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_1573441
_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 H58 Mo12 N12 O72, 8(C2 H8 N)'
_chemical_formula_sum            'C112 H122 Mo12 N20 O72'
_chemical_formula_weight         4051.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-29
_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                90
_cell_formula_units_Z            4
_cell_length_a                   37.4589(18)
_cell_length_b                   29.3487(9)
_cell_length_c                   20.1896(6)
_cell_measurement_reflns_used    8200
_cell_measurement_temperature    150.5(9)
_cell_measurement_theta_max      71.9060
_cell_measurement_theta_min      2.9090
_cell_volume                     22195.8(14)
_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      150.5(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_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    -15.00  44.00   1.00   12.00    --   46.89 -40.00 124.00   59
  2  \w   -143.00-115.00   1.00   40.00    --  -86.25 -40.00 124.00   28
  3  \w   -148.00-112.00   1.00   40.00    --  -86.25 -93.00 -80.00   36
  4  \w    -45.00 -18.00   1.00   40.00    --  -86.25  40.00 -82.00   27
  5  \w    126.00 177.00   1.00   40.00    --  104.22  97.00 128.00   51
  6  \w   -107.00 -79.00   1.00   12.00    --  -46.89-125.00 -30.00   28
  7  \w    -14.00  26.00   1.00   12.00    --  -46.89  19.00  60.00   40
  8  \w     85.00 110.00   1.00   12.00    --   46.89  77.00-120.00   25
  9  \w    -25.00  21.00   1.00   12.00    --   46.89 -19.00   0.00   46
 10  \w     91.00 118.00   1.00   12.00    --   46.89  77.00  30.00   27
 11  \w     86.00 115.00   1.00   12.00    --   46.89  77.00   0.00   29
 12  \w    153.00 178.00   1.00   40.00    --  104.22  30.00-120.00   25
 13  \w     35.00  66.00   1.00   40.00    --  104.22 -61.00  30.00   31
 14  \w     95.00 149.00   1.00   40.00    --  104.22  30.00-120.00   54
 15  \w     32.00  71.00   1.00   40.00    --  104.22 -61.00  90.00   39
 16  \w     37.00  64.00   1.00   40.00    --  104.22 -61.00 -90.00   27
 17  \w     36.00 104.00   1.00   40.00    --  104.22 -94.00   0.00   68
 18  \w     32.00  68.00   1.00   40.00    --  104.22 -61.00 120.00   36
 19  \w    116.00 163.00   1.00   40.00    --  104.22  30.00-150.00   47
 20  \w     32.00  62.00   1.00   40.00    --  104.22 -61.00-180.00   30
 21  \w     32.00  57.00   1.00   40.00    --  104.22 -61.00 -60.00   25
 22  \w     36.00  69.00   1.00   40.00    --  104.22 -61.00 150.00   33
 23  \w     35.00  67.00   1.00   40.00    --  104.22 -61.00   0.00   32
;
_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      0.0345393000
_diffrn_orient_matrix_UB_12      0.0252576000
_diffrn_orient_matrix_UB_13      -0.0190690000
_diffrn_orient_matrix_UB_21      -0.0154232000
_diffrn_orient_matrix_UB_22      0.0094659000
_diffrn_orient_matrix_UB_23      -0.0694250000
_diffrn_orient_matrix_UB_31      -0.0161638000
_diffrn_orient_matrix_UB_32      0.0450037000
_diffrn_orient_matrix_UB_33      0.0253543000
_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  0.0886
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64040
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.170
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.960
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64479
_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    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             8056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.743
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         11464
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1258P)^2^+146.1005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8013
_reflns_number_total             11464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05037a2.cif
_cod_data_source_block           beaver-107
_cod_depositor_comments
'Adding full bibliography for 1573437--1573441.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1573441
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Mo C N O'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.755
_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, All N(H) groups
2. Restrained distances
 C27-C26 \\sim C26-C25
 with sigma of 0.02
 C8-C26 \\sim C7-C27
 with sigma of 0.02
 C26-C25 \\sim C25-C7
 with sigma of 0.02
 C8-C7 \\sim C7-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(N1S) \\sim Ueq, Uanis(C3S)
\\sim Ueq, Uanis(N2S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(N3S) \\sim Ueq,
Uanis(C5S) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N6) \\sim
Ueq, Uanis(N2) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(N1) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C3S) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C2S, N1S, C1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4S, N2S, C3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5S, N3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H3SD(0.5) H3SE(0.5) H1(0.5) H1SA(0.5) H1SB(0.5) H1SD(0.5)
 H1SE(0.5) H2SB(0.5) H2SC(0.5) C25(0.5) H25(0.5) N6(0.5) H6A(0.5) H6B(0.5)
 C26(0.5) C27(0.5) H27(0.5)
6.a Rotating group:
 N2(H2A,H2B), N3(H3A,H3B), N6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 N3S(H3SD,H3SE), N1S(H1SA,H1SB), N2S(H2SD,H2SE)
6.c Me refined with riding coordinates:
 C1S(H1SC,H1SD,H1SE), C2S(H2SA,H2SB,H2SC)
6.d Aromatic/amide H refined with riding coordinates:
 C19(H19), C23(H23), C11(H11), C3(H3), C8(H8), C5(H5), C15(H15), C21(H21),
 C13(H13), C25(H25)
6.e Tetrahedral OH refined with everything fixed:
 N1(H1), C27(H27)
6.f Idealised Me refined as rotating group:
 C5S(H5SA,H5SB,H5SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC)
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              70157
_shelx_hkl_checksum              35483
_shelx_fab_checksum              65373
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.716