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_1573440
_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         'C96 H60 Mo12 N12 O72, 12(C4 H12 N)'
_chemical_formula_sum            'C144 H204 Mo12 N24 O72'
_chemical_formula_weight         4574.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-17 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.6430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.4926(3)
_cell_length_b                   21.0361(2)
_cell_length_c                   24.7119(3)
_cell_measurement_reflns_used    46360
_cell_measurement_temperature    156(9)
_cell_measurement_theta_max      77.5390
_cell_measurement_theta_min      3.1930
_cell_volume                     11867.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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      156(9)
_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 0.983
_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   -121.00 -66.00   1.00   10.00    --  -47.14 -32.00 125.00   55
  2  \w    -33.00  -7.00   1.00   10.00    --  -47.14  32.00 -75.00   26
  3  \w     34.00  71.00   1.00   10.00    --   47.14  32.00 -75.00   37
  4  \w    -23.00  36.00   1.00   10.00    --   47.14 -32.00 125.00   59
  5  \w   -141.00-116.00   1.00   35.00    --  -86.25 -32.00 125.00   25
  6  \w    -37.00 -12.00   1.00   35.00    --  -86.25  32.00 -75.00   25
  7  \w     95.00 178.00   1.00   35.00    --  107.75  32.00 -75.00   83
  8  \w   -117.00 -85.00   1.00   10.00    --  -47.14 -77.00  30.00   32
  9  \w   -118.00 -86.00   1.00   10.00    --  -47.14 -77.00 120.00   32
 10  \w   -115.00 -87.00   1.00   10.00    --  -47.14 -77.00 -30.00   28
 11  \w   -119.00 -87.00   1.00   10.00    --  -47.14 -77.00 -90.00   32
 12  \w   -114.00 -79.00   1.00   10.00    --  -47.14-125.00 -60.00   35
 13  \w     44.00  69.00   1.00   10.00    --   47.14  37.00   0.00   25
 14  \w    -27.00  25.00   1.00   10.00    --   47.14 -19.00   0.00   52
 15  \w     91.00 116.00   1.00   10.00    --   47.14  57.00  90.00   25
 16  \w     39.00  85.00   1.00   10.00    --   47.14  57.00   0.00   46
 17  \w     32.00  99.00   1.00   10.00    --   47.14  57.00  60.00   67
 18  \w     36.00  85.00   1.00   10.00    --   47.14  57.00  90.00   49
 19  \w     88.00 114.00   1.00   10.00    --   47.14  57.00   0.00   26
 20  \w    -93.00 -68.00   1.00   35.00    --  -86.25 -66.00  73.34   25
 21  \w    -97.00 -71.00   1.00   35.00    --  -86.25 -64.00  32.22   26
 22  \w    -94.00 -68.00   1.00   35.00    --  -86.25 -68.00  -9.18   26
 23  \w    -92.00 -67.00   1.00   35.00    --  -86.25 -68.00  16.60   25
 24  \w    -94.00 -68.00   1.00   35.00    --  -86.25 -66.00 -17.40   26
 25  \w   -156.00-119.00   1.00   35.00    --  -86.25 -94.00-120.00   37
 26  \w    -95.00 -68.00   1.00   35.00    --  -86.25 -65.00 -32.17   27
 27  \w   -159.00-118.00   1.00   35.00    --  -86.25 -65.00 -32.17   41
 28  \w   -102.00 -76.00   1.00   35.00    --  -86.25 -45.00  60.00   26
 29  \w    -94.00 -68.00   1.00   35.00    --  -86.25 -66.00   1.67   26
 30  \w    -93.00 -67.00   1.00   35.00    --  -86.25 -68.00  25.44   26
 31  \w    -92.00 -67.00   1.00   35.00    --  -86.25 -67.00  51.74   25
 32  \w    -93.00 -67.00   1.00   35.00    --  -86.25 -67.00  58.35   26
 33  \w    -94.00 -69.00   1.00   35.00    --  -86.25 -64.00  67.28   25
 34  \w    -94.00 -68.00   1.00   35.00    --  -86.25 -66.00  42.35   26
 35  \w    -93.00 -67.00   1.00   35.00    --  -86.25 -67.00  -4.05   26
 36  \w    -94.00 -68.00   1.00   35.00    --  -86.25 -68.00  16.26   26
 37  \w    -93.00 -68.00   1.00   35.00    --  -86.25 -65.00  34.50   25
 38  \w    -95.00 -70.00   1.00   35.00    --  -86.25 -59.00  68.96   25
 39  \w   -139.00-113.00   1.00   35.00    --  -86.25 -68.00  28.27   26
 40  \w    -92.00 -67.00   1.00   35.00    --  -86.25 -67.00  53.63   25
 41  \w    -92.00 -67.00   1.00   35.00    --  -86.25 -68.00  28.27   25
 42  \w   -115.00 -89.00   1.00   35.00    --  -86.25 -94.00-120.00   26
 43  \w    -99.00 -73.00   1.00   35.00    --  -86.25 -55.00  47.60   26
 44  \w    -92.00 -67.00   1.00   35.00    --  -86.25 -68.00  68.21   25
 45  \w    -97.00 -71.00   1.00   35.00    --  -86.25 -63.00   3.74   26
 46  \w     91.00 175.00   1.00   35.00    --  107.75  61.00  90.00   84
 47  \w     70.00  96.00   1.00   35.00    --  107.75 -77.00 150.00   26
 48  \w     66.00 101.00   1.00   35.00    --  107.75-125.00  90.00   35
 49  \w     35.00  61.00   1.00   35.00    --  107.75 -77.00 150.00   26
 50  \w    136.00 169.00   1.00   35.00    --  107.75  77.00   0.00   33
 51  \w     37.00  70.00   1.00   35.00    --  107.75 -61.00 -60.00   33
 52  \w     85.00 112.00   1.00   35.00    --  107.75  77.00   0.00   27
 53  \w     41.00  67.00   1.00   35.00    --  107.75-125.00-180.00   26
 54  \w    143.00 174.00   1.00   35.00    --  107.75  45.00 -60.00   31
 55  \w     93.00 175.00   1.00   35.00    --  107.75  61.00   0.00   82
 56  \w    100.00 126.00   1.00   35.00    --  107.75  45.00 -60.00   26
 57  \w     93.00 124.00   1.00   35.00    --  107.75  61.00  30.00   31
 58  \w    127.00 153.00   1.00   35.00    --  107.75  61.00 -30.00   26
 59  \w     35.00  71.00   1.00   35.00    --  107.75 -61.00-120.00   36
 60  \w     86.00 112.00   1.00   35.00    --  107.75-125.00-180.00   26
 61  \w     91.00 129.00   1.00   35.00    --  107.75  61.00  60.00   38
 62  \w     35.00  71.00   1.00   35.00    --  107.75 -61.00-150.00   36
 63  \w     94.00 119.00   1.00   35.00    --  107.75  61.00 -30.00   25
 64  \w    115.00 170.00   1.00   35.00    --  107.75  77.00 -30.00   55
 65  \w     41.00  70.00   1.00   35.00    --  107.75 -61.00   0.00   29
 66  \w     36.00 106.00   1.00   35.00    --  107.75 -77.00-150.00   70
 67  \w     95.00 154.00   1.00   35.00    --  107.75  45.00  60.00   59
 68  \w     85.00 111.00   1.00   35.00    --  107.75  77.00 -30.00   26
 69  \w     38.00  93.00   1.00   35.00    --  107.75 -77.00-180.00   55
 70  \w    148.00 173.00   1.00   35.00    --  107.75  77.00  60.00   25
 71  \w     87.00 113.00   1.00   35.00    --  107.75  77.00  30.00   26
 72  \w     85.00 116.00   1.00   35.00    --  107.75  77.00  60.00   31
 73  \w     39.00 106.00   1.00   35.00    --  107.75 -77.00 -60.00   67
 74  \w     35.00  61.00   1.00   35.00    --  107.75 -61.00 150.00   26
 75  \w     37.00  63.00   1.00   35.00    --  107.75 -61.00  30.00   26
 76  \w     35.00  60.00   1.00   35.00    --  107.75 -61.00 -30.00   25
;
_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      0.0622798000
_diffrn_orient_matrix_UB_12      -0.0268345000
_diffrn_orient_matrix_UB_13      0.0212888000
_diffrn_orient_matrix_UB_21      -0.0132622000
_diffrn_orient_matrix_UB_22      -0.0135231000
_diffrn_orient_matrix_UB_23      0.0570512000
_diffrn_orient_matrix_UB_31      -0.0223304000
_diffrn_orient_matrix_UB_32      -0.0667974000
_diffrn_orient_matrix_UB_33      -0.0201357000
_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  0.1342
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            218226
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.884
_diffrn_reflns_theta_min         2.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (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    1.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.239
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         24921
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+46.0129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20248
_reflns_number_total             24921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05037a2.cif
_cod_data_source_block           beaver-108
_cod_depositor_comments
'Adding full bibliography for 1573437--1573441.cif.'
_cod_database_code               1573440
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Mo C N O'
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N101-C104
 2.5 with sigma of 0.02
 C93-C91
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N51) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N21)
\\sim Ueq, Uanis(N41) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C74) \\sim Ueq, Uanis(N71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(N111) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(N101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C101) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(N61)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C83) \\sim Ueq, Uanis(N81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(N91) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C93) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C104) \\sim Ueq, Uanis(N101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C101) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(N91) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C91) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C93) = Uanis(C94)
4.a Rotating group:
 N1(H1A,H1B), N11(H11A,H11B), N21(H21A,H21B), N31(H31A,H31B), N41(H41A,H41B)
4.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B), N61(H61C,H61D), C71(H71A,H71B), C72(H72A,
 H72B), N71(H71C,H71D), C81(H81A,H81B), C82(H82A,H82B), N81(H81C,H81D),
 C91(H91A,H91B), C92(H92A,H92B), N91(H91C,H91D), C101(H10A,H10B), C102(H10C,
 H10D), N101(H10K,H10L), C111(H11C,H11D), C112(H11E,H11F), N111(H11M,H11N)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C13(H13), C16(H16), C18(H18), C23(H23), C26(H26),
 C28(H28), C33(H33), C36(H36), C38(H38), C43(H43), C46(H46), C48(H48), C53(H53),
  C56(H56), C58(H58)
4.d X=CH2 refined with riding coordinates:
 N51(H51A,H51B)
4.e Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C), C103(H10E,H10F,H10G), C104(H10H,H10I,H10J), C113(H11G,H11H,H11I),
 C114(H11J,H11K,H11L)
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              92337
_shelx_hkl_checksum              2810
_shelx_fab_checksum              75286
_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 5.462
_oxdiff_exptl_absorpt_empirical_full_min 0.282