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_7713771
_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
'C66 H45.716 Mo6 N6 O30, 3(C2 H8 N), 4.202(C3 H7 N1 O1)'
_chemical_formula_sum            'C85.08 H101.63 Mo6 N13.36 O34.36'
_chemical_formula_weight         2436.82
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-21 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   39.015(4)
_cell_length_b                   39.015(4)
_cell_length_c                   13.9911(13)
_cell_measurement_reflns_used    1061
_cell_measurement_temperature    149.8(4)
_cell_measurement_theta_max      36.3630
_cell_measurement_theta_min      3.3790
_cell_volume                     18444(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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      3.00  54.00   1.00   80.00    --  -35.40 -13.00 -90.00   51
  2  \w    -54.00 -26.00   1.00   80.00    --  -35.40 -13.00 -90.00   28
  3  \w    -56.00  40.00   1.00   80.00    --  -35.40  76.00 150.00   96
  4  \w   -123.00   4.00   1.00   80.00    --  -35.40 -36.00-114.00  127
  5  \w    -66.00  19.00   1.00   80.00    --  -35.40  57.00 -30.00   85
  6  \w   -119.00 -11.00   1.00   80.00    --  -35.40 -65.00-111.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0284293000
_diffrn_orient_matrix_UB_12      -0.0204328000
_diffrn_orient_matrix_UB_13      -0.0840764000
_diffrn_orient_matrix_UB_21      0.0308166000
_diffrn_orient_matrix_UB_22      0.0305436000
_diffrn_orient_matrix_UB_23      -0.0694287000
_diffrn_orient_matrix_UB_31      0.0179553000
_diffrn_orient_matrix_UB_32      -0.0269765000
_diffrn_orient_matrix_UB_33      -0.0145708000
_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  0.1699
_diffrn_reflns_av_unetI/netI     0.1369
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12642
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        41.103
_diffrn_reflns_theta_max         41.103
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.468
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.316
_exptl_crystal_description       needle
_exptl_crystal_F_000             7395
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.1145
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2869
_refine_ls_wR_factor_ref         0.3268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1408
_reflns_number_total             2615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02482b2.cif
_cod_data_source_block           MUV27-bpy-c3
_cod_original_cell_volume        18444(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7713771
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.135
_olex2_refinement_description
;
1. Restrained distances
 C29-C28
 2.4 with sigma of 0.02
 C26-C22
 1.45 with sigma of 0.02
 C11-N3 \\sim C18-N2
 with sigma of 0.02
 C9-C10 \\sim C16-C17
 with sigma of 0.02
 C9-C11 \\sim C16-C18
 with sigma of 0.04
 C10-C11 \\sim C17-C18
 with sigma of 0.02
 C9-C12 \\sim C16-C14
 with sigma of 0.04
 C10-N3 \\sim C17-N2
 with sigma of 0.04
 N3-C12 \\sim N2-C14
 with sigma of 0.02
 C8-C9 \\sim C8-C16
 with sigma of 0.02
 C11-C12 \\sim C18-C14
 with sigma of 0.04
 C8-C13 \\sim C8-C15
 with sigma of 0.04
 N13S-C14S \\sim N13S-C15S
 with sigma of 0.02
 C8-C10 \\sim C8-C17
 with sigma of 0.04
 C13-C10 \\sim C15-C17
 with sigma of 0.04
 C13-C9 \\sim C15-C16
 with sigma of 0.02
 C13-N3 \\sim C15-N2
 with sigma of 0.04
 C13-C12 \\sim C15-C14
 with sigma of 0.02
 N8S-C9S \\sim N8S-C10S
 with sigma of 0.02
 N4-C29 \\sim N4-C28
 with sigma of 0.02
2. Restrained planarity
 C12S, O11S, N13S, C14S, C15S
 with sigma of 0.1
 C7S, O6S, N8S, C9S, C10S
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N4: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C13 \\sim C10 \\sim C11 \\sim N3 \\sim C12 \\sim C9: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
C17 \\sim C18 \\sim N3 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C14S \\sim C12S \\sim O11S \\sim N13S \\sim C15S: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
C12S \\sim O11S \\sim N13S \\sim C14S \\sim C15S: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C7S \\sim N8S \\sim C10S \\sim C9S \\sim O6S: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C7S \\sim O6S \\sim N8S \\sim C9S \\sim C10S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C29 \\sim N4 \\sim C28: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C6 \\sim C7 \\sim C3 \\sim C8: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
C5 \\sim N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12S, O11S, N13S, C14S, C15S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7S, O6S, N8S, C9S, C10S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C12S)=Sof(H12S)=Sof(O11S)=Sof(N13S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15S)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(H8A)=Sof(H8B)=FVAR(1)
 Sof(C7S)=Sof(H7S)=Sof(O6S)=Sof(N8S)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H9SC)=
 Sof(C10S)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(C15)=Sof(H15)=Sof(C14)=
 Sof(H14)=Sof(N2)=1-FVAR(3)
 Sof(N3)=Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(C13)=Sof(H13)=
 Sof(C12)=Sof(H12)=FVAR(3)
6.a Free rotating group:
 C12S(O11S,N13S,C14S,C15S), C7S(O6S,N8S,C9S,C10S)
6.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C8(H8A,H8B), C6(H6A,H6B), C7(H7A,H7B)
6.c Me refined with riding coordinates:
 C14S(H14A,H14B,H14C), C15S(H15A,H15B,H15C), C9S(H9SA,H9SB,H9SC), C10S(H10A,
 H10B,H10C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
6.d Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C23(H23), C1(H1), C2(H2), C4(H4), C5(H5), C11(H11),
 C10(H10), C13(H13), C12(H12), C12S(H12S), C7S(H7S), C18(H18), C17(H17),
 C15(H15), C14(H14)
6.e Fitted hexagon refined as free rotating group:
 C21(C20,C25,C24,C23,C22), C1(C2,C3,C4,C5,N1), N3(C11,C10,C9,C13,C12), C18(C17,
 C16,C15,C14,N2)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 816 electrons were 
found in a volume of 3621\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[C3H7NO] per Formula Unit 
which account for 720 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              399
_shelx_fab_checksum              23825
_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 2.175
_oxdiff_exptl_absorpt_empirical_full_min 0.399