Dinitrogen cleavage by a dinuclear uranium(iii) complex.
Jori, Nadir; Keener, Megan; Rajeshkumar, Thayalan; Scopelliti, Rosario; Maron, Laurent; Mazzanti, Marinella; Chemical science 14 (2023) 13485–13494; doi:10.1039/d3sc05253b

data_1570265
_publ_section_title
;
 Dinitrogen cleavage by a dinuclear uranium(iii) complex.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              13485
_journal_page_last               13494
_journal_paper_doi               10.1039/d3sc05253b
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C72 H162 K O25 Si6 U2'
_chemical_formula_sum            'C72 H162 K O25 Si6 U2'
_chemical_formula_weight         2111.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.240(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8351(7)
_cell_length_b                   31.0417(9)
_cell_length_c                   14.2077(6)
_cell_measurement_reflns_used    17289
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      28.9230
_cell_measurement_theta_min      3.1090
_cell_volume                     5375.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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     -5.00  21.00   1.00   35.00    --   11.42-102.00 -14.00   26
  2  \w     39.00  76.00   1.00   35.00    --   11.42 178.00 -90.00   37
  3  \w    -14.00  12.00   1.00   35.00    --   11.42 -99.00 -60.00   26
  4  \w     56.00  99.00   1.00   35.00    --   11.42 178.00  90.00   43
  5  \w    -44.00  14.00   1.00   35.00    --  -11.81  77.00 120.00   58
  6  \w    -41.00  21.00   1.00   35.00    --  -11.81 -77.00-150.00   62
  7  \w     -6.00  19.00   1.00   35.00    --  -11.81 -77.00 120.00   25
  8  \w    -40.00 -13.00   1.00   35.00    --  -11.81 -77.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0220905000
_diffrn_orient_matrix_UB_12      0.0175508000
_diffrn_orient_matrix_UB_13      0.0155980000
_diffrn_orient_matrix_UB_21      0.0028795000
_diffrn_orient_matrix_UB_22      0.0131232000
_diffrn_orient_matrix_UB_23      -0.0394748000
_diffrn_orient_matrix_UB_31      -0.0537435000
_diffrn_orient_matrix_UB_32      -0.0064933000
_diffrn_orient_matrix_UB_33      -0.0375373000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37630
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.831
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.172
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.186
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 4328 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         18660
_refine_ls_number_restraints     3252
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.724
_reflns_Friedel_fraction_max     0.702
_reflns_number_gt                13699
_reflns_number_total             18660
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.2971\% 
around [-0.08 1.00 0.03] (reciprocal) or [-0.37 0.93 -0.03] (direct)
;
_cod_data_source_file            d3sc05253b2.cif
_cod_data_source_block           mk-889
_cod_depositor_comments
'Adding full bibliography for 1570263--1570267.cif.'
_cod_database_code               1570265
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C72 H162 O25 Si6 K1 U2'
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.372
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O29-C88 = O31-C104
 1.43 with sigma of 0.02
 C102-C100 = C100-C98 = C97-C100 = C90-C88 = C89-C88 = C91-C88
 1.54 with sigma of 0.02
 C106-C104
 1.54 with sigma of 0.02
 C104-C105 = C104-C107
 1.54 with sigma of 0.02
 C89-O29
 2.5 with sigma of 0.02
 O31-C104 = O34-C108 = O29-C88 = O32-C92 = O33-C96
 1.43 with sigma of 0.02
 C96-O30
 1.43 with sigma of 0.02
 O33-C100
 1.43 with sigma of 0.02
 C67-C64 = C65-C64 = C66-C64
 1.54 with sigma of 0.02
 C84-O27
 1.43 with sigma of 0.02
 C85-C84
 1.54 with sigma of 0.02
 C84-C87
 1.54 with sigma of 0.02
 C84-C86
 1.54 with sigma of 0.02
 O23-C72 = O26-C76 = O25-C68 = O22-C64 = O27-C84 = O24-C80
 1.43 with sigma of 0.02
 C96-C101 = C99-C96 = C97-C96 = C100-C98 = C102-C100 = C103-C100
 1.54 with sigma of 0.02
 O33-C96 = O30-C100
 1.43 with sigma of 0.02
 O33-C99
 2.5 with sigma of 0.02
 O33-C97
 2.5 with sigma of 0.02
 C99-O33
 2.5 with sigma of 0.02
 C103-O30
 2.5 with sigma of 0.02
 C102-O30
 2.5 with sigma of 0.02
 O25-C68 = O22-C64
 1.43 with sigma of 0.02
 C51-C48 = C49-C48 = C50-C48
 1.54 with sigma of 0.02
 O16-C48 = O13-C32 = O14-C44 = O11-C36 = O15-C40 = O12-C28
 1.43 with sigma of 0.02
 O33-C100 = O30-C96
 1.43 with sigma of 0.02
 C99-C96 = C97-C96 = C96-C98 = C102-C100 = C100-C101 = C103-C100
 1.54 with sigma of 0.02
 C101-O33
 2.5 with sigma of 0.02
 C102-O33
 2.5 with sigma of 0.02
 C103-O33
 2.5 with sigma of 0.02
 C99-O30
 2.5 with sigma of 0.02
 C98-O30
 2.5 with sigma of 0.02
 C97-O30
 2.5 with sigma of 0.02
 C45-C44 = C47-C44 = C46-C44 = C38-C36 = C37-C36 = C39-C36
 1.54 with sigma of 0.02
 K1-C9
 3.7 with sigma of 0.02
 C98-C102 \\sim C102-C97 \\sim C98-C97
 with sigma of 0.02
 C90-C89 \\sim C89-C91 \\sim C90-C91
 with sigma of 0.02
 C106-C105 \\sim C105-C107 \\sim C106-C107
 with sigma of 0.02
 Si7-O29 \\sim Si7-O32
 with sigma of 0.02
 Si7-O31 \\sim Si7-O34
 with sigma of 0.02
 O29-C88 \\sim O32-C92
 with sigma of 0.02
 C88-C91 \\sim C92-C95
 with sigma of 0.02
 C88-C90 \\sim C92-C94
 with sigma of 0.02
 C88-C89 \\sim C92-C93
 with sigma of 0.02
 C107-C104 \\sim C111-C108
 with sigma of 0.02
 C98-C100 \\sim C101-C96
 with sigma of 0.02
 C100-C102 \\sim C96-C99
 with sigma of 0.02
 C100-C97 \\sim C96-C103
 with sigma of 0.02
 C105-C104 \\sim C109-C108
 with sigma of 0.02
 O31-C104 \\sim O34-C108
 with sigma of 0.02
 C104-C106 \\sim C108-C110
 with sigma of 0.02
 Si7-C88 \\sim Si7-C92
 with sigma of 0.02
 Si7-C100 \\sim Si7-C96
 with sigma of 0.02
 Si7-C104 \\sim Si7-C108
 with sigma of 0.02
 O29-C91 \\sim O32-C95
 with sigma of 0.02
 O29-C90 \\sim O32-C94
 with sigma of 0.02
 O29-C89 \\sim O32-C93
 with sigma of 0.02
 C107-C105 \\sim C111-C109
 with sigma of 0.02
 C107-O31 \\sim C111-O34
 with sigma of 0.02
 C107-C106 \\sim C111-C110
 with sigma of 0.02
 C98-C102 \\sim C101-C99
 with sigma of 0.02
 C98-C97 \\sim C101-C103
 with sigma of 0.02
 C91-C90 \\sim C95-C94
 with sigma of 0.02
 C91-C89 \\sim C95-C93
 with sigma of 0.02
 C90-C89 \\sim C94-C93
 with sigma of 0.02
 C105-O31 \\sim C109-O34
 with sigma of 0.02
 C105-C106 \\sim C109-C110
 with sigma of 0.02
 O31-C106 \\sim O34-C110
 with sigma of 0.02
 C102-C97 \\sim C99-C103
 with sigma of 0.02
 Si7-O31 \\sim Si7-O34 \\sim Si7-O29 \\sim Si7-O32 \\sim Si7-O33
 with sigma of 0.02
 Si7-O30 \\sim Si7-O33 \\sim Si7-O31 \\sim Si7-O34 \\sim Si7-O29 \\sim Si7-O32
 with sigma of 0.02
 O30-O29 \\sim O29-O31
 with sigma of 0.02
 O33-O32 \\sim O32-O34
 with sigma of 0.02
 C67-C65 \\sim C65-C66 \\sim C66-C67
 with sigma of 0.02
 Si6-O22 \\sim Si6-O25
 with sigma of 0.02
 Si6-O23 \\sim Si6-O26
 with sigma of 0.02
 Si6-O24 \\sim Si6-O27
 with sigma of 0.02
 O22-C64 \\sim O25-C68
 with sigma of 0.02
 O23-C72 \\sim O26-C76
 with sigma of 0.02
 C72-C75 \\sim C76-C78
 with sigma of 0.02
 C72-C73 \\sim C76-C77
 with sigma of 0.02
 C72-C74 \\sim C76-C79
 with sigma of 0.02
 C64-C66 \\sim C68-C71
 with sigma of 0.02
 C64-C65 \\sim C68-C69
 with sigma of 0.02
 C64-C67 \\sim C68-C70
 with sigma of 0.02
 Si6-C72 \\sim Si6-C76
 with sigma of 0.02
 Si6-C64 \\sim Si6-C68
 with sigma of 0.02
 O22-C66 \\sim O25-C71
 with sigma of 0.02
 O22-C65 \\sim O25-C69
 with sigma of 0.02
 O22-C67 \\sim O25-C70
 with sigma of 0.02
 O23-C75 \\sim O26-C78
 with sigma of 0.02
 O23-C73 \\sim O26-C77
 with sigma of 0.02
 O23-C74 \\sim O26-C79
 with sigma of 0.02
 C75-C73 \\sim C78-C77
 with sigma of 0.02
 C75-C74 \\sim C78-C79
 with sigma of 0.02
 C73-C74 \\sim C77-C79
 with sigma of 0.02
 C66-C65 \\sim C71-C69
 with sigma of 0.02
 C66-C67 \\sim C71-C70
 with sigma of 0.02
 C65-C67 \\sim C69-C70
 with sigma of 0.02
 C87-C86 \\sim C86-C85 \\sim C87-C85
 with sigma of 0.02
 O26-O25 \\sim O25-O27
 with sigma of 0.02
 O23-O22 \\sim O22-O24
 with sigma of 0.02
 Si6-O22 \\sim Si6-O25 \\sim Si6-O27 \\sim Si6-O24 \\sim Si6-O26 \\sim Si6-O23
 with sigma of 0.02
 C99-C101 \\sim C101-C97 \\sim C97-C99
 with sigma of 0.02
 C103-C98 \\sim C98-C102 \\sim C103-C102
 with sigma of 0.02
 Si3-O11 \\sim Si4-O14
 with sigma of 0.02
 Si3-O13 \\sim Si4-O16
 with sigma of 0.02
 Si3-O12 \\sim Si4-O15
 with sigma of 0.02
 O11-C36 \\sim O14-C44
 with sigma of 0.02
 O13-C32 \\sim O16-C48
 with sigma of 0.02
 O12-C28 \\sim O15-C40
 with sigma of 0.02
 C30-C28 \\sim C41-C40
 with sigma of 0.02
 C28-C31 \\sim C40-C43
 with sigma of 0.02
 C28-C29 \\sim C40-C42
 with sigma of 0.02
 C36-C39 \\sim C44-C47
 with sigma of 0.02
 C36-C37 \\sim C44-C46
 with sigma of 0.02
 C36-C38 \\sim C44-C45
 with sigma of 0.02
 C32-C34 \\sim C48-C51
 with sigma of 0.02
 C32-C35 \\sim C48-C49
 with sigma of 0.02
 C32-C33 \\sim C48-C50
 with sigma of 0.02
 Si3-C28 \\sim Si4-C40
 with sigma of 0.02
 Si3-C36 \\sim Si4-C44
 with sigma of 0.02
 Si3-C32 \\sim Si4-C48
 with sigma of 0.02
 O10-O11 \\sim O10-O14
 with sigma of 0.02
 O10-O13 \\sim O10-O16
 with sigma of 0.02
 O10-O12 \\sim O10-O15
 with sigma of 0.02
 O11-O13 \\sim O14-O16
 with sigma of 0.02
 O11-O12 \\sim O14-O15
 with sigma of 0.02
 O11-C39 \\sim O14-C47
 with sigma of 0.02
 O11-C37 \\sim O14-C46
 with sigma of 0.02
 O11-C38 \\sim O14-C45
 with sigma of 0.02
 O13-O12 \\sim O16-O15
 with sigma of 0.02
 O13-C34 \\sim O16-C51
 with sigma of 0.02
 O13-C35 \\sim O16-C49
 with sigma of 0.02
 O13-C33 \\sim O16-C50
 with sigma of 0.02
 O12-C30 \\sim O15-C41
 with sigma of 0.02
 O12-C31 \\sim O15-C43
 with sigma of 0.02
 O12-C29 \\sim O15-C42
 with sigma of 0.02
 C30-C31 \\sim C41-C43
 with sigma of 0.02
 C30-C29 \\sim C41-C42
 with sigma of 0.02
 C31-C29 \\sim C43-C42
 with sigma of 0.02
 C39-C37 \\sim C47-C46
 with sigma of 0.02
 C39-C38 \\sim C47-C45
 with sigma of 0.02
 C37-C38 \\sim C46-C45
 with sigma of 0.02
 C34-C35 \\sim C51-C49
 with sigma of 0.02
 C34-C33 \\sim C51-C50
 with sigma of 0.02
 C35-C33 \\sim C49-C50
 with sigma of 0.02
 C49-C51 \\sim C51-C50
 with sigma of 0.02
 Si3-O10 \\sim Si4-O10
 with sigma of 0.02
 Si4-O14 \\sim Si4-O15 \\sim Si4-O16 \\sim Si3-O13 \\sim Si3-O12 \\sim Si3-O11
 with sigma of 0.02
 C99-C98 \\sim C98-C97 \\sim C99-C97
 with sigma of 0.02
 C102-C101 \\sim C101-C103 \\sim C102-C103
 with sigma of 0.02
 C62-C60 \\sim C63-C60 \\sim C61-C60 \\sim C59-C56 \\sim C58-C56 \\sim C57-C56
\\sim C54-C52 \\sim C55-C52
 \\sim C53-C52
 with sigma of 0.02
 C62-C63 \\sim C63-C61 \\sim C61-C62
 with sigma of 0.02
 C59-C58 \\sim C58-C57 \\sim C57-C59
 with sigma of 0.02
 C54-C55 \\sim C55-C53 \\sim C53-C54
 with sigma of 0.02
 C19-C13 \\sim C15-C13 \\sim C18-C13 \\sim C16-C13 \\sim C17-C13 \\sim C14-C13
 with sigma of 0.02
 C19-C17 \\sim C17-C18 \\sim C18-C19
 with sigma of 0.02
 C15-C14 \\sim C14-C16 \\sim C15-C16
 with sigma of 0.02
 C45-C46 \\sim C46-C47 \\sim C45-C47
 with sigma of 0.02
 C38-C37 \\sim C37-C39 \\sim C38-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si7 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim C88 \\sim
C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim
C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si6 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim
C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim
C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si3 \\sim Si4 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C63) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C61)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O22, O23, O24, C64, C65, C66, C67, C72, C73, C74, C75, C80, C81, C82, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, O26, O27, C68, C69, C70, C71, C76, C77, C78, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O32)=Sof(O33)=Sof(O34)=Sof(C92)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=
 Sof(C100)=Sof(C101)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C102)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C108)=
 Sof(C109)=Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C110)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C111)=Sof(H11G)=Sof(H11H)=Sof(H11I)=1-FVAR(1)
 Sof(O29)=Sof(O30)=Sof(O31)=Sof(C88)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=
 Sof(C96)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 Sof(H98C)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C104)=Sof(C105)=Sof(H10M)=
 Sof(H10N)=Sof(H10O)=Sof(C106)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C107)=
 Sof(H10S)=Sof(H10T)=Sof(H10U)=FVAR(1)
 Sof(O25)=Sof(O26)=Sof(O27)=Sof(C68)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C76)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)=
 Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C84)=Sof(C85)=Sof(H85A)=
 Sof(H85B)=Sof(H85C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C87)=Sof(H87A)=
 Sof(H87B)=Sof(H87C)=1-FVAR(2)
 Sof(O22)=Sof(O23)=Sof(O24)=Sof(C64)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C72)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C74)=Sof(H74A)=Sof(H74B)=
 Sof(H74C)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C80)=Sof(C81)=Sof(H81A)=
 Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=
 Sof(H83B)=Sof(H83C)=FVAR(2)
 Sof(Si4)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(C40)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C44)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=1-FVAR(3)
 Sof(Si3)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(C28)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(4)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(4)
 Fixed X: U1(0.118131) U2(0.18205)
 Fixed Y: U1(0.55823) U2(0.44234)
 Fixed Z: U1(0.369821) U2(0.41286)
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C),
 C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C93(H93A,
 H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C),
 C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C101(H10D,H10E,H10F), C102(H10G,H10H,
 H10I), C103(H10J,H10K,H10L), C105(H10M,H10N,H10O), C106(H10P,H10Q,H10R),
 C107(H10S,H10T,H10U), C109(H10V,H10W,H10X), C110(H11D,H11E,H11F), C111(H11G,
 H11H,H11I)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 94 electrons were 
found in a volume of 570\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
1.1[C4H8O] per Asymmetric Unit 
which account for 88 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4454
_shelx_fab_checksum              73184
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.734
_oxdiff_exptl_absorpt_empirical_full_min 0.145
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2