96.77(17) . . ?
O5 Mo2 O1 96.69(15) . . ?
O3 Mo2 O1 147.81(15) . . ?
O9 Mo2 O2 100.78(16) . 2_655 ?
O5 Mo2 O2 156.44(16) . 2_655 ?
O3 Mo2 O2 74.68(14) . 2_655 ?
O1 Mo2 O2 74.76(13) . 2_655 ?
O9 Mo2 OW2 177.16(17) . . ?
O5 Mo2 OW2 80.79(17) . . ?
O3 Mo2 OW2 80.72(15) . . ?
O1 Mo2 OW2 82.53(14) . . ?
O2 Mo2 OW2 76.38(14) 2_655 . ?
O9 Mo2 Mo1 101.32(13) . 2_655 ?
O5 Mo2 Mo1 143.08(13) . 2_655 ?
O3 Mo2 Mo1 40.62(10) . 2_655 ?
O1 Mo2 Mo1 108.49(10) . 2_655 ?
O2 Mo2 Mo1 34.09(9) 2_655 2_655 ?
OW2 Mo2 Mo1 76.36(10) . 2_655 ?
Mo1 O1 Mo2 134.26(19) . . ?
Mo1 O1 Dy1 111.40(14) . 2_655 ?
Mo2 O1 Dy1 111.44(14) . 2_655 ?
Mo1 O2 Mo2 105.13(15) . 2_645 ?
Mo1 O2 Dy1 146.24(18) . . ?
Mo2 O2 Dy1 108.55(14) 2_645 . ?
Mo2 O3 Mo1 105.04(15) . 2_655 ?
Mo2 O3 Dy1 142.65(18) . 1_565 ?
Mo1 O3 Dy1 107.05(14) 2_655 1_565 ?
Mo1 O4 Dy1 154.07(19) . 3_665 ?
Mo2 O5 Dy1 156.9(2) . 3_665 ?
I1 O6 Dy1 129.37(19) . 4_566 ?
I1 OW1 Dy1 145.1(2) . . ?

_refine_diff_density_max         1.139
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.260

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Yb
_database_code_depnum_ccdc_archive 'CCDC 1886388'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Ytterbium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         IMo2O12Yb
_chemical_formula_sum            'I Mo2 O12 Yb'
_chemical_formula_weight         683.82

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5242(16)
_cell_length_b                   11.321(2)
_cell_length_c                   11.203(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.308(7)
_cell_angle_gamma                90
_cell_volume                     953.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2184
_cell_measurement_theta_min      2.559
_cell_measurement_theta_max      27.550

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.764
_exptl_crystal_F_000             1212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.023
_exptl_absorpt_coefficient_mu    15.614
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18385
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.559
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2184
_reflns_number_gt                1916
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0686P)²] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2184
_refine_ls_number_parameters     145
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.117
_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
Yb1 Yb 0.58345(5) 0.25527(3) 0.11736(3) 0.00610(15) Uani 1 1 d . . . . .
I1 I 0.38706(7) 0.10964(4) 0.40172(5) 0.00854(17) Uani 1 1 d . . . . .
Mo1 Mo 0.59625(9) 0.59522(6) 0.20270(7) 0.00685(19) Uani 1 1 d . . . . .
Mo2 Mo 0.63453(10) 0.91099(6) 0.16716(7) 0.00662(19) Uani 1 1 d . . . . .
O1 O 0.7033(8) 0.7502(4) 0.2201(6) 0.0069(13) Uani 1 1 d . U . . .
O2 O 0.6527(8) 0.4350(5) 0.1989(5) 0.0085(12) Uani 1 1 d . . . . .
O3 O 0.6960(8) 1.0731(5) 0.1598(5) 0.0094(12) Uani 1 1 d . . . . .
O4 O 0.4918(8) 0.6225(5) 0.0630(5) 0.0115(13) Uani 1 1 d . . . . .
O5 O 0.5397(8) 0.8696(5) 0.0286(6) 0.0135(13) Uani 1 1 d . . . . .
O6 O 0.3423(8) 0.2150(5) 0.5194(5) 0.0118(13) Uani 1 1 d . . . . .
O7 O 0.6194(8) 0.0741(5) 0.4385(6) 0.0124(13) Uani 1 1 d . . . . .
O8 O 0.4193(9) 0.6005(5) 0.2947(6) 0.0165(14) Uani 1 1 d . . . . .
O9 O 0.4514(8) 0.9241(5) 0.2525(6) 0.0132(13) Uani 1 1 d . . . . .
O10 O 0.4260(8) 0.2164(6) 0.2863(5) 0.0141(13) Uani 1 1 d . . . . .
OW1 O 0.2941(9) 0.3144(7) 0.1076(6) 0.0256(17) Uani 1 1 d . . . . .
OW2 O 0.8970(9) 0.8968(5) 0.0588(6) 0.0160(14) Uani 1 1 d . . . . .


_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
Yb1 O2 2.282(5) . ?
Yb1 O3 2.272(6) 1_545 ?
Yb1 OW1 2.276(6) . ?
Yb1 O6 2.299(6) 4_665 ?
Yb1 O10 2.315(6) . ?
Yb1 O5 2.326(6) 3_665 ?
Yb1 O1 2.378(6) 2_645 ?
Yb1 O4 2.495(6) 3_665 ?
Yb1 Mo1 3.5726(9) 2_645 ?
Yb1 Mo2 3.6091(9) 2_645 ?
Yb1 I1 3.7199(8) 4_665 ?
I1 O10 1.803(6) . ?
I1 O6 1.819(6) . ?
I1 O7 1.825(6) . ?
I1 Yb1 3.7199(8) 4_566 ?
Mo1 O8 1.718(7) . ?
Mo1 O4 1.750(6) . ?
Mo1 O2 1.864(5) . ?
Mo1 O1 1.937(5) . ?
Mo1 O3 2.165(6) 2_645 ?
Mo1 Mo2 3.2157(11) 2_645 ?
Mo1 Yb1 3.5726(9) 2_655 ?
Mo2 O9 1.715(6) . ?
Mo2 O5 1.746(6) . ?
Mo2 O3 1.895(6) . ?
Mo2 O1 1.977(5) . ?
Mo2 O2 2.167(6) 2_655 ?
Mo2 OW2 2.365(7) . ?
Mo2 Mo1 3.2157(11) 2_655 ?
Mo2 Yb1 3.6091(9) 2_655 ?
O1 Yb1 2.379(6) 2_655 ?
O2 Mo2 2.167(6) 2_645 ?
O3 Mo1 2.165(6) 2_655 ?
O3 Yb1 2.272(6) 1_565 ?
O4 Yb1 2.495(6) 3_665 ?
O5 Yb1 2.326(6) 3_665 ?
O6 Yb1 2.299(6) 4_566 ?

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
O2 Yb1 O3 130.4(2) . 1_545 ?
O2 Yb1 OW1 87.7(3) . . ?
O3 Yb1 OW1 128.6(2) 1_545 . ?
O2 Yb1 O6 82.9(2) . 4_665 ?
O3 Yb1 O6 85.2(2) 1_545 4_665 ?
OW1 Yb1 O6 139.6(2) . 4_665 ?
O2 Yb1 O10 87.6(2) . . ?
O3 Yb1 O10 81.7(2) 1_545 . ?
OW1 Yb1 O10 64.9(2) . . ?
O6 Yb1 O10 152.8(2) 4_665 . ?
O2 Yb1 O5 154.4(2) . 3_665 ?
O3 Yb1 O5 74.3(2) 1_545 3_665 ?
OW1 Yb1 O5 78.0(3) . 3_665 ?
O6 Yb1 O5 94.3(2) 4_665 3_665 ?
O10 Yb1 O5 104.9(2) . 3_665 ?
O2 Yb1 O1 65.10(18) . 2_645 ?
O3 Yb1 O1 65.41(18) 1_545 2_645 ?
OW1 Yb1 O1 131.2(2) . 2_645 ?
O6 Yb1 O1 79.1(2) 4_665 2_645 ?
O10 Yb1 O1 73.8(2) . 2_645 ?
O5 Yb1 O1 139.54(19) 3_665 2_645 ?
O2 Yb1 O4 82.56(19) . 3_665 ?
O3 Yb1 O4 138.0(2) 1_545 3_665 ?
OW1 Yb1 O4 67.2(2) . 3_665 ?
O6 Yb1 O4 72.6(2) 4_665 3_665 ?
O10 Yb1 O4 131.3(2) . 3_665 ?
O5 Yb1 O4 72.3(2) 3_665 3_665 ?
O1 Yb1 O4 139.24(18) 2_645 3_665 ?
O2 Yb1 Mo1 95.07(14) . 2_645 ?
O3 Yb1 Mo1 35.36(14) 1_545 2_645 ?
OW1 Yb1 Mo1 142.99(16) . 2_645 ?
O6 Yb1 Mo1 77.20(15) 4_665 2_645 ?
O10 Yb1 Mo1 78.35(15) . 2_645 ?
O5 Yb1 Mo1 109.21(15) 3_665 2_645 ?
O1 Yb1 Mo1 30.33(11) 2_645 2_645 ?
O4 Yb1 Mo1 149.79(14) 3_665 2_645 ?
O2 Yb1 Mo2 34.73(14) . 2_645 ?
O3 Yb1 Mo2 95.70(14) 1_545 2_645 ?
OW1 Yb1 Mo2 115.1(2) . 2_645 ?
O6 Yb1 Mo2 76.18(16) 4_665 2_645 ?
O10 Yb1 Mo2 81.51(16) . 2_645 ?
O5 Yb1 Mo2 166.92(16) 3_665 2_645 ?
O1 Yb1 Mo2 30.62(11) 2_645 2_645 ?
O4 Yb1 Mo2 112.27(14) 3_665 2_645 ?
Mo1 Yb1 Mo2 60.34(2) 2_645 2_645 ?
O2 Yb1 I1 75.95(15) . 4_665 ?
O3 Yb1 I1 105.99(16) 1_545 4_665 ?
OW1 Yb1 I1 117.33(17) . 4_665 ?
O6 Yb1 I1 22.39(15) 4_665 4_665 ?
O10 Yb1 I1 163.11(16) . 4_665 ?
O5 Yb1 I1 91.78(16) 3_665 4_665 ?
O1 Yb1 I1 95.40(15) 2_645 4_665 ?
O4 Yb1 I1 51.06(14) 3_665 4_665 ?
Mo1 Yb1 I1 99.03(2) 2_645 4_665 ?
Mo2 Yb1 I1 82.74(2) 2_645 4_665 ?
O10 I1 O6 96.9(3) . . ?
O10 I1 O7 97.4(3) . . ?
O6 I1 O7 100.6(3) . . ?
O10 I1 Yb1 108.2(2) . 4_566 ?
O6 I1 Yb1 28.77(19) . 4_566 ?
O7 I1 Yb1 123.5(2) . 4_566 ?
O8 Mo1 O4 101.5(3) . . ?
O8 Mo1 O2 103.3(3) . . ?
O4 Mo1 O2 104.2(3) . . ?
O8 Mo1 O1 103.7(3) . . ?
O4 Mo1 O1 95.7(3) . . ?
O2 Mo1 O1 142.1(3) . . ?
O8 Mo1 O3 97.6(3) . 2_645 ?
O4 Mo1 O3 160.4(3) . 2_645 ?
O2 Mo1 O3 75.2(2) . 2_645 ?
O1 Mo1 O3 75.4(2) . 2_645 ?
O8 Mo1 Mo2 103.9(2) . 2_645 ?
O4 Mo1 Mo2 140.52(19) . 2_645 ?
O2 Mo1 Mo2 40.47(18) . 2_645 ?
O1 Mo1 Mo2 106.85(18) . 2_645 ?
O3 Mo1 Mo2 34.78(15) 2_645 2_645 ?
O8 Mo1 Yb1 99.5(2) . 2_655 ?
O4 Mo1 Yb1 133.11(19) . 2_655 ?
O2 Mo1 Yb1 110.94(18) . 2_655 ?
O1 Mo1 Yb1 38.32(18) . 2_655 ?
O3 Mo1 Yb1 37.41(14) 2_645 2_655 ?
Mo2 Mo1 Yb1 71.02(2) 2_645 2_655 ?
O9 Mo2 O5 102.1(3) . . ?
O9 Mo2 O3 98.2(3) . . ?
O5 Mo2 O3 108.2(3) . . ?
O9 Mo2 O1 96.8(3) . . ?
O5 Mo2 O1 96.5(3) . . ?
O3 Mo2 O1 147.5(3) . . ?
O9 Mo2 O2 101.0(3) . 2_655 ?
O5 Mo2 O2 156.0(3) . 2_655 ?
O3 Mo2 O2 74.6(2) . 2_655 ?
O1 Mo2 O2 74.4(2) . 2_655 ?
O9 Mo2 OW2 176.8(3) . . ?
O5 Mo2 OW2 81.1(3) . . ?
O3 Mo2 OW2 80.4(2) . . ?
O1 Mo2 OW2 83.0(2) . . ?
O2 Mo2 OW2 75.8(2) 2_655 . ?
O9 Mo2 Mo1 101.3(2) . 2_655 ?
O5 Mo2 Mo1 143.6(2) . 2_655 ?
O3 Mo2 Mo1 40.66(17) . 2_655 ?
O1 Mo2 Mo1 107.97(18) . 2_655 ?
O2 Mo2 Mo1 33.94(14) 2_655 2_655 ?
OW2 Mo2 Mo1 75.70(15) . 2_655 ?
O9 Mo2 Yb1 97.7(2) . 2_655 ?
O5 Mo2 Yb1 132.21(19) . 2_655 ?
O3 Mo2 Yb1 111.36(18) . 2_655 ?
O1 Mo2 Yb1 37.80(18) . 2_655 ?
O2 Mo2 Yb1 36.86(14) 2_655 2_655 ?
OW2 Mo2 Yb1 80.18(16) . 2_655 ?
Mo1 Mo2 Yb1 70.78(2) 2_655 2_655 ?
Mo1 O1 Mo2 134.5(3) . . ?
Mo1 O1 Yb1 111.3(2) . 2_655 ?
Mo2 O1 Yb1 111.6(2) . 2_655 ?
Mo1 O2 Mo2 105.6(3) . 2_645 ?
Mo1 O2 Yb1 145.9(3) . . ?
Mo2 O2 Yb1 108.4(2) 2_645 . ?
Mo2 O3 Mo1 104.6(3) . 2_655 ?
Mo2 O3 Yb1 143.0(3) . 1_565 ?
Mo1 O3 Yb1 107.2(2) 2_655 1_565 ?
Mo1 O4 Yb1 154.3(3) . 3_665 ?
Mo2 O5 Yb1 157.7(3) . 3_665 ?
I1 O6 Yb1 128.8(3) . 4_566 ?
I1 O10 Yb1 144.8(3) . . ?

_refine_diff_density_max         2.539
_refine_diff_density_min         -3.532
_refine_diff_density_rms         0.705

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ho
_database_code_depnum_ccdc_archive 'CCDC 1886385'
_audit_update_record             
;
2019-01-25 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Holmium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         HoIMo2O12
_chemical_formula_sum            'Ho I Mo2 O12'
_chemical_formula_weight         675.71

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5554(4)
_cell_length_b                   11.3436(6)
_cell_length_c                   11.2689(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.2717(15)
_cell_angle_gamma                90
_cell_volume                     965.05(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2239
_cell_measurement_theta_min      2.549
_cell_measurement_theta_max      27.649

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Pink
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.651
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    13.935
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20837
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.189
_diffrn_reflns_theta_max         27.649
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2237
_reflns_number_gt                2124
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0044P)²+3.2799P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00282(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2237
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0150
_refine_ls_wR_factor_ref         0.0328
_refine_ls_wR_factor_gt          0.0324
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Ho1 Ho 0.58158(2) 0.25569(2) 0.11604(2) 0.00660(5) Uani 1 1 d . . . . .
I1 I 0.38706(3) 0.10876(2) 0.40059(2) 0.00847(6) Uani 1 1 d . . . . .
Mo1 Mo 0.59793(4) 0.59635(3) 0.20279(3) 0.00746(7) Uani 1 1 d . . . . .
Mo2 Mo 0.63643(4) 0.91139(2) 0.16794(3) 0.00671(7) Uani 1 1 d . . . . .
O1 O 0.7047(3) 0.7506(2) 0.2199(2) 0.0099(5) Uani 1 1 d . . . . .
O2 O 0.6529(3) 0.4359(2) 0.1975(2) 0.0099(5) Uani 1 1 d . . . . .
O3 O 0.6964(3) 1.0716(2) 0.1602(2) 0.0108(5) Uani 1 1 d . . . . .
O4 O 0.4957(3) 0.6217(2) 0.0636(2) 0.0134(5) Uani 1 1 d . . . . .
O5 O 0.5421(4) 0.8719(2) 0.0308(2) 0.0142(5) Uani 1 1 d . . . . .
O6 O 0.3420(3) 0.2136(2) 0.5167(2) 0.0146(5) Uani 1 1 d . . . . .
O7 O 0.6178(3) 0.0748(2) 0.4376(2) 0.0130(5) Uani 1 1 d . . . . .
O8 O 0.4240(4) 0.6021(2) 0.2930(2) 0.0186(6) Uani 1 1 d . . . . .
O9 O 0.4548(3) 0.9234(2) 0.2520(2) 0.0166(6) Uani 1 1 d . . . . .
O10 O 0.4215(3) 0.2134(2) 0.2848(2) 0.0175(6) Uani 1 1 d . . . . .
OW1 O 0.2894(4) 0.3149(3) 0.1073(3) 0.0300(8) Uani 1 1 d . . . . .
OW2 O 0.8981(4) 0.8972(2) 0.0593(2) 0.0201(6) Uani 1 1 d . . . . .


_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
Ho1 O2 2.296(2) . ?
Ho1 O3 2.308(2) 1_545 ?
Ho1 OW1 2.306(3) . ?
Ho1 O6 2.328(3) 4_665 ?
Ho1 O10 2.343(3) . ?
Ho1 O5 2.363(2) 3_665 ?
Ho1 O1 2.406(2) 2_645 ?
Ho1 O4 2.506(2) 3_665 ?
Ho1 Mo1 3.5926(3) 2_645 ?
I1 O10 1.791(3) . ?
I1 O6 1.811(2) . ?
I1 O7 1.818(2) . ?
Mo1 O8 1.695(3) . ?
Mo1 O4 1.745(2) . ?
Mo1 O2 1.869(2) . ?
Mo1 O1 1.933(2) . ?
Mo1 O3 2.165(2) 2_645 ?
Mo1 Mo2 3.2125(4) 2_645 ?
Mo1 Ho1 3.5926(3) 2_655 ?
Mo2 O9 1.704(3) . ?
Mo2 O5 1.735(2) . ?
Mo2 O3 1.876(2) . ?
Mo2 O1 1.978(2) . ?
Mo2 O2 2.172(2) 2_655 ?
Mo2 OW2 2.371(3) . ?
Mo2 Mo1 3.2125(4) 2_655 ?
O1 Ho1 2.406(2) 2_655 ?
O2 Mo2 2.172(2) 2_645 ?
O3 Mo1 2.165(2) 2_655 ?
O3 Ho1 2.308(2) 1_565 ?
O4 Ho1 2.506(2) 3_665 ?
O5 Ho1 2.363(2) 3_665 ?
O6 Ho1 2.328(3) 4_566 ?

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
O2 Ho1 O3 129.72(8) . 1_545 ?
O2 Ho1 OW1 88.10(11) . . ?
O3 Ho1 OW1 128.59(11) 1_545 . ?
O2 Ho1 O6 82.51(9) . 4_665 ?
O3 Ho1 O6 85.50(9) 1_545 4_665 ?
OW1 Ho1 O6 139.62(10) . 4_665 ?
O2 Ho1 O10 88.75(9) . . ?
O3 Ho1 O10 80.87(9) 1_545 . ?
OW1 Ho1 O10 64.56(9) . . ?
O6 Ho1 O10 153.37(9) 4_665 . ?
O2 Ho1 O5 154.86(8) . 3_665 ?
O3 Ho1 O5 74.43(8) 1_545 3_665 ?
OW1 Ho1 O5 78.30(11) . 3_665 ?
O6 Ho1 O5 94.20(9) 4_665 3_665 ?
O10 Ho1 O5 103.92(10) . 3_665 ?
O2 Ho1 O1 64.82(8) . 2_645 ?
O3 Ho1 O1 65.02(8) 1_545 2_645 ?
OW1 Ho1 O1 130.68(10) . 2_645 ?
O6 Ho1 O1 79.57(9) 4_665 2_645 ?
O10 Ho1 O1 73.96(9) . 2_645 ?
O5 Ho1 O1 139.28(8) 3_665 2_645 ?
O2 Ho1 O4 82.67(8) . 3_665 ?
O3 Ho1 O4 138.58(8) 1_545 3_665 ?
OW1 Ho1 O4 67.16(9) . 3_665 ?
O6 Ho1 O4 72.71(9) 4_665 3_665 ?
O10 Ho1 O4 131.16(9) . 3_665 ?
O5 Ho1 O4 72.62(9) 3_665 3_665 ?
O1 Ho1 O4 139.60(8) 2_645 3_665 ?
O2 Ho1 Mo1 94.50(6) . 2_645 ?
O3 Ho1 Mo1 35.23(6) 1_545 2_645 ?
OW1 Ho1 Mo1 142.51(7) . 2_645 ?
O6 Ho1 Mo1 77.59(6) 4_665 2_645 ?
O10 Ho1 Mo1 78.09(6) . 2_645 ?
O5 Ho1 Mo1 109.19(6) 3_665 2_645 ?
O1 Ho1 Mo1 30.09(5) 2_645 2_645 ?
O4 Ho1 Mo1 150.28(6) 3_665 2_645 ?
O10 I1 O6 97.35(13) . . ?
O10 I1 O7 98.15(12) . . ?
O6 I1 O7 100.36(12) . . ?
O8 Mo1 O4 101.93(13) . . ?
O8 Mo1 O2 103.63(12) . . ?
O4 Mo1 O2 102.89(11) . . ?
O8 Mo1 O1 103.63(12) . . ?
O4 Mo1 O1 96.25(11) . . ?
O2 Mo1 O1 142.41(11) . . ?
O8 Mo1 O3 97.42(12) . 2_645 ?
O4 Mo1 O3 160.43(11) . 2_645 ?
O2 Mo1 O3 75.06(10) . 2_645 ?
O1 Mo1 O3 76.18(10) . 2_645 ?
O8 Mo1 Mo2 103.81(9) . 2_645 ?
O4 Mo1 Mo2 139.62(9) . 2_645 ?
O2 Mo1 Mo2 40.75(7) . 2_645 ?
O1 Mo1 Mo2 107.16(7) . 2_645 ?
O3 Mo1 Mo2 34.32(6) 2_645 2_645 ?
O8 Mo1 Ho1 99.26(9) . 2_655 ?
O4 Mo1 Ho1 133.83(8) . 2_655 ?
O2 Mo1 Ho1 111.25(7) . 2_655 ?
O1 Mo1 Ho1 38.61(7) . 2_655 ?
O3 Mo1 Ho1 37.94(6) 2_645 2_655 ?
Mo2 Mo1 Ho1 71.095(9) 2_645 2_655 ?
O9 Mo2 O5 101.81(13) . . ?
O9 Mo2 O3 98.59(12) . . ?
O5 Mo2 O3 107.46(11) . . ?
O9 Mo2 O1 96.64(12) . . ?
O5 Mo2 O1 96.83(11) . . ?
O3 Mo2 O1 147.84(11) . . ?
O9 Mo2 O2 100.70(11) . 2_655 ?
O5 Mo2 O2 156.73(11) . 2_655 ?
O3 Mo2 O2 74.75(10) . 2_655 ?
O1 Mo2 O2 74.68(9) . 2_655 ?
O9 Mo2 OW2 177.16(11) . . ?
O5 Mo2 OW2 81.03(12) . . ?
O3 Mo2 OW2 80.45(10) . . ?
O1 Mo2 OW2 82.94(10) . . ?
O2 Mo2 OW2 76.48(10) 2_655 . ?
O9 Mo2 Mo1 101.42(9) . 2_655 ?
O5 Mo2 Mo1 143.11(9) . 2_655 ?
O3 Mo2 Mo1 40.60(7) . 2_655 ?
O1 Mo2 Mo1 108.48(7) . 2_655 ?
O2 Mo2 Mo1 34.17(6) 2_655 2_655 ?
OW2 Mo2 Mo1 76.10(7) . 2_655 ?
Mo1 O1 Mo2 134.59(13) . . ?
Mo1 O1 Ho1 111.29(10) . 2_655 ?
Mo2 O1 Ho1 111.38(10) . 2_655 ?
Mo1 O2 Mo2 105.08(10) . 2_645 ?
Mo1 O2 Ho1 146.19(12) . . ?
Mo2 O2 Ho1 108.61(10) 2_645 . ?
Mo2 O3 Mo1 105.08(11) . 2_655 ?
Mo2 O3 Ho1 142.88(13) . 1_565 ?
Mo1 O3 Ho1 106.83(10) 2_655 1_565 ?
Mo1 O4 Ho1 153.94(13) . 3_665 ?
Mo2 O5 Ho1 156.79(14) . 3_665 ?
I1 O6 Ho1 129.23(13) . 4_566 ?
I1 O10 Ho1 145.25(15) . . ?

_refine_diff_density_max         1.022
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.153

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Th
_database_code_depnum_ccdc_archive 'CCDC 1886390'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Thorium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         FIMoO7Th
_chemical_formula_sum            'F I Mo O7 Th'
_chemical_formula_weight         585.88

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   7.261(3)
_cell_length_b                   8.769(4)
_cell_length_c                   21.820(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1389.3(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1590
_cell_measurement_theta_min      3.370
_cell_measurement_theta_max      27.527

_exptl_crystal_description       Octahedral
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    5.602
_exptl_crystal_F_000             2000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    27.645
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_T_max  0.413
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5098
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.370
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1590
_reflns_number_gt                1397
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0454P)²] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1590
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_restrained_S_all      1.200
_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
Th1 Th 0.84140(5) 0.68931(4) 0.38296(2) 0.00650(14) Uani 1 1 d . . . . .
I1 I 0.46878(10) 0.50190(9) 0.27211(3) 0.0143(2) Uani 1 1 d . . . . .
Mo1 Mo 0.83747(12) 0.65759(11) 0.56699(4) 0.0073(2) Uani 1 1 d . . . . .
F1 F 0.7205(9) 0.4480(7) 0.4001(3) 0.0115(13) Uani 1 1 d . . . . .
O2 O 0.5046(11) 0.5135(9) 0.1902(4) 0.0160(17) Uani 1 1 d . . . . .
O3 O 0.6306(12) 0.6720(9) 0.6114(4) 0.0170(19) Uani 1 1 d . . . . .
O4 O 0.9187(11) 0.4677(9) 0.5695(4) 0.0133(16) Uani 1 1 d . . . . .
O5 O 0.5983(14) 0.3302(9) 0.2846(4) 0.0208(19) Uani 1 1 d . . . . .
O6 O 0.6463(12) 0.6333(11) 0.2934(4) 0.026(2) Uani 1 1 d . . . . .
O7 O 0.7997(13) 0.7068(10) 0.4903(4) 0.0183(18) Uani 1 1 d . . . . .
O8 O 1.0067(10) 0.7766(9) 0.5962(4) 0.0148(16) Uani 1 1 d . . . . .


_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
Th1 F1 2.321(6) . ?
Th1 F1 2.342(6) 8_765 ?
Th1 O7 2.367(8) . ?
Th1 O3 2.430(8) 4_566 ?
Th1 O4 2.451(7) 5_766 ?
Th1 O6 2.463(8) . ?
Th1 O8 2.491(8) 4_466 ?
Th1 O5 2.515(8) 8_765 ?
Th1 O2 2.516(8) 6_656 ?
I1 O6 1.790(9) . ?
I1 O5 1.796(9) . ?
I1 O2 1.809(8) . ?
Mo1 O8 1.734(8) . ?
Mo1 O7 1.749(8) . ?
Mo1 O4 1.768(7) . ?
Mo1 O3 1.792(8) . ?
F1 Th1 2.342(6) 8_755 ?
O2 Th1 2.516(8) 6_556 ?
O3 Th1 2.430(8) 4_466 ?
O4 Th1 2.451(7) 5_766 ?
O5 Th1 2.515(8) 8_755 ?
O8 Th1 2.491(8) 4_566 ?

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
F1 Th1 F1 141.69(15) . 8_765 ?
F1 Th1 O7 81.5(3) . . ?
F1 Th1 O7 75.8(3) 8_765 . ?
F1 Th1 O3 140.8(3) . 4_566 ?
F1 Th1 O3 70.9(3) 8_765 4_566 ?
O7 Th1 O3 91.6(3) . 4_566 ?
F1 Th1 O4 71.9(2) . 5_766 ?
F1 Th1 O4 127.8(2) 8_765 5_766 ?
O7 Th1 O4 73.0(3) . 5_766 ?
O3 Th1 O4 69.2(3) 4_566 5_766 ?
F1 Th1 O6 74.2(3) . . ?
F1 Th1 O6 102.1(3) 8_765 . ?
O7 Th1 O6 136.4(3) . . ?
O3 Th1 O6 129.6(3) 4_566 . ?
O4 Th1 O6 129.3(3) 5_766 . ?
F1 Th1 O8 73.2(2) . 4_466 ?
F1 Th1 O8 70.6(2) 8_765 4_466 ?
O7 Th1 O8 71.7(3) . 4_466 ?
O3 Th1 O8 140.7(3) 4_566 4_466 ?
O4 Th1 O8 133.1(3) 5_766 4_466 ?
O6 Th1 O8 66.9(3) . 4_466 ?
F1 Th1 O5 130.6(3) . 8_765 ?
F1 Th1 O5 72.2(3) 8_765 8_765 ?
O7 Th1 O5 146.6(3) . 8_765 ?
O3 Th1 O5 69.3(3) 4_566 8_765 ?
O4 Th1 O5 120.9(3) 5_766 8_765 ?
O6 Th1 O5 61.4(3) . 8_765 ?
O8 Th1 O5 105.5(3) 4_466 8_765 ?
F1 Th1 O2 73.8(2) . 6_656 ?
F1 Th1 O2 141.7(2) 8_765 6_656 ?
O7 Th1 O2 136.7(3) . 6_656 ?
O3 Th1 O2 86.1(3) 4_566 6_656 ?
O4 Th1 O2 65.8(3) 5_766 6_656 ?
O6 Th1 O2 69.2(3) . 6_656 ?
O8 Th1 O2 130.5(3) 4_466 6_656 ?
O5 Th1 O2 71.2(3) 8_765 6_656 ?
O6 I1 O5 97.1(4) . . ?
O6 I1 O2 96.7(4) . . ?
O5 I1 O2 97.0(4) . . ?
O8 Mo1 O7 108.3(4) . . ?
O8 Mo1 O4 108.6(4) . . ?
O7 Mo1 O4 108.3(4) . . ?
O8 Mo1 O3 110.6(4) . . ?
O7 Mo1 O3 111.6(4) . . ?
O4 Mo1 O3 109.2(4) . . ?
Th1 F1 Th1 158.4(3) . 8_755 ?
I1 O2 Th1 126.4(4) . 6_556 ?
Mo1 O3 Th1 141.9(4) . 4_466 ?
Mo1 O4 Th1 141.2(4) . 5_766 ?
I1 O5 Th1 129.2(4) . 8_755 ?
I1 O6 Th1 138.5(5) . . ?
Mo1 O7 Th1 155.6(5) . . ?
Mo1 O8 Th1 146.2(4) . 4_566 ?

_refine_diff_density_max         1.627
_refine_diff_density_min         -3.106
_refine_diff_density_rms         0.480

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Gd
_database_code_depnum_ccdc_archive 'CCDC 1886382'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Gadolinium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         GdIMo2O12'
_chemical_formula_sum            'Gd I Mo2 O12'
_chemical_formula_weight         668.03

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.6068(10)
_cell_length_b                   11.3865(15)
_cell_length_c                   11.3561(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.129(3)
_cell_angle_gamma                90
_cell_volume                     982.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2252
_cell_measurement_theta_min      2.534
_cell_measurement_theta_max      27.559

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.514
_exptl_crystal_F_000             1188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    12.379
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17536
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.534
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2252
_reflns_number_gt                2241
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0670P)²+7.0095P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0232(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2252
_refine_ls_number_parameters     146
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1290
_refine_ls_wR_factor_gt          0.1136
_refine_ls_goodness_of_fit_ref   1.452
_refine_ls_restrained_S_all      1.448
_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
Gd1 Gd 0.57916(5) 0.25600(3) 0.11479(3) 0.0054(2) Uani 1 1 d . . . . .
I1 I 0.38736(7) 0.10705(4) 0.40007(4) 0.0076(2) Uani 1 1 d . . . . .
Mo1 Mo 0.59900(9) 0.59776(6) 0.20352(6) 0.0063(2) Uani 1 1 d . . . . .
Mo2 Mo 0.63941(9) 0.91168(6) 0.16855(6) 0.0058(2) Uani 1 1 d . . . . .
O1 O 0.7060(9) 0.7512(4) 0.2187(5) 0.0076(12) Uani 1 1 d . . . . .
O2 O 0.6512(7) 0.4383(5) 0.1987(5) 0.0080(11) Uani 1 1 d . U . . .
O3 O 0.6982(7) 1.0712(5) 0.1603(5) 0.0076(11) Uani 1 1 d . U . . .
O4 O 0.4968(8) 0.6227(5) 0.0657(5) 0.0115(12) Uani 1 1 d . . . . .
O5 O 0.5455(9) 0.8737(5) 0.0318(6) 0.0134(12) Uani 1 1 d . . . . .
O6 O 0.3420(8) 0.2120(6) 0.5149(5) 0.0128(12) Uani 1 1 d . . . . .
O7 O 0.6180(8) 0.0748(5) 0.4363(5) 0.0115(12) Uani 1 1 d . U . . .
O8 O 0.4265(9) 0.6052(6) 0.2942(6) 0.0182(14) Uani 1 1 d . . . . .
O9 O 0.4584(8) 0.9236(5) 0.2517(6) 0.0131(12) Uani 1 1 d . . . . .
O10 O 0.4172(8) 0.2124(6) 0.2844(5) 0.0161(13) Uani 1 1 d . . . . .
OW1 O 0.2836(10) 0.3142(8) 0.1073(6) 0.0298(18) Uani 1 1 d . . . . .
OW2 O 0.9000(10) 0.8965(6) 0.0604(6) 0.0192(14) Uani 1 1 d . . . . .


_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
Gd1 O2 2.341(6) . ?
Gd1 O3 2.341(5) 1_545 ?
Gd1 OW1 2.343(7) . ?
Gd1 O6 2.363(6) 4_665 ?
Gd1 O10 2.377(6) . ?
Gd1 O5 2.395(6) 3_665 ?
Gd1 O1 2.453(6) 2_645 ?
Gd1 O4 2.521(6) 3_665 ?
Gd1 Mo1 3.6224(8) 2_645 ?
I1 O10 1.799(6) . ?
I1 O6 1.811(6) . ?
I1 O7 1.824(6) . ?
Mo1 O8 1.700(7) . ?
Mo1 O4 1.744(6) . ?
Mo1 O2 1.860(6) . ?
Mo1 O1 1.933(5) . ?
Mo1 O3 2.164(6) 2_645 ?
Mo1 Mo2 3.2163(10) 2_645 ?
Mo1 Gd1 3.6224(8) 2_655 ?
Mo2 O9 1.704(6) . ?
Mo2 O5 1.740(6) . ?
Mo2 O3 1.874(5) . ?
Mo2 O1 1.975(5) . ?
Mo2 O2 2.173(5) 2_655 ?
Mo2 OW2 2.376(7) . ?
Mo2 Mo1 3.2164(10) 2_655 ?
O1 Gd1 2.453(6) 2_655 ?
O2 Mo2 2.173(5) 2_645 ?
O3 Mo1 2.164(6) 2_655 ?
O3 Gd1 2.341(5) 1_565 ?
O4 Gd1 2.521(6) 3_665 ?
O5 Gd1 2.395(6) 3_665 ?
O6 Gd1 2.363(6) 4_566 ?

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
O2 Gd1 O3 128.6(2) . 1_545 ?
O2 Gd1 OW1 88.5(3) . . ?
O3 Gd1 OW1 128.7(3) 1_545 . ?
O2 Gd1 O6 82.5(2) . 4_665 ?
O3 Gd1 O6 85.3(2) 1_545 4_665 ?
OW1 Gd1 O6 140.1(2) . 4_665 ?
O2 Gd1 O10 88.6(2) . . ?
O3 Gd1 O10 80.9(2) 1_545 . ?
OW1 Gd1 O10 64.1(2) . . ?
O6 Gd1 O10 153.4(2) 4_665 . ?
O2 Gd1 O5 155.6(2) . 3_665 ?
O3 Gd1 O5 74.9(2) 1_545 3_665 ?
OW1 Gd1 O5 78.1(3) . 3_665 ?
O6 Gd1 O5 94.7(2) 4_665 3_665 ?
O10 Gd1 O5 103.3(2) . 3_665 ?
O2 Gd1 O1 64.33(18) . 2_645 ?
O3 Gd1 O1 64.44(18) 1_545 2_645 ?
OW1 Gd1 O1 130.2(2) . 2_645 ?
O6 Gd1 O1 79.8(2) 4_665 2_645 ?
O10 Gd1 O1 73.8(2) . 2_645 ?
O5 Gd1 O1 139.21(18) 3_665 2_645 ?
O2 Gd1 O4 83.6(2) . 3_665 ?
O3 Gd1 O4 138.3(2) 1_545 3_665 ?
OW1 Gd1 O4 68.0(2) . 3_665 ?
O6 Gd1 O4 72.4(2) 4_665 3_665 ?
O10 Gd1 O4 131.5(2) . 3_665 ?
O5 Gd1 O4 72.5(2) 3_665 3_665 ?
O1 Gd1 O4 139.90(19) 2_645 3_665 ?
O2 Gd1 Mo1 93.79(13) . 2_645 ?
O3 Gd1 Mo1 34.85(14) 1_545 2_645 ?
OW1 Gd1 Mo1 142.06(17) . 2_645 ?
O6 Gd1 Mo1 77.54(15) 4_665 2_645 ?
O10 Gd1 Mo1 78.13(15) . 2_645 ?
O5 Gd1 Mo1 109.32(14) 3_665 2_645 ?
O1 Gd1 Mo1 29.91(12) 2_645 2_645 ?
O4 Gd1 Mo1 149.92(14) 3_665 2_645 ?
O10 I1 O6 96.8(3) . . ?
O10 I1 O7 98.8(3) . . ?
O6 I1 O7 100.3(3) . . ?
O8 Mo1 O4 102.0(3) . . ?
O8 Mo1 O2 103.7(3) . . ?
O4 Mo1 O2 102.8(3) . . ?
O8 Mo1 O1 103.5(3) . . ?
O4 Mo1 O1 96.0(3) . . ?
O2 Mo1 O1 142.7(3) . . ?
O8 Mo1 O3 96.9(3) . 2_645 ?
O4 Mo1 O3 161.0(3) . 2_645 ?
O2 Mo1 O3 74.8(2) . 2_645 ?
O1 Mo1 O3 77.0(2) . 2_645 ?
O8 Mo1 Mo2 103.7(2) . 2_645 ?
O4 Mo1 Mo2 139.5(2) . 2_645 ?
O2 Mo1 Mo2 40.62(17) . 2_645 ?
O1 Mo1 Mo2 107.68(18) . 2_645 ?
O3 Mo1 Mo2 34.18(14) 2_645 2_645 ?
O8 Mo1 Gd1 98.7(2) . 2_655 ?
O4 Mo1 Gd1 134.4(2) . 2_655 ?
O2 Mo1 Gd1 111.21(17) . 2_655 ?
O1 Mo1 Gd1 39.27(18) . 2_655 ?
O3 Mo1 Gd1 38.17(14) 2_645 2_655 ?
Mo2 Mo1 Gd1 71.14(2) 2_645 2_655 ?
O9 Mo2 O5 101.6(3) . . ?
O9 Mo2 O3 98.6(3) . . ?
O5 Mo2 O3 106.7(3) . . ?
O9 Mo2 O1 96.8(3) . . ?
O5 Mo2 O1 96.9(3) . . ?
O3 Mo2 O1 148.5(3) . . ?
O9 Mo2 O2 101.0(3) . 2_655 ?
O5 Mo2 O2 156.9(3) . 2_655 ?
O3 Mo2 O2 74.3(2) . 2_655 ?
O1 Mo2 O2 75.8(2) . 2_655 ?
O9 Mo2 OW2 177.4(3) . . ?
O5 Mo2 OW2 81.0(3) . . ?
O3 Mo2 OW2 80.8(2) . . ?
O1 Mo2 OW2 82.6(3) . . ?
O2 Mo2 OW2 76.4(2) 2_655 . ?
O9 Mo2 Mo1 101.3(2) . 2_655 ?
O5 Mo2 Mo1 142.5(2) . 2_655 ?
O3 Mo2 Mo1 40.46(17) . 2_655 ?
O1 Mo2 Mo1 109.36(18) . 2_655 ?
O2 Mo2 Mo1 33.86(15) 2_655 2_655 ?
OW2 Mo2 Mo1 76.54(17) . 2_655 ?
Mo1 O1 Mo2 135.1(3) . . ?
Mo1 O1 Gd1 110.8(2) . 2_655 ?
Mo2 O1 Gd1 111.0(2) . 2_655 ?
Mo1 O2 Mo2 105.5(3) . 2_645 ?
Mo1 O2 Gd1 146.2(3) . . ?
Mo2 O2 Gd1 108.3(2) 2_645 . ?
Mo2 O3 Mo1 105.4(3) . 2_655 ?
Mo2 O3 Gd1 142.3(3) . 1_565 ?
Mo1 O3 Gd1 107.0(2) 2_655 1_565 ?
Mo1 O4 Gd1 154.1(3) . 3_665 ?
Mo2 O5 Gd1 155.9(3) . 3_665 ?
I1 O6 Gd1 129.4(3) . 4_566 ?
I1 O10 Gd1 144.5(4) . . ?

_refine_diff_density_max         5.136
_refine_diff_density_min         -5.649
_refine_diff_density_rms         1.383

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Y
_database_code_depnum_ccdc_archive 'CCDC 1886389'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Yttrium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         IMo2O12Y
_chemical_formula_sum            'I Mo2 O12 Y'
_chemical_formula_weight         599.69

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5639(6)
_cell_length_b                   11.3372(9)
_cell_length_c                   11.2573(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.219(2)
_cell_angle_gamma                90
_cell_volume                     964.63(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2227
_cell_measurement_theta_min      3.188
_cell_measurement_theta_max      27.597

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.129
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    11.785
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19679
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.188
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2227
_reflns_number_gt                2159
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+4.3740P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00479(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2227
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0467
_refine_ls_wR_factor_gt          0.0464
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_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
Y1 Y 0.58158(5) 0.25586(3) 0.11605(3) 0.00618(9) Uani 1 1 d . . . . .
I1 I 0.38703(3) 0.10818(2) 0.40058(2) 0.00732(8) Uani 1 1 d . . . . .
Mo1 Mo 0.59737(4) 0.59656(3) 0.20351(3) 0.00660(9) Uani 1 1 d . . . . .
Mo2 Mo 0.63725(4) 0.91148(3) 0.16753(3) 0.00589(9) Uani 1 1 d . . . . .
O1 O 0.7051(4) 0.7508(2) 0.2201(2) 0.0085(5) Uani 1 1 d . . . . .
O2 O 0.6524(3) 0.4357(2) 0.1979(2) 0.0081(5) Uani 1 1 d . . . . .
O3 O 0.6969(3) 1.0718(2) 0.1600(2) 0.0093(5) Uani 1 1 d . . . . .
O4 O 0.4948(4) 0.6220(2) 0.0642(2) 0.0110(6) Uani 1 1 d . . . . .
O5 O 0.5431(4) 0.8719(2) 0.0302(2) 0.0126(6) Uani 1 1 d . . . . .
O6 O 0.3420(4) 0.2130(2) 0.5167(2) 0.0119(6) Uani 1 1 d . . . . .
O7 O 0.6178(4) 0.0743(2) 0.4369(2) 0.0111(5) Uani 1 1 d . . . . .
O8 O 0.4231(4) 0.6028(3) 0.2940(3) 0.0153(6) Uani 1 1 d . . . . .
O9 O 0.4544(4) 0.9238(3) 0.2515(3) 0.0138(6) Uani 1 1 d . . . . .
O10 O 0.4221(4) 0.2135(3) 0.2852(2) 0.0142(6) Uani 1 1 d . . . . .
OW1 O 0.2910(4) 0.3161(3) 0.1077(3) 0.0255(8) Uani 1 1 d . . . . .
OW2 O 0.8987(4) 0.8964(3) 0.0597(3) 0.0155(6) Uani 1 1 d . . . . .


_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
Y1 O2 2.293(3) . ?
Y1 OW1 2.300(3) . ?
Y1 O3 2.308(3) 1_545 ?
Y1 O6 2.330(3) 4_665 ?
Y1 O10 2.343(3) . ?
Y1 O5 2.362(3) 3_665 ?
Y1 O1 2.404(3) 2_645 ?
Y1 O4 2.505(3) 3_665 ?
Y1 Mo1 3.5922(5) 2_645 ?
Y1 Mo2 3.6291(5) 2_645 ?
I1 O10 1.791(3) . ?
I1 O6 1.808(3) . ?
I1 O7 1.819(3) . ?
Mo1 O8 1.698(3) . ?
Mo1 O4 1.747(3) . ?
Mo1 O2 1.872(3) . ?
Mo1 O1 1.935(3) . ?
Mo1 O3 2.163(3) 2_645 ?
Mo1 Mo2 3.2116(5) 2_645 ?
Mo1 Y1 3.5921(5) 2_655 ?
Mo2 O9 1.711(3) . ?
Mo2 O5 1.736(3) . ?
Mo2 O3 1.875(3) . ?
Mo2 O1 1.978(3) . ?
Mo2 O2 2.172(3) 2_655 ?
Mo2 OW2 2.366(3) . ?
Mo2 Mo1 3.2116(5) 2_655 ?
Mo2 Y1 3.6291(5) 2_655 ?
O1 Y1 2.404(3) 2_655 ?
O2 Mo2 2.172(3) 2_645 ?
O3 Mo1 2.163(3) 2_655 ?
O3 Y1 2.308(3) 1_565 ?
O4 Y1 2.505(3) 3_665 ?
O5 Y1 2.362(3) 3_665 ?
O6 Y1 2.330(3) 4_566 ?

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
O2 Y1 OW1 87.73(12) . . ?
O2 Y1 O3 129.63(10) . 1_545 ?
OW1 Y1 O3 129.02(11) . 1_545 ?
O2 Y1 O6 82.50(10) . 4_665 ?
OW1 Y1 O6 139.45(11) . 4_665 ?
O3 Y1 O6 85.44(10) 1_545 4_665 ?
O2 Y1 O10 88.59(10) . . ?
OW1 Y1 O10 64.71(10) . . ?
O3 Y1 O10 80.94(10) 1_545 . ?
O6 Y1 O10 153.24(10) 4_665 . ?
O2 Y1 O5 155.02(9) . 3_665 ?
OW1 Y1 O5 78.37(12) . 3_665 ?
O3 Y1 O5 74.46(9) 1_545 3_665 ?
O6 Y1 O5 94.61(10) 4_665 3_665 ?
O10 Y1 O5 103.68(10) . 3_665 ?
O2 Y1 O1 64.76(9) . 2_645 ?
OW1 Y1 O1 130.57(10) . 2_645 ?
O3 Y1 O1 64.98(9) 1_545 2_645 ?
O6 Y1 O1 79.47(10) 4_665 2_645 ?
O10 Y1 O1 73.91(9) . 2_645 ?
O5 Y1 O1 139.30(9) 3_665 2_645 ?
O2 Y1 O4 82.93(9) . 3_665 ?
OW1 Y1 O4 67.22(10) . 3_665 ?
O3 Y1 O4 138.29(9) 1_545 3_665 ?
O6 Y1 O4 72.55(9) 4_665 3_665 ?
O10 Y1 O4 131.43(10) . 3_665 ?
O5 Y1 O4 72.60(9) 3_665 3_665 ?
O1 Y1 O4 139.61(9) 2_645 3_665 ?
O2 Y1 Mo1 94.46(7) . 2_645 ?
OW1 Y1 Mo1 142.78(8) . 2_645 ?
O3 Y1 Mo1 35.19(7) 1_545 2_645 ?
O6 Y1 Mo1 77.42(7) 4_665 2_645 ?
O10 Y1 Mo1 78.19(7) . 2_645 ?
O5 Y1 Mo1 109.20(7) 3_665 2_645 ?
O1 Y1 Mo1 30.12(6) 2_645 2_645 ?
O4 Y1 Mo1 149.94(7) 3_665 2_645 ?
O2 Y1 Mo2 34.52(6) . 2_645 ?
OW1 Y1 Mo2 114.67(9) . 2_645 ?
O3 Y1 Mo2 95.11(7) 1_545 2_645 ?
O6 Y1 Mo2 76.37(7) 4_665 2_645 ?
O10 Y1 Mo2 82.00(7) . 2_645 ?
O5 Y1 Mo2 166.90(7) 3_665 2_645 ?
O1 Y1 Mo2 30.47(6) 2_645 2_645 ?
O4 Y1 Mo2 112.70(6) 3_665 2_645 ?
Mo1 Y1 Mo2 59.934(10) 2_645 2_645 ?
O10 I1 O6 97.09(13) . . ?
O10 I1 O7 97.81(13) . . ?
O6 I1 O7 100.49(12) . . ?
O8 Mo1 O4 101.76(14) . . ?
O8 Mo1 O2 103.85(13) . . ?
O4 Mo1 O2 102.85(12) . . ?
O8 Mo1 O1 103.79(13) . . ?
O4 Mo1 O1 96.21(12) . . ?
O2 Mo1 O1 142.18(11) . . ?
O8 Mo1 O3 97.65(12) . 2_645 ?
O4 Mo1 O3 160.36(12) . 2_645 ?
O2 Mo1 O3 75.08(11) . 2_645 ?
O1 Mo1 O3 76.11(11) . 2_645 ?
O8 Mo1 Mo2 104.00(10) . 2_645 ?
O4 Mo1 Mo2 139.64(9) . 2_645 ?
O2 Mo1 Mo2 40.80(8) . 2_645 ?
O1 Mo1 Mo2 107.04(8) . 2_645 ?
O3 Mo1 Mo2 34.30(7) 2_645 2_645 ?
O8 Mo1 Y1 99.40(10) . 2_655 ?
O4 Mo1 Y1 133.76(9) . 2_655 ?
O2 Mo1 Y1 111.26(8) . 2_655 ?
O1 Mo1 Y1 38.56(8) . 2_655 ?
O3 Mo1 Y1 37.95(7) 2_645 2_655 ?
Mo2 Mo1 Y1 71.084(12) 2_645 2_655 ?
O9 Mo2 O5 101.55(14) . . ?
O9 Mo2 O3 98.47(13) . . ?
O5 Mo2 O3 107.53(12) . . ?
O9 Mo2 O1 96.64(13) . . ?
O5 Mo2 O1 96.97(12) . . ?
O3 Mo2 O1 147.83(11) . . ?
O9 Mo2 O2 100.99(12) . 2_655 ?
O5 Mo2 O2 156.68(12) . 2_655 ?
O3 Mo2 O2 74.81(11) . 2_655 ?
O1 Mo2 O2 74.52(10) . 2_655 ?
O9 Mo2 OW2 177.26(12) . . ?
O5 Mo2 OW2 81.18(12) . . ?
O3 Mo2 OW2 80.76(11) . . ?
O1 Mo2 OW2 82.80(11) . . ?
O2 Mo2 OW2 76.27(10) 2_655 . ?
O9 Mo2 Mo1 101.64(10) . 2_655 ?
O5 Mo2 Mo1 143.05(10) . 2_655 ?
O3 Mo2 Mo1 40.55(8) . 2_655 ?
O1 Mo2 Mo1 108.43(8) . 2_655 ?
O2 Mo2 Mo1 34.27(7) 2_655 2_655 ?
OW2 Mo2 Mo1 76.05(7) . 2_655 ?
O9 Mo2 Y1 97.70(10) . 2_655 ?
O5 Mo2 Y1 132.98(9) . 2_655 ?
O3 Mo2 Y1 111.47(8) . 2_655 ?
O1 Mo2 Y1 38.04(8) . 2_655 ?
O2 Mo2 Y1 36.75(7) 2_655 2_655 ?
OW2 Mo2 Y1 80.19(7) . 2_655 ?
Mo1 Mo2 Y1 70.995(11) 2_655 2_655 ?
Mo1 O1 Mo2 134.43(14) . . ?
Mo1 O1 Y1 111.33(11) . 2_655 ?
Mo2 O1 Y1 111.49(11) . 2_655 ?
Mo1 O2 Mo2 104.93(12) . 2_645 ?
Mo1 O2 Y1 146.23(14) . . ?
Mo2 O2 Y1 108.73(11) 2_645 . ?
Mo2 O3 Mo1 105.15(12) . 2_655 ?
Mo2 O3 Y1 142.81(14) . 1_565 ?
Mo1 O3 Y1 106.87(11) 2_655 1_565 ?
Mo1 O4 Y1 154.05(15) . 3_665 ?
Mo2 O5 Y1 156.69(16) . 3_665 ?
I1 O6 Y1 129.28(14) . 4_566 ?
I1 O10 Y1 145.21(16) . . ?

_refine_diff_density_max         0.884
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.156

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Er
_database_code_depnum_ccdc_archive 'CCDC 1886386'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Erbium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         ErIMo2O12
_chemical_formula_sum            'Er I Mo2 O12'
_chemical_formula_weight         678.04

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5508(4)
_cell_length_b                   11.3352(6)
_cell_length_c                   11.2366(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.3336(16)
_cell_angle_gamma                90
_cell_volume                     960.94(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2222
_cell_measurement_theta_min      2.553
_cell_measurement_theta_max      27.575

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.687
_exptl_crystal_F_000             1204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    14.494
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25584
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.553
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2222
_reflns_number_gt                2102
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0135P)²+3.2673P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00240(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2222
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0165
_refine_ls_wR_factor_ref         0.0378
_refine_ls_wR_factor_gt          0.0372
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_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
Er1 Er 0.58233(2) 0.25556(2) 0.11639(2) 0.00666(6) Uani 1 1 d . . . . .
I1 I 0.38698(3) 0.10913(2) 0.40077(2) 0.00850(7) Uani 1 1 d . . . . .
Mo1 Mo 0.59761(4) 0.59598(3) 0.20260(3) 0.00741(8) Uani 1 1 d . . . . .
Mo2 Mo 0.63568(4) 0.91124(3) 0.16778(3) 0.00677(8) Uani 1 1 d . . . . .
O1 O 0.7049(4) 0.7506(2) 0.2202(3) 0.0096(6) Uani 1 1 d . . . . .
O2 O 0.6530(4) 0.4353(2) 0.1972(2) 0.0097(5) Uani 1 1 d . . . . .
O3 O 0.6960(4) 1.0719(2) 0.1601(2) 0.0102(6) Uani 1 1 d . . . . .
O4 O 0.4945(4) 0.6219(2) 0.0632(3) 0.0131(6) Uani 1 1 d . . . . .
O5 O 0.5408(4) 0.8711(2) 0.0303(2) 0.0143(6) Uani 1 1 d . . . . .
O6 O 0.3414(4) 0.2145(3) 0.5173(3) 0.0149(6) Uani 1 1 d . . . . .
O7 O 0.6181(4) 0.0748(2) 0.4378(3) 0.0130(6) Uani 1 1 d . . . . .
O8 O 0.4231(4) 0.6015(3) 0.2929(3) 0.0176(6) Uani 1 1 d . . . . .
O9 O 0.4537(4) 0.9236(3) 0.2521(3) 0.0166(6) Uani 1 1 d . . . . .
O10 O 0.4225(4) 0.2143(3) 0.2848(3) 0.0172(6) Uani 1 1 d . . . . .
OW1 O 0.2916(4) 0.3146(4) 0.1075(3) 0.0298(9) Uani 1 1 d . . . . .
OW2 O 0.8972(4) 0.8968(3) 0.0588(3) 0.0202(7) Uani 1 1 d . . . . .


_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
Er1 O2 2.285(3) . ?
Er1 O3 2.297(3) 1_545 ?
Er1 OW1 2.293(3) . ?
Er1 O6 2.315(3) 4_665 ?
Er1 O10 2.333(3) . ?
Er1 O5 2.349(3) 3_665 ?
Er1 O1 2.391(3) 2_645 ?
Er1 O4 2.498(3) 3_665 ?
I1 O10 1.794(3) . ?
I1 O6 1.816(3) . ?
I1 O7 1.819(3) . ?
Mo1 O8 1.697(3) . ?
Mo1 O4 1.746(3) . ?
Mo1 O2 1.870(3) . ?
Mo1 O1 1.937(3) . ?
Mo1 O3 2.165(3) 2_645 ?
Mo1 Mo2 3.2129(5) 2_645 ?
Mo2 O9 1.706(3) . ?
Mo2 O5 1.736(3) . ?
Mo2 O3 1.880(3) . ?
Mo2 O1 1.978(3) . ?
Mo2 O2 2.174(3) 2_655 ?
Mo2 OW2 2.371(3) . ?
Mo2 Mo1 3.2129(5) 2_655 ?
O1 Er1 2.391(3) 2_655 ?
O2 Mo2 2.174(3) 2_645 ?
O3 Mo1 2.165(3) 2_655 ?
O3 Er1 2.297(3) 1_565 ?
O4 Er1 2.498(3) 3_665 ?
O5 Er1 2.349(3) 3_665 ?
O6 Er1 2.315(3) 4_566 ?

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
O2 Er1 O3 130.09(10) . 1_545 ?
O2 Er1 OW1 87.97(12) . . ?
O3 Er1 OW1 128.49(12) 1_545 . ?
O2 Er1 O6 82.65(10) . 4_665 ?
O3 Er1 O6 85.40(10) 1_545 4_665 ?
OW1 Er1 O6 139.70(11) . 4_665 ?
O2 Er1 O10 88.66(11) . . ?
O3 Er1 O10 81.14(10) 1_545 . ?
OW1 Er1 O10 64.40(11) . . ?
O6 Er1 O10 153.45(10) 4_665 . ?
O2 Er1 O5 154.57(9) . 3_665 ?
O3 Er1 O5 74.34(9) 1_545 3_665 ?
OW1 Er1 O5 78.30(12) . 3_665 ?
O6 Er1 O5 94.02(11) 4_665 3_665 ?
O10 Er1 O5 104.12(11) . 3_665 ?
O2 Er1 O1 64.99(9) . 2_645 ?
O3 Er1 O1 65.22(9) 1_545 2_645 ?
OW1 Er1 O1 130.72(11) . 2_645 ?
O6 Er1 O1 79.51(10) 4_665 2_645 ?
O10 Er1 O1 74.09(10) . 2_645 ?
O5 Er1 O1 139.37(9) 3_665 2_645 ?
O2 Er1 O4 82.41(9) . 3_665 ?
O3 Er1 O4 138.50(9) 1_545 3_665 ?
OW1 Er1 O4 67.19(11) . 3_665 ?
O6 Er1 O4 72.74(10) 4_665 3_665 ?
O10 Er1 O4 130.99(10) . 3_665 ?
O5 Er1 O4 72.58(10) 3_665 3_665 ?
O1 Er1 O4 139.47(9) 2_645 3_665 ?
O10 I1 O6 97.17(14) . . ?
O10 I1 O7 97.92(13) . . ?
O6 I1 O7 100.58(13) . . ?
O8 Mo1 O4 101.64(14) . . ?
O8 Mo1 O2 103.61(13) . . ?
O4 Mo1 O2 103.12(12) . . ?
O8 Mo1 O1 103.73(13) . . ?
O4 Mo1 O1 96.23(12) . . ?
O2 Mo1 O1 142.29(12) . . ?
O8 Mo1 O3 97.61(13) . 2_645 ?
O4 Mo1 O3 160.47(12) . 2_645 ?
O2 Mo1 O3 75.22(11) . 2_645 ?
O1 Mo1 O3 75.85(11) . 2_645 ?
O8 Mo1 Mo2 103.91(10) . 2_645 ?
O4 Mo1 Mo2 139.91(10) . 2_645 ?
O2 Mo1 Mo2 40.82(8) . 2_645 ?
O1 Mo1 Mo2 106.95(8) . 2_645 ?
O3 Mo1 Mo2 34.42(7) 2_645 2_645 ?
O9 Mo2 O5 101.70(15) . . ?
O9 Mo2 O3 98.50(13) . . ?
O5 Mo2 O3 107.76(12) . . ?
O9 Mo2 O1 96.86(13) . . ?
O5 Mo2 O1 96.78(12) . . ?
O3 Mo2 O1 147.57(12) . . ?
O9 Mo2 O2 100.77(13) . 2_655 ?
O5 Mo2 O2 156.67(13) . 2_655 ?
O3 Mo2 O2 74.81(11) . 2_655 ?
O1 Mo2 O2 74.35(11) . 2_655 ?
O9 Mo2 OW2 177.22(13) . . ?
O5 Mo2 OW2 81.08(13) . . ?
O3 Mo2 OW2 80.48(11) . . ?
O1 Mo2 OW2 82.82(11) . . ?
O2 Mo2 OW2 76.47(11) 2_655 . ?
O9 Mo2 Mo1 101.47(10) . 2_655 ?
O5 Mo2 Mo1 143.35(10) . 2_655 ?
O3 Mo2 Mo1 40.61(8) . 2_655 ?
O1 Mo2 Mo1 108.18(8) . 2_655 ?
O2 Mo2 Mo1 34.21(7) 2_655 2_655 ?
OW2 Mo2 Mo1 76.06(8) . 2_655 ?
Mo1 O1 Mo2 134.29(15) . . ?
Mo1 O1 Er1 111.40(12) . 2_655 ?
Mo2 O1 Er1 111.60(11) . 2_655 ?
Mo1 O2 Mo2 104.97(12) . 2_645 ?
Mo1 O2 Er1 146.35(14) . . ?
Mo2 O2 Er1 108.55(11) 2_645 . ?
Mo2 O3 Mo1 104.96(12) . 2_655 ?
Mo2 O3 Er1 142.99(14) . 1_565 ?
Mo1 O3 Er1 106.86(11) 2_655 1_565 ?
Mo1 O4 Er1 154.00(15) . 3_665 ?
Mo2 O5 Er1 157.14(16) . 3_665 ?
I1 O6 Er1 129.17(15) . 4_566 ?
I1 O10 Er1 145.07(17) . . ?

_refine_diff_density_max         0.939
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.191

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tm
_database_code_depnum_ccdc_archive 'CCDC 1886387'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Thulium molybdate iodate'
_chemical_melting_point          N/A
_chemical_formula_moiety         IMo2O12Tm
_chemical_formula_sum            'I Mo2 O12 Tm'
_chemical_formula_weight         679.71

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.5360(6)
_cell_length_b                   11.3220(9)
_cell_length_c                   11.1946(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.284(2)
_cell_angle_gamma                90
_cell_volume                     954.39(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2202
_cell_measurement_theta_min      3.249
_cell_measurement_theta_max      27.565

_exptl_crystal_description       Tablet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      'Not measured'
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    4.730
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    15.096
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_process_details   SHELTXPREP
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Turbo X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21351
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.249
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2202
_reflns_number_gt                2139
_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0146P)²+2.9943P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00252(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2202
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0161
_refine_ls_wR_factor_ref         0.0390
_refine_ls_wR_factor_gt          0.0387
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_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
Tm1 Tm 0.58293(2) 0.25568(2) 0.11676(2) 0.00567(6) Uani 1 1 d . . . . .
I1 I 0.38694(3) 0.10897(2) 0.40108(2) 0.00768(7) Uani 1 1 d . . . . .
Mo1 Mo 0.59687(4) 0.59589(3) 0.20297(3) 0.00657(8) Uani 1 1 d . . . . .
Mo2 Mo 0.63584(4) 0.91135(3) 0.16713(3) 0.00574(8) Uani 1 1 d . . . . .
O1 O 0.7047(4) 0.75046(19) 0.2205(2) 0.0089(5) Uani 1 1 d . . . . .
O2 O 0.6526(3) 0.4351(2) 0.1975(2) 0.0084(5) Uani 1 1 d . . . . .
O3 O 0.6966(3) 1.0724(2) 0.1599(2) 0.0088(5) Uani 1 1 d . . . . .
O4 O 0.4939(4) 0.6221(2) 0.0627(2) 0.0116(5) Uani 1 1 d . . . . .
O5 O 0.5407(4) 0.8706(2) 0.0290(2) 0.0123(5) Uani 1 1 d . . . . .
O6 O 0.3421(4) 0.2140(2) 0.5184(2) 0.0133(5) Uani 1 1 d . . . . .
O7 O 0.6186(3) 0.0742(2) 0.4380(2) 0.0114(5) Uani 1 1 d . . . . .
O8 O 0.4222(4) 0.6014(2) 0.2941(2) 0.0156(6) Uani 1 1 d . . . . .
O9 O 0.4531(4) 0.9237(2) 0.2520(3) 0.0144(6) Uani 1 1 d . . . . .
O10 O 0.4233(4) 0.2152(3) 0.2857(2) 0.0157(6) Uani 1 1 d . . . . .
OW1 O 0.2941(4) 0.3159(3) 0.1082(3) 0.0256(7) Uani 1 1 d . . . . .
OW2 O 0.8978(4) 0.8969(2) 0.0594(3) 0.0173(6) Uani 1 1 d . . . . .


_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
Tm1 O2 2.276(2) . ?
Tm1 O3 2.289(2) 1_545 ?
Tm1 OW1 2.279(3) . ?
Tm1 O6 2.306(3) 4_665 ?
Tm1 O10 2.328(3) . ?
Tm1 O5 2.335(3) 3_665 ?
Tm1 O1 2.377(3) 2_645 ?
Tm1 O4 2.488(3) 3_665 ?
I1 O10 1.794(3) . ?
I1 O6 1.813(3) . ?
I1 O7 1.821(3) . ?
Mo1 O8 1.698(3) . ?
Mo1 O4 1.749(3) . ?
Mo1 O2 1.870(2) . ?
Mo1 O1 1.936(2) . ?
Mo1 O3 2.159(3) 2_645 ?
Mo1 Mo2 3.2099(5) 2_645 ?
Mo2 O9 1.710(3) . ?
Mo2 O5 1.741(3) . ?
Mo2 O3 1.883(2) . ?
Mo2 O1 1.980(2) . ?
Mo2 O2 2.172(3) 2_655 ?
Mo2 OW2 2.360(3) . ?
Mo2 Mo1 3.2099(5) 2_655 ?
O1 Tm1 2.377(3) 2_655 ?
O2 Mo2 2.172(3) 2_645 ?
O3 Mo1 2.159(3) 2_655 ?
O3 Tm1 2.289(2) 1_565 ?
O4 Tm1 2.488(3) 3_665 ?
O5 Tm1 2.335(3) 3_665 ?
O6 Tm1 2.306(3) 4_566 ?

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
O2 Tm1 O3 130.30(9) . 1_545 ?
O2 Tm1 OW1 87.40(11) . . ?
O3 Tm1 OW1 128.96(11) 1_545 . ?
O2 Tm1 O6 82.53(10) . 4_665 ?
O3 Tm1 O6 85.35(9) 1_545 4_665 ?
OW1 Tm1 O6 139.55(10) . 4_665 ?
O2 Tm1 O10 88.38(10) . . ?
O3 Tm1 O10 81.45(10) 1_545 . ?
OW1 Tm1 O10 64.49(10) . . ?
O6 Tm1 O10 153.20(10) 4_665 . ?
O2 Tm1 O5 154.56(9) . 3_665 ?
O3 Tm1 O5 74.22(9) 1_545 3_665 ?
OW1 Tm1 O5 78.46(11) . 3_665 ?
O6 Tm1 O5 94.56(10) 4_665 3_665 ?
O10 Tm1 O5 104.04(10) . 3_665 ?
O2 Tm1 O1 65.19(8) . 2_645 ?
O3 Tm1 O1 65.23(8) 1_545 2_645 ?
OW1 Tm1 O1 130.70(10) . 2_645 ?
O6 Tm1 O1 79.20(10) 4_665 2_645 ?
O10 Tm1 O1 74.11(10) . 2_645 ?
O5 Tm1 O1 139.29(8) 3_665 2_645 ?
O2 Tm1 O4 82.35(9) . 3_665 ?
O3 Tm1 O4 138.37(9) 1_545 3_665 ?
OW1 Tm1 O4 66.95(10) . 3_665 ?
O6 Tm1 O4 72.91(9) 4_665 3_665 ?
O10 Tm1 O4 130.86(9) . 3_665 ?
O5 Tm1 O4 72.70(9) 3_665 3_665 ?
O1 Tm1 O4 139.51(8) 2_645 3_665 ?
O10 I1 O6 96.90(13) . . ?
O10 I1 O7 97.83(12) . . ?
O6 I1 O7 100.48(12) . . ?
O8 Mo1 O4 101.93(13) . . ?
O8 Mo1 O2 103.67(12) . . ?
O4 Mo1 O2 103.17(11) . . ?
O8 Mo1 O1 103.77(12) . . ?
O4 Mo1 O1 96.12(12) . . ?
O2 Mo1 O1 142.12(12) . . ?
O8 Mo1 O3 97.55(12) . 2_645 ?
O4 Mo1 O3 160.20(11) . 2_645 ?
O2 Mo1 O3 75.35(10) . 2_645 ?
O1 Mo1 O3 75.61(10) . 2_645 ?
O8 Mo1 Mo2 103.84(10) . 2_645 ?
O4 Mo1 Mo2 139.92(9) . 2_645 ?
O2 Mo1 Mo2 40.85(8) . 2_645 ?
O1 Mo1 Mo2 106.80(8) . 2_645 ?
O3 Mo1 Mo2 34.51(7) 2_645 2_645 ?
O9 Mo2 O5 101.71(14) . . ?
O9 Mo2 O3 98.49(12) . . ?
O5 Mo2 O3 108.12(12) . . ?
O9 Mo2 O1 96.59(12) . . ?
O5 Mo2 O1 96.75(11) . . ?
O3 Mo2 O1 147.45(12) . . ?
O9 Mo2 O2 100.78(12) . 2_655 ?
O5 Mo2 O2 156.57(12) . 2_655 ?
O3 Mo2 O2 74.77(10) . 2_655 ?
O1 Mo2 O2 74.16(10) . 2_655 ?
O9 Mo2 OW2 176.85(12) . . ?
O5 Mo2 OW2 81.43(12) . . ?
O3 Mo2 OW2 80.53(10) . . ?
O1 Mo2 OW2 82.84(11) . . ?
O2 Mo2 OW2 76.09(10) 2_655 . ?
O9 Mo2 Mo1 101.54(9) . 2_655 ?
O5 Mo2 Mo1 143.50(9) . 2_655 ?
O3 Mo2 Mo1 40.51(8) . 2_655 ?
O1 Mo2 Mo1 108.06(8) . 2_655 ?
O2 Mo2 Mo1 34.27(6) 2_655 2_655 ?
OW2 Mo2 Mo1 75.76(7) . 2_655 ?
Mo1 O1 Mo2 134.19(15) . . ?
Mo1 O1 Tm1 111.53(11) . 2_655 ?
Mo2 O1 Tm1 111.63(11) . 2_655 ?
Mo1 O2 Mo2 104.89(11) . 2_645 ?
Mo1 O2 Tm1 146.45(13) . . ?
Mo2 O2 Tm1 108.54(10) 2_645 . ?
Mo2 O3 Mo1 104.97(11) . 2_655 ?
Mo2 O3 Tm1 142.89(14) . 1_565 ?
Mo1 O3 Tm1 106.96(10) 2_655 1_565 ?
Mo1 O4 Tm1 154.15(14) . 3_665 ?
Mo2 O5 Tm1 157.20(14) . 3_665 ?
I1 O6 Tm1 129.02(14) . 4_566 ?
I1 O10 Tm1 144.66(16) . . ?

_refine_diff_density_max         1.103
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.226

