Imparting structural robustness of Metal-Organic Cages based on oxo-dimolybdenum clusters
Delaporte , Solène; Abánades Lázaro, Isabel; Lopez-Cabrelles, Javier; Mazarakioti, Eleni C.; Chebourou, Sarah; Vitórica-Yrezábal, Iñigo J.; Giménez-Marqués, Mónica; Minguez Espallargas, Guillermo; Dalton Transactions  (2023) –; doi:10.1039/D3DT02482B

data_7713774
_publ_section_title
;
 Imparting structural robustness of Metal-Organic Cages based on
 oxo-dimolybdenum clusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02482B
_journal_year                    2023
_chemical_formula_moiety
'C126 H90 Mo12 N12 O60, 6(C2 H8 N), 6.636(C3 H7 N O), 1.364(C3 H4 N O)'
_chemical_formula_sum            'C162 H189.79 Mo12 N26 O68'
_chemical_formula_weight         4740.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-21 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                78.085(4)
_cell_angle_beta                 69.613(4)
_cell_angle_gamma                81.101(4)
_cell_formula_units_Z            1
_cell_length_a                   14.5261(7)
_cell_length_b                   18.4437(10)
_cell_length_c                   20.6426(9)
_cell_measurement_reflns_used    5540
_cell_measurement_temperature    119.9(2)
_cell_measurement_theta_max      24.1290
_cell_measurement_theta_min      3.0320
_cell_volume                     5051.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -18.00  54.00   1.00   20.00    --  -14.73  57.00  90.00   72
  2  \w     -9.00  31.00   1.00   20.00    --   15.83  77.00  90.00   40
  3  \w    -12.00  41.00   1.00   20.00    --   15.83  77.00 -30.00   53
  4  \w      5.00  88.00   1.00   20.00    --   15.83  38.00  30.00   83
  5  \w    -42.00  -7.00   1.00   20.00    --   15.83 -77.00 120.00   35
  6  \w      1.00  44.00   1.00   20.00    --   15.83 -77.00 120.00   43
  7  \w      1.00  84.00   1.00   20.00    --   15.83  57.00-120.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0483957000
_diffrn_orient_matrix_UB_12      0.0148553000
_diffrn_orient_matrix_UB_13      0.0008894000
_diffrn_orient_matrix_UB_21      0.0187040000
_diffrn_orient_matrix_UB_22      0.0335923000
_diffrn_orient_matrix_UB_23      -0.0208136000
_diffrn_orient_matrix_UB_31      0.0066272000
_diffrn_orient_matrix_UB_32      -0.0144362000
_diffrn_orient_matrix_UB_33      -0.0307773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.1917
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36477
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.830
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         17806
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9635
_reflns_number_total             17806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02482b2.cif
_cod_data_source_block           muv27-bpy-c2
_cod_database_code               7713774
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C11 H10 N O Mo'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.961
_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
 N7-C67 = N7-C66
 1.45 with sigma of 0.02
 C67-C66
 2.4 with sigma of 0.02
 N8S-C10S \\sim N8T-C10T
 with sigma of 0.02
 C9S-C7S \\sim C9T-C7T
 with sigma of 0.04
 N8S-C9S \\sim N8T-C9T
 with sigma of 0.02
 O6S-C7S \\sim O6T-C7T
 with sigma of 0.02
 N8S-O6S \\sim N8T-O6T
 with sigma of 0.04
 N8S-C7S \\sim N8T-C7T
 with sigma of 0.02
 C10S-C9S \\sim C10T-C9T
 with sigma of 0.04
 C10S-C7S \\sim C10T-C7T
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O10 \\sim C20 \\sim O9: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
C66 \\sim N7 \\sim C67: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
O6T \\sim N8S \\sim C10S \\sim C9S \\sim C7S \\sim O6S \\sim C7T \\sim N8T
\\sim C10T \\sim C9T: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C13, C14, C19, C18, C17, C16, C15, O6, O5, O10, O9, O7, O8, C21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C10S, N8S, C9S, C7S, O6S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11S, C12S, N13S, C14S, C15S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C61, C60, C59, C58, C57, C56, C55, C62, C63
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N8T, C10T, C9T, O6T, C7T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8S, C10S, C9S, O6S, C7S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N8T)=Sof(C10T)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9T)=Sof(H9TA)=Sof(H9TB)=
 Sof(H9TC)=Sof(C7T)=Sof(H7T)=Sof(O6T)=1-FVAR(1)
 Sof(N8S)=Sof(C10S)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9S)=Sof(O6S)=Sof(C7S)=
 Sof(H7S)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 N9(H9A,H9B), N8(H8A,H8B), C27(H27A,H27B), C7(H7A,H7B), C39(H39A,H39B),
 C40(H40A,H40B), C6(H6A,H6B), C28(H28A,H28B), N7(H7C,H7D)
6.b Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C20S(H20A,H20B,H20C), C19S(H19A,
 H19B,H19C), C10S(H10D,H10E,H10F), C15S(H15A,H15B,H15C), C67(H67A,H67B,H67C),
 C14S(H14A,H14B,H14C), C66(H66A,H66B,H66C), C10T(H10A,H10B,H10C), C9T(H9TA,H9TB,
 H9TC)
6.c Aromatic/amide H refined with riding coordinates:
 C61(H61), C1(H1), C57(H57), C52(H52), C2(H2), C9(H9), C19(H19), C17(H17),
 C50(H50), C26(H26), C12(H12), C25(H25), C43(H43), C15(H15), C59(H59), C48(H48),
  C5(H5), C10(H10), C38(H38), C33(H33), C35(H35), C30(H30), C11(H11), C44(H44),
 C42(H42), C37(H37), C4(H4), C34(H34), C45(H45), C32(H32), C22(H22), C31(H31),
 C23(H23), C2S(H2S), C17S(H17S), C12S(H12S), C7S(H7S), C7T(H7T)
6.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C), C68(H68A,H68B,
 H68C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62637
_shelx_fab_checksum              41795
_olex2_date_sample_data_collection 2022-11-03
_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 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.916