# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2111565'
_audit_update_record             
;
2021-09-23 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_audit_creation_date             2021-06-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H2 I4 Mo2 O18, H2 O, 2(C H6 N3)'
_chemical_formula_sum            'C2 H15 I4 Mo2 N6 O19'
_chemical_formula_weight         1126.68
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   23.8979(5)
_cell_length_b                   13.1994(3)
_cell_length_c                   7.8514(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2476.63(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8060
_cell_measurement_theta_min      2.2730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'New Gemini, Dual, Cu at zero, EosS2'
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31269
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.926
_diffrn_reflns_theta_min         2.299
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  74.00   0.50    0.33    --    4.56  77.00 120.00  156
  2  ω     -6.00  77.00   0.50    0.33    --    4.56  37.00  60.00  166
  3  ω    -21.00  38.00   0.50    0.33    --    4.56 -99.00 -60.00  118
  4  ω    -21.00  34.00   0.50    0.33    --    4.56 -99.00 -30.00  110
  5  ω      2.00  28.00   0.50    0.33    --   -5.65 -99.00  60.00   52
  6  ω    -78.00 -35.00   0.50    0.33    --   -5.65 -57.00-150.00   86
  7  ω     -1.00  18.50   0.50    0.33    --   -5.65 -99.00 150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141527000
_diffrn_orient_matrix_UB_12      -0.0115250000
_diffrn_orient_matrix_UB_13      0.0467288000
_diffrn_orient_matrix_UB_21      0.0258114000
_diffrn_orient_matrix_UB_22      -0.0067189000
_diffrn_orient_matrix_UB_23      -0.0262039000
_diffrn_orient_matrix_UB_31      0.0037754000
_diffrn_orient_matrix_UB_32      0.0893735000
_diffrn_orient_matrix_UB_33      0.0040639000
_diffrn_oxdiff_digest_frames     
;
017013c837595d93800f5330efc52051fd00042c312
;
_diffrn_oxdiff_digest_hkl        
;
015fc6b961d6216ca48ea53c07a7ffe2db178f
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.688
_reflns_number_gt                5540
_reflns_number_total             6226
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.885
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0522P)²+4.9427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0911
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All O(H,H) groups
3.a Riding coordinates:
 O18(H18A,H18B), O19(H19), O19(H1)
3.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N2(H2A,H2B), N6(H6A,H6B), N5(H5A,H5B), N1(H1A,H1B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
I2 I 0.71402(2) 0.76550(4) 0.72593(7) 0.01682(13) Uani 1 1 d . . . . .
I3 I 0.69495(2) 0.76610(4) 0.23365(8) 0.01833(13) Uani 1 1 d . . . . .
I1 I 0.71556(2) 0.49881(4) 0.48843(7) 0.02004(13) Uani 1 1 d . . . . .
I4 I 0.71854(2) 1.03055(4) 0.47929(8) 0.02188(14) Uani 1 1 d . . . . .
Mo1 Mo 0.59125(3) 0.62824(6) 0.52477(12) 0.02436(19) Uani 1 1 d . . . . .
Mo2 Mo 0.59286(3) 0.90888(6) 0.52292(12) 0.02286(18) Uani 1 1 d . . . . .
O6 O 0.6654(3) 0.6623(5) 0.6871(8) 0.0235(14) Uani 1 1 d . . . . .
O8 O 0.6672(3) 0.8737(5) 0.6850(8) 0.0227(14) Uani 1 1 d . . . . .
O7 O 0.7510(3) 0.7652(5) 0.5257(10) 0.0264(14) Uani 1 1 d . . . . .
O3 O 0.6384(3) 0.4971(4) 0.5115(10) 0.0245(14) Uani 1 1 d . . . . .
O11 O 0.6568(3) 0.8722(5) 0.3237(9) 0.0247(15) Uani 1 1 d . . . . .
O15 O 0.6417(3) 1.0371(5) 0.5087(9) 0.0267(15) Uani 1 1 d . . . . .
O9 O 0.6559(3) 0.6601(5) 0.3224(9) 0.0246(14) Uani 1 1 d . . . . .
O2 O 0.7164(3) 0.4200(6) 0.3008(10) 0.0341(18) Uani 1 1 d . . . . .
O10 O 0.6622(4) 0.7660(5) 0.0285(10) 0.0307(16) Uani 1 1 d . . . . .
O17 O 0.7212(4) 1.1059(6) 0.2880(10) 0.0372(19) Uani 1 1 d . . . . .
O16 O 0.7349(4) 1.1232(6) 0.6358(12) 0.043(2) Uani 1 1 d . . . . .
O12 O 0.5784(3) 0.7680(5) 0.5252(12) 0.0305(17) Uani 1 1 d . . . . .
O1 O 0.7290(4) 0.4079(7) 0.6498(11) 0.041(2) Uani 1 1 d . . . . .
O4 O 0.5571(3) 0.5919(6) 0.7029(12) 0.044(2) Uani 1 1 d . . . . .
O14 O 0.5603(3) 0.9483(6) 0.7045(11) 0.0384(18) Uani 1 1 d . . . . .
O18 O 0.6620(4) 0.5176(7) 0.9707(13) 0.053(2) Uani 1 1 d . . . . .
H18A H 0.652581 0.517515 1.088876 0.063 Uiso 1 1 d R . . . .
H18B H 0.690711 0.467925 0.953516 0.063 Uiso 1 1 d R . . . .
O13 O 0.5476(4) 0.9466(7) 0.3707(11) 0.043(2) Uani 1 1 d . . . . .
O19 O 0.8276(4) 0.5121(7) 0.4501(14) 0.058(3) Uani 1 1 d . . . . .
H19 H 0.821528 0.505647 0.338750 0.070 Uiso 1 1 d R . . . .
H1 H 0.799378 0.545977 0.497250 0.070 Uiso 1 1 d R . . . .
O5 O 0.5467(3) 0.5928(6) 0.3695(13) 0.044(2) Uani 1 1 d . . . . .
N3 N 0.5748(6) 0.3584(9) 0.808(2) 0.087(6) Uani 1 1 d . . . . .
H3A H 0.539900 0.373351 0.798394 0.105 Uiso 1 1 calc R . . . .
H3B H 0.598723 0.405090 0.831389 0.105 Uiso 1 1 calc R . . . .
N4 N 0.6294(7) 0.2588(11) 0.247(4) 0.116(10) Uani 1 1 d . . . . .
H4A H 0.652637 0.308482 0.252181 0.139 Uiso 1 1 calc R . . . .
H4B H 0.640636 0.199949 0.215200 0.139 Uiso 1 1 calc R . . . .
N2 N 0.5562(6) 0.1940(12) 0.754(3) 0.097(7) Uani 1 1 d . . . . .
H2A H 0.521187 0.207998 0.743392 0.117 Uiso 1 1 calc R . . . .
H2B H 0.567628 0.132746 0.740687 0.117 Uiso 1 1 calc R . . . .
N6 N 0.5563(5) 0.3607(10) 0.339(2) 0.085(5) Uani 1 1 d . . . . .
H6A H 0.520842 0.369776 0.350534 0.102 Uiso 1 1 calc R . . . .
H6B H 0.579089 0.409548 0.360058 0.102 Uiso 1 1 calc R . . . .
C2 C 0.5754(7) 0.2733(14) 0.290(4) 0.087(8) Uani 1 1 d . . . . .
N5 N 0.5401(6) 0.1971(14) 0.257(3) 0.130(11) Uani 1 1 d . . . . .
H5A H 0.504620 0.205862 0.268253 0.156 Uiso 1 1 calc R . . . .
H5B H 0.552861 0.139348 0.224326 0.156 Uiso 1 1 calc R . . . .
N1 N 0.6447(10) 0.2397(16) 0.822(5) 0.184(17) Uani 1 1 d . . . . .
H1A H 0.654768 0.177167 0.821080 0.221 Uiso 1 1 calc R . . . .
H1B H 0.668731 0.286157 0.845860 0.221 Uiso 1 1 calc R . . . .
C1 C 0.5914(6) 0.2648(12) 0.788(3) 0.060(5) 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
I2 O6 1.816(7) . ?
I2 O8 1.843(7) . ?
I2 O7 1.803(7) . ?
I3 O11 1.814(7) . ?
I3 O9 1.820(7) . ?
I3 O10 1.791(8) . ?
I1 O3 1.854(6) . ?
I1 O2 1.803(7) . ?
I1 O1 1.775(8) . ?
I4 O15 1.854(7) . ?
I4 O17 1.803(8) . ?
I4 O16 1.777(8) . ?
Mo1 O6 2.229(7) . ?
Mo1 O3 2.067(6) . ?
Mo1 O9 2.256(7) . ?
Mo1 O12 1.870(6) . ?
Mo1 O4 1.688(8) . ?
Mo1 O5 1.685(8) . ?
Mo2 O8 2.233(7) . ?
Mo2 O11 2.240(7) . ?
Mo2 O15 2.058(6) . ?
Mo2 O12 1.892(6) . ?
Mo2 O14 1.706(8) . ?
Mo2 O13 1.686(7) . ?
N3 C1 1.307(18) . ?
N4 C2 1.35(3) . ?
N2 C1 1.29(2) . ?
N6 C2 1.30(2) . ?
C2 N5 1.34(2) . ?
N1 C1 1.34(3) . ?

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
O6 I2 O8 99.4(3) . . ?
O7 I2 O6 99.5(3) . . ?
O7 I2 O8 98.4(3) . . ?
O11 I3 O9 100.8(3) . . ?
O10 I3 O11 97.6(3) . . ?
O10 I3 O9 96.9(3) . . ?
O2 I1 O3 94.8(3) . . ?
O1 I1 O3 95.9(4) . . ?
O1 I1 O2 101.0(4) . . ?
O17 I4 O15 96.5(4) . . ?
O16 I4 O15 95.7(4) . . ?
O16 I4 O17 100.9(4) . . ?
O6 Mo1 O9 79.7(2) . . ?
O3 Mo1 O6 76.4(2) . . ?
O3 Mo1 O9 75.4(3) . . ?
O12 Mo1 O6 86.0(3) . . ?
O12 Mo1 O3 156.3(3) . . ?
O12 Mo1 O9 86.0(3) . . ?
O4 Mo1 O6 88.1(4) . . ?
O4 Mo1 O3 93.9(3) . . ?
O4 Mo1 O9 165.3(3) . . ?
O4 Mo1 O12 101.5(4) . . ?
O5 Mo1 O6 166.5(4) . . ?
O5 Mo1 O3 94.3(3) . . ?
O5 Mo1 O9 88.6(4) . . ?
O5 Mo1 O12 99.9(4) . . ?
O5 Mo1 O4 102.4(5) . . ?
O8 Mo2 O11 79.1(2) . . ?
O15 Mo2 O8 75.6(3) . . ?
O15 Mo2 O11 75.7(2) . . ?
O12 Mo2 O8 86.3(3) . . ?
O12 Mo2 O11 85.3(3) . . ?
O12 Mo2 O15 155.9(3) . . ?
O14 Mo2 O8 87.2(3) . . ?
O14 Mo2 O11 164.0(3) . . ?
O14 Mo2 O15 93.0(3) . . ?
O14 Mo2 O12 102.0(4) . . ?
O13 Mo2 O8 167.1(4) . . ?
O13 Mo2 O11 90.4(4) . . ?
O13 Mo2 O15 94.7(4) . . ?
O13 Mo2 O12 100.3(4) . . ?
O13 Mo2 O14 102.1(4) . . ?
I2 O6 Mo1 139.1(4) . . ?
I2 O8 Mo2 138.0(3) . . ?
I1 O3 Mo1 122.5(3) . . ?
I3 O11 Mo2 141.4(4) . . ?
I4 O15 Mo2 122.0(3) . . ?
I3 O9 Mo1 139.8(4) . . ?
Mo1 O12 Mo2 160.0(4) . . ?
N6 C2 N4 122.4(16) . . ?
N6 C2 N5 120.3(16) . . ?
N5 C2 N4 116.7(18) . . ?
N3 C1 N1 119.8(17) . . ?
N2 C1 N3 120.9(16) . . ?
N2 C1 N1 118.9(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.734
_oxdiff_exptl_absorpt_empirical_full_min 0.681
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.94(3)
2 0.06(3)

