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_1573437
_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, 48(C3 H7 N O), 12(C2 H8 N)'
_chemical_formula_sum            'C126 H170 Mo12 N26 O74'
_chemical_formula_weight         4384.15
_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                 104.0860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.4316(3)
_cell_length_b                   20.2535(3)
_cell_length_c                   24.6419(3)
_cell_measurement_reflns_used    32674
_cell_measurement_temperature    157(10)
_cell_measurement_theta_max      76.0330
_cell_measurement_theta_min      2.8550
_cell_volume                     11342.7(3)
_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      157(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 0.984
_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    -69.00  23.00   1.00    8.00    --  -47.14  93.00-119.00   92
  2  \w     32.00  70.00   1.00    8.00    --   47.14 -93.00 128.00   38
  3  \w    -13.00  27.00   1.00    8.00    --   47.14 -93.00 128.00   40
  4  \w    -70.00 -45.00   1.00   30.00    --  -86.25  93.00-119.00   25
  5  \w    148.00 174.00   1.00   30.00    --  107.75  93.00-119.00   26
  6  \w    111.00 136.00   1.00   30.00    --  107.75  93.00-119.00   25
  7  \w    -39.00  17.00   1.00    8.00    --  -47.14  37.00  60.00   56
  8  \w   -116.00 -85.00   1.00    8.00    --  -47.14 -77.00 -30.00   31
  9  \w   -118.00 -89.00   1.00    8.00    --  -47.14 -77.00-180.00   29
 10  \w   -119.00 -94.00   1.00    8.00    --  -47.14 -77.00 150.00   25
 11  \w     85.00 110.00   1.00    8.00    --   47.14  77.00 -90.00   25
 12  \w     86.00 111.00   1.00    8.00    --   47.14  77.00 150.00   25
 13  \w     92.00 119.00   1.00    8.00    --   47.14  77.00-150.00   27
 14  \w     67.00  95.00   1.00    8.00    --   47.14-125.00 120.00   28
 15  \w     86.00 113.00   1.00    8.00    --   47.14  77.00-120.00   27
 16  \w    -17.00  25.00   1.00    8.00    --   47.14 -19.00-120.00   42
 17  \w     89.00 115.00   1.00    8.00    --   47.14  77.00 -60.00   26
 18  \w     87.00 113.00   1.00    8.00    --   47.14  77.00 -30.00   26
 19  \w    -26.00  41.00   1.00    8.00    --   47.14 -37.00 120.00   67
 20  \w   -145.00-120.00   1.00   30.00    --  -86.25 -93.00 128.00   25
 21  \w    -49.00 -17.00   1.00   30.00    --  -86.25  45.00 -90.00   32
 22  \w     94.00 138.00   1.00   30.00    --  107.75  61.00-180.00   44
 23  \w     96.00 176.00   1.00   30.00    --  107.75  45.00  90.00   80
 24  \w     44.00  69.00   1.00   30.00    --  107.75 -94.00  30.00   25
 25  \w     36.00 102.00   1.00   30.00    --  107.75 -77.00 -90.00   66
 26  \w     67.00  94.00   1.00   30.00    --  107.75 -77.00-180.00   27
 27  \w     35.00 102.00   1.00   30.00    --  107.75 -94.00 -90.00   67
 28  \w     99.00 178.00   1.00   30.00    --  107.75  45.00 -30.00   79
 29  \w     37.00  63.00   1.00   30.00    --  107.75 -77.00-180.00   26
 30  \w    129.00 175.00   1.00   30.00    --  107.75  45.00-150.00   46
 31  \w     91.00 173.00   1.00   30.00    --  107.75  61.00 -60.00   82
 32  \w     36.00 106.00   1.00   30.00    --  107.75 -77.00  60.00   70
 33  \w     37.00  69.00   1.00   30.00    --  107.75 -61.00 -60.00   32
 34  \w    139.00 176.00   1.00   30.00    --  107.75  15.00  30.00   37
 35  \w     71.00 106.00   1.00   30.00    --  107.75 -94.00-180.00   35
 36  \w     42.00  70.00   1.00   30.00    --  107.75 -61.00-180.00   28
 37  \w     85.00 119.00   1.00   30.00    --  107.75  77.00-180.00   34
 38  \w     39.00  78.00   1.00   30.00    --  107.75 -77.00 120.00   39
 39  \w     39.00  65.00   1.00   30.00    --  107.75 -94.00-180.00   26
 40  \w    147.00 175.00   1.00   30.00    --  107.75  61.00-180.00   28
 41  \w     44.00  71.00   1.00   30.00    --  107.75 -61.00  60.00   27
 42  \w     37.00  63.00   1.00   30.00    --  107.75 -61.00-150.00   26
 43  \w     98.00 123.00   1.00   30.00    --  107.75  61.00  60.00   25
 44  \w    132.00 157.00   1.00   30.00    --  107.75  61.00  60.00   25
 45  \w     36.00 105.00   1.00   30.00    --  107.75 -94.00  60.00   69
 46  \w     35.00  70.00   1.00   30.00    --  107.75 -61.00 -30.00   35
 47  \w     79.00 104.00   1.00   30.00    --  107.75 -94.00-150.00   25
 48  \w    110.00 164.00   1.00   30.00    --  107.75  45.00   0.00   54
 49  \w     72.00 103.00   1.00   30.00    --  107.75 -93.00 128.00   31
;
_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      0.0258154000
_diffrn_orient_matrix_UB_12      -0.0700624000
_diffrn_orient_matrix_UB_13      0.0114164000
_diffrn_orient_matrix_UB_21      -0.0260121000
_diffrn_orient_matrix_UB_22      -0.0054745000
_diffrn_orient_matrix_UB_23      0.0515298000
_diffrn_orient_matrix_UB_31      -0.0570036000
_diffrn_orient_matrix_UB_32      -0.0291892000
_diffrn_orient_matrix_UB_33      -0.0369753000
_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  0.0917
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            150150
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.870
_diffrn_reflns_theta_min         2.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67741
_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    1.284
_exptl_crystal_description       prism
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         23869
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0865
_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^)+(0.1053P)^2^+280.5682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19835
_reflns_number_total             23869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05037a2.cif
_cod_data_source_block           beaver-105
_cod_depositor_comments
'Adding full bibliography for 1573437--1573441.cif.'
_cod_database_code               1573437
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Mo C N O'
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. 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
2. Restrained distances
 N111-C111
 1.47 with sigma of 0.02
 N111-C112
 1.47 with sigma of 0.02
 C3S-C2S
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C111 \\sim N111: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(N1S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(O1S) \\sim Ueq, Uanis(C2S)
\\sim Ueq, Uanis(C3S) \\sim Ueq: with sigma of 0.025 and sigma for terminal
atoms of 0.05
Uanis(C2S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(N91)
\\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(N101) \\sim Ueq,
Uanis(C101) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N41) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N61) \\sim Ueq, Uanis(N91)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(N111) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N31) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C91) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C102) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1S, C2S, C3S, N1S, O1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C111, C112, N111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 N11(H11A,H11B), N21(H21A,H21B), N31(H31A,H31B), N41(H41A,H41B), N51(H51A,H51B)
5.b Secondary CH2 refined with riding coordinates:
 N61(H61D,H61E), N71(H71D,H71E), N81(H81D,H81E), N91(H91D,H91E), N101(H10G,
 H10H), N111(H11I,H11J)
5.c Me refined with riding coordinates:
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C111(H11C,H11D,H11E), C112(H11F,
 H11G,H11H)
5.d 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), C1S(H1S)
5.e X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.f Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              93754
_shelx_hkl_checksum              55690
_shelx_fab_checksum              75690
_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 2.273
_oxdiff_exptl_absorpt_empirical_full_min 0.713