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_7713776
_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
'C109.712 H91.329 Mo12 N21.904 O61.904, 6(C2 H8 N), 1.384(C5 H6 N2), 4.879(C3 H7 N O), 7.556(H2 O)'
_chemical_formula_sum            'C143.29 H196.96 Mo12 N35.56 O74.36'
_chemical_formula_weight         4758.54
_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             2022-12-09
_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                90
_cell_angle_beta                 110.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7115(3)
_cell_length_b                   20.0909(2)
_cell_length_c                   27.2180(4)
_cell_measurement_reflns_used    21884
_cell_measurement_temperature    119.9(2)
_cell_measurement_theta_max      22.2380
_cell_measurement_theta_min      3.0020
_cell_volume                     10106.5(3)
_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    -38.00  53.00   1.00   15.00    --  -15.90  57.00 -90.00   91
  2  \w    -15.00  42.00   1.00   15.00    --   16.91  77.00-180.00   57
  3  \w    -42.00  49.00   1.00   15.00    --   16.91 -77.00-180.00   91
  4  \w    -10.00  89.00   1.00   15.00    --   16.91  38.00-120.00   99
  5  \w     -5.00  86.00   1.00   15.00    --   16.91  57.00  60.00   91
  6  \w    -10.00  89.00   1.00   15.00    --   16.91  38.00-180.00   99
  7  \w     -5.00  86.00   1.00   15.00    --   16.91  57.00 -30.00   91
  8  \w    -52.00  39.00   1.00   15.00    --   16.91 -57.00  60.00   91
  9  \w      7.00  77.00   1.00   15.00    --   18.00-126.00  40.40   70
 10  \w    -56.00 -33.00   1.00   15.00    --  -15.90 129.00-140.74   23
 11  \w    -73.00  -4.00   1.00   15.00    --  -15.90 123.00  81.21   69
 12  \w    -78.00  -9.00   1.00   15.00    --  -15.90 131.00 139.95   69
 13  \w    -12.00  13.00   1.00   15.00    --  -15.90 -73.00-145.00   25
;
_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      -0.0362112000
_diffrn_orient_matrix_UB_12      0.0090064000
_diffrn_orient_matrix_UB_13      -0.0035896000
_diffrn_orient_matrix_UB_21      0.0015365000
_diffrn_orient_matrix_UB_22      -0.0192385000
_diffrn_orient_matrix_UB_23      0.0222043000
_diffrn_orient_matrix_UB_31      0.0126260000
_diffrn_orient_matrix_UB_32      0.0281913000
_diffrn_orient_matrix_UB_33      0.0163216000
_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  0.1207
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            167847
_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         2.820
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97580
_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    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             4809
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1158
_refine_ls_number_reflns         17832
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0998P)^2^+50.1812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11707
_reflns_number_total             17832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02482b2.cif
_cod_data_source_block           muv27-py-NH2-DMF
_cod_database_code               7713776
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C11 H10 N O Mo4'
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N19-C71 = N19-C73
 1.45 with sigma of 0.02
 C32A-N10A
 1.45 with sigma of 0.002
 N14-C60
 1.45 with sigma of 0.02
 C71-C73
 2.4 with sigma of 0.02
 C25A-C19A
 2.4 with sigma of 0.02
 C14-N6 \\sim C9-N4
 with sigma of 0.04
 C13-N6 \\sim C8-N4
 with sigma of 0.02
 C31A-N10A \\sim N10A-C33A
 with sigma of 0.02
 N6-C12 \\sim N4-C7
 with sigma of 0.04
 C15-C11 \\sim C10-C6
 with sigma of 0.04
 C61-N14 \\sim N14-C59
 with sigma of 0.02
 N3S-C4S \\sim N3S-C5S
 with sigma of 0.02
 N19-C73 \\sim N19A-C73A
 with sigma of 0.02
 C15-C14 \\sim C10-C9
 with sigma of 0.02
 C71-C73 \\sim C71A-C73A
 with sigma of 0.04
 N5-C15 \\sim N3-C10
 with sigma of 0.02
 N5-C12 \\sim N3-C7
 with sigma of 0.04
 N5-C11 \\sim N3-C6
 with sigma of 0.02
 N5-C14 \\sim N3-C9
 with sigma of 0.04
 C15-C13 \\sim C10-C8
 with sigma of 0.04
 C14-C12 \\sim C9-C7
 with sigma of 0.04
 Mo2-N5 \\sim Mo2-N3
 with sigma of 0.02
 Mo2-C11 \\sim Mo2-C6
 with sigma of 0.04
 C14-C13 \\sim C9-C8
 with sigma of 0.02
 C11-C13 \\sim C6-C8
 with sigma of 0.04
 C11-C12 \\sim C6-C7
 with sigma of 0.02
 C13-C12 \\sim C8-C7
 with sigma of 0.02
 Mo2-C15 \\sim Mo2-C10
 with sigma of 0.04
 N17-C72 \\sim N17-C1M
 with sigma of 0.02
 N23-C66 \\sim N23-C65
 with sigma of 0.02
 N16-C75 \\sim N16-C25A
 with sigma of 0.02
 N16-C68 \\sim N16-C19A
 with sigma of 0.02
 N22-C76 \\sim N22-C1H
 with sigma of 0.02
 C76-C1H \\sim C9S-C10S
 with sigma of 0.04
 C70-O43 \\sim C7S-O6S
 with sigma of 0.02
 C70-N22 \\sim C7S-N8S
 with sigma of 0.02
 C70-C76 \\sim C7S-C9S
 with sigma of 0.04
 C70-C1H \\sim C7S-C10S
 with sigma of 0.04
 N22-C76 \\sim N8S-C9S
 with sigma of 0.02
 N22-C1H \\sim N8S-C10S
 with sigma of 0.02
 O43-N22 \\sim O6S-N8S
 with sigma of 0.04
 N18-C64 \\sim N18-C1L
 with sigma of 0.02
 Mo5-O31 \\sim Mo5-O32
 with sigma of 0.02
 C71-N19 \\sim C71A-N19A
 with sigma of 0.02
 C33-C31 \\sim C33A-C31A
 with sigma of 0.04
 C33-C32 \\sim C33A-C32A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 N9-C34 \\sim N9-C34A
 with sigma of 0.02
 N9-C33 \\sim N9-C33A
 with sigma of 0.04
 N9-C31 \\sim N9-C31A
 with sigma of 0.04
 N9-C30 \\sim N9-C30A
 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 C34-C32 \\sim C34A-C32A
 with sigma of 0.04
 C30-C32 \\sim C30A-C32A
 with sigma of 0.04
3. Restrained planarity
 N10A, C32A, C33A, C34A, C31A, C30A
 with sigma of 0.1
 N9, C30A, C31A, C32A, C33A, C34A, N10A
 with sigma of 0.1
 C60, N13, C58, C62, C59, C61, N14
 with sigma of 0.1
 C2S, O1S, N3S, C4S, C5S
 with sigma of 0.1
 C67, O31, N17, C72, C1M
 with sigma of 0.1
 C69, O41, N23, C66, C65
 with sigma of 0.1
 C70, O43, N22, C76, C1H
 with sigma of 0.1
 C63, O32, N18, C64, C1L
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N9 \\sim C34 \\sim C30 \\sim C33 \\sim C31 \\sim C32 \\sim N10 \\sim C34A \\sim
C30A \\sim C31A \\sim C32A \\sim C33A \\sim N10A: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
N5 \\sim C15 \\sim C14 \\sim C11 \\sim C13 \\sim N6 \\sim C12 \\sim N3 \\sim C6
\\sim C7 \\sim N4 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N14 \\sim N13 \\sim C58 \\sim C62 \\sim C59 \\sim C61 \\sim C60: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C71 \\sim N19 \\sim C73: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
C2S \\sim O1S \\sim N3S \\sim C4S \\sim C5S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C73A \\sim N19A \\sim C71A \\sim C73 \\sim N19 \\sim C71: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 2A
N3S \\sim C2S \\sim O1S \\sim C4S \\sim C5S: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
C67 \\sim O31 \\sim N17 \\sim C72 \\sim C1M: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C63 \\sim O32 \\sim N18 \\sim C64 \\sim C1L \\sim C67 \\sim O31 \\sim N17 \\sim
C72 \\sim C1M: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C69 \\sim O41 \\sim N23 \\sim C66 \\sim C65: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C70 \\sim O43 \\sim N22 \\sim C76 \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N8S \\sim C9S \\sim C7S \\sim C10S \\sim O6S \\sim O43 \\sim C70 \\sim N22
\\sim C76 \\sim C1H: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
C63 \\sim O32 \\sim N18 \\sim C64 \\sim C1L: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C34A, C30A, C33A, C31A, C32A, N10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C15, C14, C11, C13, N6, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C10, C9, C6, C8, N4, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2S, O1S, N3S, C4S, C5S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71, N19, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C67, O31, N17, C72, C1M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C69, O41, N23, C66, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C75
 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
 C70, O43, N22, C76, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, O32, N18, C64, C1L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C71A, N19A, C73A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C30, C33, C31, C32, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N4)=Sof(H4A)=Sof(H4B)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(N3)=
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(N5)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C11)=Sof(H11)=Sof(C13)=
 Sof(N6)=Sof(H6A)=Sof(H6B)=Sof(C12)=Sof(H12)=FVAR(1)
 Sof(H16C)=Sof(H16D)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C19A)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(2)
 Sof(H16A)=Sof(H16B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C75)=Sof(H75A)=
 Sof(H75B)=Sof(H75C)=FVAR(2)
 Sof(C7S)=Sof(H7S)=Sof(O6S)=Sof(N8S)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H9SC)=
 Sof(C10S)=Sof(H10E)=Sof(H10F)=Sof(H10G)=Sof(O3W)=Sof(H3WA)=Sof(H3WB)=1-FVAR(3)
 Sof(C70)=Sof(H70)=Sof(O43)=Sof(N22)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=Sof(O5W)=Sof(H5WA)=Sof(H5WB)=Sof(O4W)=
 Sof(H4WA)=Sof(H4WB)=FVAR(3)
 Sof(C2S)=Sof(H2S)=Sof(O1S)=Sof(N3S)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=
 Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=0.5*(1-FVAR(5))
 Sof(C63)=Sof(H63)=Sof(O32)=Sof(N18)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=
 Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=FVAR(5)
 Sof(C67)=Sof(H67)=Sof(O31)=Sof(N17)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=1-FVAR(6)
 Sof(N13)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(C61)=Sof(H61)=
 Sof(C62)=Sof(H62)=Sof(N14)=Sof(H14A)=Sof(H14B)=FVAR(6)
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(7)
 Sof(C73A)=Sof(H73D)=Sof(H73E)=Sof(H73F)=Sof(N19A)=Sof(H19F)=Sof(H19G)=
 Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(O33)=Sof(H33B)=Sof(H33C)=1-FVAR(8)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(N19)=Sof(H19D)=Sof(H19E)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(O35)=Sof(H35A)=Sof(H35B)=FVAR(8)
 Sof(O34)=Sof(H34B)=Sof(H34C)=FVAR(9)
 Sof(C32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=Sof(C34A)=Sof(H34A)=
 Sof(C33A)=Sof(H33A)=Sof(N10A)=Sof(H10C)=Sof(H10D)=1-FVAR(10)
 Sof(C34)=Sof(H34)=Sof(C30)=Sof(H30)=Sof(C33)=Sof(H33)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(N10)=Sof(H10A)=Sof(H10B)=FVAR(10)
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
7.a Riding coordinates:
 N2(H2A,H2B), N12(H12A,H12B), N6(H6A,H6B), N4(H4A,H4B), N14(H14A,H14B),
 O34(H34B,H34C), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O5W(H5WA,H5WB), O3W(H3WA,H3WB),
  O4W(H4WA,H4WB), O33(H33B,H33C), O35(H35A,H35B), N10A(H10C,H10D)
7.b Free rotating group:
 C69(O41,N23,C66,C65), C70(O43,N22,C76,C1H), C7S(O6S,N8S,C9S,C10S), C2S(O1S,
 N3S,C4S,C5S), C63(O32,N18,C64,C1L), C67(O31,N17,C72,C1M)
7.c Rotating group:
 N8(H8A,H8B), N10(H10A,H10B)
7.d Secondary CH2 refined with riding coordinates:
 N15(H15A,H15B), N16(H16A,H16B), N16(H16C,H16D), N19(H19D,H19E), N19A(H19F,H19G)
7.e Me refined with riding coordinates:
 C02K(H02A,H02B,H02C), C02O(H02D,H02E,H02F), C68(H68A,H68B,H68C), C75(H75A,
 H75B,H75C), C66(H66A,H66B,H66C), C65(H65A,H65B,H65C), C25A(H25A,H25B,H25C),
 C19A(H19A,H19B,H19C), C76(H76A,H76B,H76C), C1H(H1HA,H1HB,H1HC), C9S(H9SA,H9SB,
 H9SC), C10S(H10E,H10F,H10G), C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC),
 C64(H64A,H64B,H64C), C1L(H1LA,H1LB,H1LC), C72(H72A,H72B,H72C), C1M(H1MA,H1MB,
 H1MC), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C73A(H73D,H73E,H73F),
 C71A(H71D,H71E,H71F)
7.f Aromatic/amide H refined with riding coordinates:
 C41(H41), C51(H51), C53(H53), C37(H37), C39(H39), C55(H55), C20(H20),
 C18(H18), C48(H48), C22(H22), C47(H47), C1(H1), C5(H5), C44(H44), C2(H2),
 C45(H45), C4(H4), C25(H25), C29(H29), C26(H26), C15(H15), C28(H28), C14(H14),
 C34(H34), C30(H30), C33(H33), C11(H11), C31(H31), C12(H12), C58(H58), C59(H59),
  C61(H61), C62(H62), C9(H9), C10(H10), C6(H6), C7(H7), C69(H69), C70(H70),
 C7S(H7S), C2S(H2S), C63(H63), C67(H67), C31A(H31A), C30A(H30A), C34A(H34A),
 C33A(H33A)
7.g Fitted hexagon refined as free rotating group:
 N13(C58,C59,C60,C61,C62), C8(C9,C10,N3,C6,C7), C32A(C31A,C30A,N9,C34A,C33A)
;
_shelx_res_checksum              84362
_olex2_date_sample_data_collection 2021-11-23
_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 1.154
_oxdiff_exptl_absorpt_empirical_full_min 0.900