Solvatomorphic diversity dictates the stability and solubility of metal-organic polyhedra.
Yadav, Ankit K.; Gładysiak, Andrzej; Wolpert, Emma H.; Ganose, Alex M.; Samel-Garloff, Bronson; Koley, Dipankar; Jelfs, Kim E.; Stylianou, Kyriakos C.; Chemical science 16 (2025) 2589–2599; doi:10.1039/d4sc05037a

data_1573438
_publ_section_title
;
 Solvatomorphic diversity dictates the stability and solubility of
 metal-organic polyhedra.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2589
_journal_page_last               2599
_journal_paper_doi               10.1039/d4sc05037a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '0.5(C192 H120 Mo24 N24 O144), 6(C2 H8 N)'
_chemical_formula_sum            'C108 H108 Mo12 N18 O72'
_chemical_formula_weight         3961.40
_chemical_properties_physical    Hygroscopic,Deliquescent
_space_group_crystal_system      hexagonal
_space_group_IT_number           175
_space_group_name_Hall           '-P 6'
_space_group_name_H-M_alt        'P 6/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   20.6212(3)
_cell_length_b                   20.6212(3)
_cell_length_c                   15.9529(3)
_cell_measurement_reflns_used    21841
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      77.5830
_cell_measurement_theta_min      2.4810
_cell_volume                     5874.87(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  44.00   1.00    3.00    --   46.89 -39.00-165.00   58
  2  \w   -122.00 -96.00   1.00   15.00    --  -86.25 -89.00  -3.00   26
  3  \w   -155.00 -75.00   1.00   15.00    --  -86.25 -39.00-165.00   80
  4  \w    118.00 174.00   1.00   15.00    --  107.75 104.00-157.00   56
  5  \w     40.00 105.00   1.00   15.00    --  107.75 -89.00  -3.00   65
  6  \w   -118.00 -93.00   1.00    3.00    --  -46.89 -77.00  90.00   25
  7  \w    -26.00  27.00   1.00    3.00    --  -46.89  19.00  60.00   53
  8  \w   -116.00 -78.00   1.00    3.00    --  -46.89-125.00 -60.00   38
  9  \w   -118.00 -93.00   1.00    3.00    --  -46.89 -77.00 120.00   25
 10  \w   -118.00 -82.00   1.00    3.00    --  -46.89-125.00 -90.00   36
 11  \w     44.00  86.00   1.00    3.00    --   46.89-125.00  60.00   42
 12  \w    126.00 178.00   1.00   15.00    --  107.75  77.00 150.00   52
 13  \w     85.00 111.00   1.00   15.00    --  107.75  77.00 150.00   26
 14  \w     39.00  81.00   1.00   15.00    --  107.75 -77.00  90.00   42
 15  \w     40.00  66.00   1.00   15.00    --  107.75 -61.00  30.00   26
 16  \w     36.00 105.00   1.00   15.00    --  107.75 -77.00-150.00   69
 17  \w     37.00  72.00   1.00   15.00    --  107.75 -77.00   0.00   35
 18  \w     76.00 106.00   1.00   15.00    --  107.75 -77.00   0.00   30
 19  \w     96.00 163.00   1.00   15.00    --  107.75  15.00 -30.00   67
 20  \w     40.00  65.00   1.00   15.00    --  107.75 -77.00  30.00   25
 21  \w     35.00  61.00   1.00   15.00    --  107.75 -61.00-180.00   26
 22  \w    107.00 178.00   1.00   15.00    --  107.75  30.00  30.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388641000
_diffrn_orient_matrix_UB_12      0.0007665000
_diffrn_orient_matrix_UB_13      0.0822026000
_diffrn_orient_matrix_UB_21      -0.0767828000
_diffrn_orient_matrix_UB_22      -0.0428498000
_diffrn_orient_matrix_UB_23      -0.0436787000
_diffrn_orient_matrix_UB_31      -0.0060818000
_diffrn_orient_matrix_UB_32      -0.0747951000
_diffrn_orient_matrix_UB_33      0.0258327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.793
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.350
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4302
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.1340
_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/[\s^2^(Fo^2^)+(0.1208P)^2^+103.3306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3398
_refine_ls_wR_factor_ref         0.3421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4101
_reflns_number_total             4302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05037a2.cif
_cod_data_source_block           beaver-106
_cod_depositor_comments
'Adding full bibliography for 1573437--1573441.cif.'
_cod_original_cell_volume        5874.9(2)
_cod_database_code               1573438
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Mo C N O'
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.954(3)
 0.046(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C2-C1
 1.51 with sigma of 0.02
 C61-N61
 1.47 with sigma of 0.02
 O6-C1 \\sim C1-O5
 with sigma of 0.02
 O5-C2 \\sim C2-O6
 with sigma of 0.02
 Mo2-O3 \\sim O3-Mo1
 with sigma of 0.02
 C61-N61 \\sim N61-C62
 with sigma of 0.02
4. Restrained planarity
 C12, C33, C11, C13, C31, C32, C34, C35
 with sigma of 0.1
 C1, C2, C3, C4, C6, C7, C8, N1
 with sigma of 0.1
5. Rigid bond restraints
 C12, C33, C11, C13, C32, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 C1, O5, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, O32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, O7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Uiso/Uaniso restraints and constraints
C2 \\sim C3: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
C1 \\sim O5 \\sim O6: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
C6 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C7 \\sim C8: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
C3 \\sim C4: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
C4 \\sim C5: within 2A with sigma of 0.0005 and sigma for terminal atoms of
0.001 within 2A
C4 \\sim C8: within 2A with sigma of 0.0005 and sigma for terminal atoms of
0.001 within 2A
C5 \\sim O8: within 2A with sigma of 0.00005 and sigma for terminal atoms of
0.0001 within 2A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.000005 and sigma for terminal atoms of
0.00001
Uanis(O8) \\sim Ueq: with sigma of 0.00005 and sigma for terminal atoms of
0.0001
Uanis(C5) = Uanis(C1)
Uanis(O8) = Uanis(O6)
Uanis(O8) = Uanis(O7) = Uanis(O33) = Uanis(O34)
Uanis(C5) = Uanis(C35)
Uanis(O8) = Uanis(O7)
Uanis(C62) = Uanis(C61)
7. Rigid body (RIGU) restrains
 C12, C33, N31, C11, C13, C31, C32, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C62, N61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Fixed Sof: H33(0.5) H31A(0.5) H31B(0.5) C1(0.5) C2(0.5) C3(0.5) H3(0.5)
 C4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C11(0.5) H11(0.5)
 C13(0.5) H13(0.5) C31(0.5) C32(0.5) C34(0.5) C35(0.5) Mo1(0.5) Mo2(0.5)
 N1(0.5) H1A(0.5) H1B(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) O6(0.5)
 O7(0.5) O8(0.5) O31(0.5) O32(0.5) O33(0.5) O34(0.5) C61(0.5) H61A(0.5)
 H61B(0.5) H61C(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) N61(0.5) H61D(0.5)
 H61E(0.5)
9.a Secondary CH2 refined with riding coordinates:
 N61(H61D,H61E)
9.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C3(H3), C6(H6), C8(H8), C11(H11), C13(H13)
9.c X=CH2 refined with riding coordinates:
 N31(H31A,H31B), N1(H1A,H1B)
9.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              77114
_shelx_hkl_checksum              11304
_shelx_fab_checksum              16976
_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 3.603
_oxdiff_exptl_absorpt_empirical_full_min 0.389