Single-crystal-to-single-crystal intercalation of a low-bandgap superatomic crystal
Evan S. O'Brien; M. Tuan Trinh; Rose L. Kann; Jia Chen; Giselle A. Elbaz; Amrita Masurkar; Timothy L. Atallah; Maria V. Paley; Nilam Patel; Daniel W. Paley; Ioannis Kymissis; Andrew C. Crowther; Andrew J. Millis; David R. Reichman; X.-Y. Zhu; Xavier Roy; Nature Chemistry 9 (2017) 1170–1174; doi:10.1038/nchem.2844

data_1551545
_publ_section_title
;
 Single-crystal-to-single-crystal intercalation of a low-bandgap
 superatomic crystal
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1170
_journal_page_last               1174
_journal_paper_doi               10.1038/nchem.2844
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C54 H126 Co6 P6 Te8, 3(C60), 2(C6 N4)'
_chemical_formula_sum            'C246 H126 Co6 N8 P6 Te8'
_chemical_formula_weight         4753.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 104.260(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.5695(10)
_cell_length_b                   17.0560(5)
_cell_length_c                   21.1219(8)
_cell_measurement_reflns_used    13214
_cell_measurement_temperature    102(4)
_cell_measurement_theta_max      71.4990
_cell_measurement_theta_min      3.3490
_cell_volume                     9276.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     19.00 103.00   0.50    3.00    --   35.53  57.00 150.00  168
  2  \w     19.00 103.00   0.50    3.00    --   35.53  57.00   0.00  168
  3  \w      9.00 103.00   0.50    3.00    --   35.53  77.00-120.00  188
  4  \w      9.00 103.00   0.50    3.00    --   35.53  77.00  90.00  188
  5  \w      0.00  28.00   0.50    3.00    --   35.53  92.00 166.63   56
  6  \w      1.00  74.00   0.50    3.00    --   35.53 -99.00  60.00  146
  7  \w    -32.00  52.00   0.50    3.00    --   35.53 -57.00 120.00  168
  8  \w     55.00 108.00   0.50    3.00    --   35.53-178.00 150.00  106
  9  \w     16.00 105.00   0.50    3.00    --   35.53  37.00 -30.00  178
 10  \w      1.00  74.00   0.50    3.00    --   35.53 -99.00 -60.00  146
 11  \w    -34.00 105.00   0.50    3.00    --   35.53   0.00 120.00  278
 12  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00-180.00  140
 13  \w     38.00 116.00   0.50   15.00    --  108.00-111.00 -60.00  156
 14  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00  90.00  118
 15  \w     91.00 176.00   0.50   15.00    --  108.00  45.00 150.00  170
 16  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00 -60.00  140
 17  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00  30.00  140
 18  \w     81.00 176.00   0.50   15.00    --  108.00  77.00 -60.00  190
 19  \w     87.00 178.00   0.50   15.00    --  108.00  30.00 120.00  182
 20  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00-150.00  118
 21  \w     38.00 116.00   0.50   15.00    --  108.00-111.00-180.00  156
 22  \w    100.00 178.00   0.50   15.00    --  108.00 111.00  90.00  156
 23  \w     90.00 175.00   0.50   15.00    --  108.00  61.00-150.00  170
 24  \w     70.00 178.00   0.50   15.00    --  108.00  15.00  90.00  216
 25  \w     57.00 150.00   0.50   15.00    --  108.00 178.00 -30.00  186
 26  \w     38.00  91.00   0.50   15.00    --  108.00 -30.00 150.00  106
 27  \w     38.00 116.00   0.50   15.00    --  108.00-111.00  30.00  156
 28  \w     87.00 178.00   0.50   15.00    --  108.00  30.00   0.00  182
 29  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00 -90.00  140
 30  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00  60.00  140
 31  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00 150.00  118
 32  \w     38.00  94.00   0.50   15.00    --  108.00 -25.00 100.07  112
 33  \w     37.00 146.00   0.50   15.00    --  108.00 -15.00 120.00  218
 34  \w     38.00  91.00   0.50   15.00    --  108.00 -30.00-150.00  106
 35  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00 -90.00  118
 36  \w     38.00  91.00   0.50   15.00    --  108.00 -30.00 -60.00  106
 37  \w     37.00 146.00   0.50   15.00    --  108.00 -15.00 -30.00  218
 38  \w     38.00 116.00   0.50   15.00    --  108.00-111.00  90.00  156
 39  \w     41.00 126.00   0.50   15.00    --  108.00 -61.00  60.00  170
 40  \w     90.00 175.00   0.50   15.00    --  108.00  61.00 120.00  170
 41  \w     41.00 126.00   0.50   15.00    --  108.00 -61.00 150.00  170
 42  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00-120.00  118
 43  \w     41.00 126.00   0.50   15.00    --  108.00 -61.00-150.00  170
 44  \w     39.00 109.00   0.50   15.00    --  108.00 -94.00  90.00  140
 45  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00   0.00  118
 46  \w     40.00  99.00   0.50   15.00    --  108.00 -45.00 -60.00  118
 47  \w     90.00 175.00   0.50   15.00    --  108.00  61.00  90.00  170
 48  \w    113.00 140.00   0.50   15.00    --  108.00  45.00-180.00   54
 49  \w    112.00 139.00   0.50   15.00    --  108.00  45.00 -90.00   54
 50  \w     63.00  90.00   0.50   15.00    --  108.00 -61.00   0.00   54
 51  \w     43.00  70.00   0.50   15.00    --  108.00 -30.00  30.00   54
 52  \w     64.00 104.00   0.50   15.00    --  108.00 -85.00 -39.17   80
 53  \w    123.00 150.00   0.50   15.00    --  108.00 178.00   0.00   54
 54  \w    102.00 129.00   0.50   15.00    --  108.00  26.00 164.05   54
 55  \w     70.00  98.00   0.50   15.00    --  108.00 -77.00-150.00   56
 56  \w     41.00  67.00   0.50   15.00    --  108.00 -77.00  90.00   52
 57  \w     67.00  92.00   0.50   15.00    --  108.00 -20.00-161.17   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0480091000
_diffrn_orient_matrix_UB_12      -0.0248340000
_diffrn_orient_matrix_UB_13      -0.0238147000
_diffrn_orient_matrix_UB_21      -0.0248610000
_diffrn_orient_matrix_UB_22      0.0343011000
_diffrn_orient_matrix_UB_23      -0.0679676000
_diffrn_orient_matrix_UB_31      0.0256236000
_diffrn_orient_matrix_UB_32      0.0797463000
_diffrn_orient_matrix_UB_33      0.0218725000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         4.319
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.817
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4652
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.266
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         20903
_refine_ls_number_restraints     770
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.1048
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2802
_refine_ls_wR_factor_ref         0.2957
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17308
_reflns_number_total             20903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2844-s4.cif
_cod_data_source_block           TCNEdoped
_cod_database_code               1551545
_chemical_oxdiff_formula         'Co6 Te8 P6 C246 H126 N4'
_chemical_oxdiff_usercomment     'CoTe-3C60 4 eq TCNE'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.620(4) 0.121(2) 0.259(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C121-C126_$2 \\sim C122-C127_$2 \\sim C123-C128_$2 \\sim C124-C129_$2 \\sim
C125-C130_$2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
P1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim
C18 \\sim C19 \\sim P2 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim
C26 \\sim C27 \\sim C28 \\sim C29 \\sim P3 \\sim C31 \\sim C32 \\sim C33 \\sim
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 P1, C11, C12, C13, C14, C15, C16, C17, C18, C19, P2, C21, C22, C23, C24, C25,
 C26, C27, C28, C29, P3, C31, C32, C33, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{P2, C21, C22, C23, C24, C25, C26, C27, C28, C29} sigma for 1-2: 0.02, 1-3: 0.04
{P3, C31, C32, C33, C34, C35, C36, C37, C38, C39} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1, C11, C12, C13, C14, C15, C16, C17, C18, C19}
{C201, C202, C203, C204, C205, C206, C207, C208, C209, C210, C211, C212, C213,
C214, C215, C216, C217, C218, C219, C220, C221, C222, C223, C224, C225, C226,
C227, C228, C229, C230} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, C102, C103, C104, C105, C106, C107, C108, C109, C110, C111, C112, C113,
C114, C115, C116, C117, C118, C119, C120, C121, C122, C123, C124, C125, C126,
C127, C128, C129, C130}
7. Others
 1*[1(DFIX)]+1*[1(DFIX)]-1*[1(DFIX)]=0 with esd of 0.001
 Sof(C301)=Sof(C302)=Sof(C303)=Sof(C304)=Sof(C305)=Sof(C306)=Sof(C307)=
 Sof(C308)=Sof(C309)=Sof(C310)=Sof(C311)=Sof(C312)=Sof(C313)=Sof(C314)=
 Sof(C315)=Sof(C316)=Sof(C317)=Sof(C318)=Sof(C319)=Sof(C320)=Sof(C321)=
 Sof(C322)=Sof(C323)=Sof(C324)=Sof(C325)=Sof(C326)=Sof(C327)=Sof(C328)=
 Sof(C329)=Sof(C330)=Sof(C331)=Sof(C332)=Sof(C333)=Sof(C334)=Sof(C335)=
 Sof(C336)=Sof(C337)=Sof(C338)=Sof(C339)=Sof(C340)=Sof(C341)=Sof(C342)=
 Sof(C343)=Sof(C344)=Sof(C345)=Sof(C346)=Sof(C347)=Sof(C348)=Sof(C349)=
 Sof(C350)=Sof(C351)=Sof(C352)=Sof(C353)=Sof(C354)=Sof(C355)=Sof(C356)=
 Sof(C357)=Sof(C358)=Sof(C359)=Sof(C360)=0.5*(1-FVAR(5))
 Sof(C201)=Sof(C202)=Sof(C203)=Sof(C204)=Sof(C205)=Sof(C206)=Sof(C207)=
 Sof(C208)=Sof(C209)=Sof(C210)=Sof(C211)=Sof(C212)=Sof(C213)=Sof(C214)=
 Sof(C215)=Sof(C216)=Sof(C217)=Sof(C218)=Sof(C219)=Sof(C220)=Sof(C221)=
 Sof(C222)=Sof(C223)=Sof(C224)=Sof(C225)=Sof(C226)=Sof(C227)=Sof(C228)=
 Sof(C229)=Sof(C230)=Sof(C231)=Sof(C232)=Sof(C233)=Sof(C234)=Sof(C235)=
 Sof(C236)=Sof(C237)=Sof(C238)=Sof(C239)=Sof(C240)=Sof(C241)=Sof(C242)=
 Sof(C243)=Sof(C244)=Sof(C245)=Sof(C246)=Sof(C247)=Sof(C248)=Sof(C249)=
 Sof(C250)=Sof(C251)=Sof(C252)=Sof(C253)=Sof(C254)=Sof(C255)=Sof(C256)=
 Sof(C257)=Sof(C258)=Sof(C259)=Sof(C260)=0.5*FVAR(5)
 Uiso(C101)=Uiso(C102)=Uiso(C103)=Uiso(C104)=Uiso(C105)=Uiso(C106)=Uiso(C107)=
 Uiso(C108)=Uiso(C109)=Uiso(C110)=Uiso(C111)=Uiso(C112)=Uiso(C113)=Uiso(C114)=
 Uiso(C115)=Uiso(C116)=Uiso(C117)=Uiso(C118)=Uiso(C119)=Uiso(C120)=Uiso(C121)=
 Uiso(C122)=Uiso(C123)=Uiso(C124)=Uiso(C125)=Uiso(C126)=Uiso(C127)=Uiso(C128)=
 Uiso(C129)=Uiso(C130)=FVAR(5)
 Uiso(C201)=Uiso(C202)=Uiso(C203)=Uiso(C204)=Uiso(C205)=Uiso(C206)=Uiso(C207)=
 Uiso(C208)=Uiso(C209)=Uiso(C210)=Uiso(C211)=Uiso(C212)=Uiso(C213)=Uiso(C214)=
 Uiso(C215)=Uiso(C216)=Uiso(C217)=Uiso(C218)=Uiso(C219)=Uiso(C220)=Uiso(C221)=
 Uiso(C222)=Uiso(C223)=Uiso(C224)=Uiso(C225)=Uiso(C226)=Uiso(C227)=Uiso(C228)=
 Uiso(C229)=Uiso(C230)=Uiso(C231)=Uiso(C232)=Uiso(C233)=Uiso(C234)=Uiso(C235)=
 Uiso(C236)=Uiso(C237)=Uiso(C238)=Uiso(C239)=Uiso(C240)=Uiso(C241)=Uiso(C242)=
 Uiso(C243)=Uiso(C244)=Uiso(C245)=Uiso(C246)=Uiso(C247)=Uiso(C248)=Uiso(C249)=
 Uiso(C250)=Uiso(C251)=Uiso(C252)=Uiso(C253)=Uiso(C254)=Uiso(C255)=Uiso(C256)=
 Uiso(C257)=Uiso(C258)=Uiso(C259)=Uiso(C260)=Uiso(C301)=Uiso(C302)=Uiso(C303)=
 Uiso(C304)=Uiso(C305)=Uiso(C306)=Uiso(C307)=Uiso(C308)=Uiso(C309)=Uiso(C310)=
 Uiso(C311)=Uiso(C312)=Uiso(C313)=Uiso(C314)=Uiso(C315)=Uiso(C316)=Uiso(C317)=
 Uiso(C318)=Uiso(C319)=Uiso(C320)=Uiso(C321)=Uiso(C322)=Uiso(C323)=Uiso(C324)=
 Uiso(C325)=Uiso(C326)=Uiso(C327)=Uiso(C328)=Uiso(C329)=Uiso(C330)=Uiso(C331)=
 Uiso(C332)=Uiso(C333)=Uiso(C334)=Uiso(C335)=Uiso(C336)=Uiso(C337)=Uiso(C338)=
 Uiso(C339)=Uiso(C340)=Uiso(C341)=Uiso(C342)=Uiso(C343)=Uiso(C344)=Uiso(C345)=
 Uiso(C346)=Uiso(C347)=Uiso(C348)=Uiso(C349)=Uiso(C350)=Uiso(C351)=Uiso(C352)=
 Uiso(C353)=Uiso(C354)=Uiso(C355)=Uiso(C356)=Uiso(C357)=Uiso(C358)=Uiso(C359)=
 Uiso(C360)=FVAR(6)
 Fixed Sof: Te1(0.5) Te2(0.5) Te3(0.5) Te4(0.5) Co1(0.5) Co2(0.5) Co3(0.5)
 P1(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) P2(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5)
 H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) P3(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) H36C(0.5) C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C101(0.5) C102(0.5) C103(0.5)
 C104(0.5) C105(0.5) C106(0.5) C107(0.5) C108(0.5) C109(0.5) C110(0.5)
 C111(0.5) C112(0.5) C113(0.5) C114(0.5) C115(0.5) C116(0.5) C117(0.5)
 C118(0.5) C119(0.5) C120(0.5) C121(0.5) C122(0.5) C123(0.5) C124(0.5)
 C125(0.5) C126(0.5) C127(0.5) C128(0.5) C129(0.5) C130(0.5) C1(0.5) C2(0.5)
 N3(0.5) C4(0.5) N5(0.5) C6(0.5) C7(0.5) N8(0.5) C9(0.5) N10(0.5)
8.a Free rotating group:
 C201(C202,C203,C204,C205,C206,C207,C208,C209,C210,C211,C212,C213,C214,C215,
 C216,C217,C218,C219,C220,C221,C222,C223,C224,C225,C226,C227,C228,C229,C230,
 C231,C232,C233,C234,C235,C236,C237,C238,C239,C240,C241,C242,C243,C244,C245,
 C246,C247,C248,C249,C250,C251,C252,C253,C254,C255,C256,C257,C258,C259,C260),
 C301(C302,C303,C304,C305,C306,C307,C308,C309,C310,C311,C312,C313,C314,C315,
 C316,C317,C318,C319,C320,C321,C322,C323,C324,C325,C326,C327,C328,C329,C330,
 C331,C332,C333,C334,C335,C336,C337,C338,C339,C340,C341,C342,C343,C344,C345,
 C346,C347,C348,C349,C350,C351,C352,C353,C354,C355,C356,C357,C358,C359,C360)
8.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,
 H17B), C18(H18A,H18B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
 C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B),
  C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B)
8.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C39(H39A,H39B,H39C)
;
_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 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.595
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3
_twin_special_details
;
Component 2 rotated by 120.0615\% 
 around [-0.70 -0.00 0.71] (reciprocal) or [-0.47 -0.00 0.88] (direct)
Component 3 rotated by -119.9814\% 
 around [-0.71 -0.00 0.71] (reciprocal) or [-0.48 -0.00 0.88] (direct)
;