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_1551543
_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), 6(C7 H8)'
_chemical_formula_sum            'C276 H174 Co6 P6 Te8'
_chemical_formula_weight         5050.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 103.9803(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.47019(18)
_cell_length_b                   17.35340(7)
_cell_length_c                   38.00346(16)
_cell_measurement_reflns_used    63437
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.7820
_cell_measurement_theta_min      2.5910
_cell_volume                     18859.58(17)
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1098
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_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    -49.00  89.00   0.50    2.50    --    0.98  57.00 -60.00  276
  2  \w    -20.00  31.00   0.50   12.50    --  -30.81 -99.00-150.00  102
  3  \w    -67.00  84.00   0.50   12.50    --   32.76 -77.00 -30.00  302
  4  \w     73.00 121.00   0.50   12.50    --   32.76 125.00   0.00   96
  5  \w     73.00 121.00   0.50   12.50    --   32.76 125.00-120.00   96
  6  \w     73.00 121.00   0.50   12.50    --   32.76 125.00  60.00   96
  7  \w    -18.00 120.00   0.50   12.50    --   32.76  57.00  60.00  276
  8  \w     35.00 105.00   0.50    2.50    --    0.98 178.00 -30.00  140
  9  \w   -134.00 -67.00   0.50   12.50    --  -30.81-166.00 132.00  134
 10  \w    -20.00  31.00   0.50   12.50    --  -30.81 -99.00  90.00  102
 11  \w     73.00 121.00   0.50   12.50    --   32.76 125.00 -60.00   96
 12  \w    -50.00 121.00   0.50   12.50    --   32.76  37.00 -60.00  342
 13  \w     35.00 105.00   0.50    2.50    --    0.98 178.00 150.00  140
 14  \w    -18.00 120.00   0.50   12.50    --   32.76  57.00   0.00  276
 15  \w    -18.00 120.00   0.50   12.50    --   32.76  57.00-180.00  276
 16  \w    -20.00  85.00   0.50   12.50    --   32.76 -99.00  90.00  210
 17  \w     73.00 121.00   0.50   12.50    --   32.76 125.00-180.00   96
 18  \w    -50.00 101.00   0.50    2.50    --    0.98  77.00  60.00  302
 19  \w    -20.00  31.00   0.50   12.50    --  -30.81 -99.00-180.00  102
 20  \w    -20.00  31.00   0.50   12.50    --  -30.81 -99.00   0.00  102
 21  \w    -56.00  71.00   0.50   12.50    --   32.76 -37.00  60.00  254
 22  \w     73.00 121.00   0.50   12.50    --   32.76 125.00 120.00   96
 23  \w   -103.00 -57.00   0.50    2.50    --    0.98-178.00-150.00   92
 24  \w    -18.00 120.00   0.50   12.50    --   32.76  57.00 150.00  276
 25  \w    -56.00  61.00   0.50   12.50    --   32.76 -37.00 150.00  234
 26  \w     73.00 121.00   0.50   12.50    --   32.76 125.00 -30.00   96
;
_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      -0.0020681000
_diffrn_orient_matrix_UB_12      -0.0320640000
_diffrn_orient_matrix_UB_13      0.0110782000
_diffrn_orient_matrix_UB_21      0.0038511000
_diffrn_orient_matrix_UB_22      0.0244724000
_diffrn_orient_matrix_UB_23      0.0153856000
_diffrn_orient_matrix_UB_31      -0.0244082000
_diffrn_orient_matrix_UB_32      0.0065729000
_diffrn_orient_matrix_UB_33      -0.0032353000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            229841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.881
_diffrn_reflns_theta_min         2.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             9992
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2622
_refine_ls_number_reflns         21558
_refine_ls_number_restraints     6437
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+203.7041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17060
_reflns_number_total             21558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2844-s2.cif
_cod_data_source_block           toluenesolvate
_cod_original_cell_volume        18859.57(17)
_cod_database_code               1551543
_chemical_oxdiff_formula         'c250 h120 co6 p6 te8'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{P51, P51C}
{C58, C58C}
3. Restrained distances
 H12D_$1-H3_122
 -1.8 with sigma of 0.02
4. Restrained planarity
 C1_101, C2_101, C3_101, C4_101, C5_101, C6_101, C7_101
 C1_102, C2_102, C3_102, C4_102, C5_102, C6_102, C7_102
 C1_111, C2_111, C3_111, C4_111, C5_111, C6_111, C7_111
 C1_112, C2_112, C3_112, C4_112, C5_112, C6_112, C7_112
 C1_121, C2_121, C3_121, C4_121, C5_121, C6_121, C7_121
 C1_122, C2_122, C3_122, C4_122, C5_122, C6_122, C7_122
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
: 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
Uanis(P31) = Uanis(P31B)
Uanis(P51) = Uanis(P51C)
Uanis(C58) = Uanis(C58C)
Uanis(C21_11) = Uanis(C30_12)
Uanis(C14_11) = Uanis(C26_12)
Uanis(C28_11) = Uanis(C22_12)
6. Rigid body (RIGU) restrains
 P11, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P31, C32, C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B, C40B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P51, C52, C53, C54, C55, C56, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P31B, C32B, C33B, C34B, C35B, C36B, C37B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P51, C52, C53, C54, C55, C56, C57, C58C, C59C, C60C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1, C10_1, C11_1, C12_1,
 C13_1, C14_1, C15_1, C16_1, C17_1, C18_1, C19_1, C20_1, C21_1, C22_1, C23_1,
 C24_1, C25_1, C26_1, C27_1, C28_1, C29_1, C30_1, C31_1, C32_1, C33_1, C34_1,
 C35_1, C36_1, C37_1, C38_1, C39_1, C40_1, C41_1, C42_1, C43_1, C44_1, C45_1,
 C46_1, C47_1, C48_1, C49_1, C50_1, C51_1, C52_1, C53_1, C54_1, C55_1, C56_1,
 C57_1, C58_1, C59_1, C60_1
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2, C10_2, C11_2, C12_2,
 C13_2, C14_2, C15_2, C16_2, C17_2, C18_2, C19_2, C20_2, C21_2, C22_2, C23_2,
 C24_2, C25_2, C26_2, C27_2, C28_2, C29_2, C30_2, C31_2, C32_2, C33_2, C34_2,
 C35_2, C36_2, C37_2, C38_2, C39_2, C40_2, C41_2, C42_2, C43_2, C44_2, C45_2,
 C46_2, C47_2, C48_2, C49_2, C50_2, C51_2, C52_2, C53_2, C54_2, C55_2, C56_2,
 C57_2, C58_2, C59_2, C60_2
 C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3, C10_3, C11_3, C12_3,
 C13_3, C14_3, C15_3, C16_3, C17_3, C18_3, C19_3, C20_3, C21_3, C22_3, C23_3,
 C24_3, C25_3, C26_3, C27_3, C28_3, C29_3, C30_3, C31_3, C32_3, C33_3, C34_3,
 C35_3, C36_3, C37_3, C38_3, C39_3, C40_3, C41_3, C42_3, C43_3, C44_3, C45_3,
 C46_3, C47_3, C48_3, C49_3, C50_3, C51_3, C52_3, C53_3, C54_3, C55_3, C56_3,
 C57_3, C58_3, C59_3, C60_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_11, C2_11, C3_11, C4_11, C5_11, C6_11, C7_11, C8_11, C9_11, C10_11, C11_11,
  C12_11, C13_11, C14_11, C15_11, C16_11, C17_11, C18_11, C19_11, C20_11,
 C21_11, C22_11, C23_11, C24_11, C25_11, C26_11, C27_11, C28_11, C29_11, C30_11
 C1_12, C2_12, C3_12, C4_12, C5_12, C6_12, C7_12, C8_12, C9_12, C10_12, C11_12,
  C12_12, C13_12, C14_12, C15_12, C16_12, C17_12, C18_12, C19_12, C20_12,
 C21_12, C22_12, C23_12, C24_12, C25_12, C26_12, C27_12, C28_12, C29_12, C30_12
 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{Co10, P11, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B} sigma for
1-2: 0.02, 1-3: 0.04
{Co30, P31, C32, C33, C34, C35, C36, C37, C38, C39, C40} sigma for 1-2: 0.02,
1-3: 0.04
{Co30, P31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B, C39B, C40B} sigma for
1-2: 0.02, 1-3: 0.04
{Co50, P51, C52, C53, C54, C55, C56, C57, C58, C59, C60} sigma for 1-2: 0.02,
1-3: 0.04
{Co50, P51, C52, C53, C54, C55, C56, C57, C58C, C59C, C60C} sigma for 1-2:
0.02, 1-3: 0.04
as
{Co10, P11, C12, C13, C14, C15, C16, C17, C18, C19, C20}
{Co50, P51B, C52B, C53B, C54B, C55B, C56B, C57B, C58B, C59B, C60B} sigma for
1-2: 0.02, 1-3: 0.04
{Co50, P51, C52, C53, C54, C55, C56, C57, C58, C59C, C60C} sigma for 1-2: 0.02,
1-3: 0.04
as
{Co50, P51, C52, C53, C54, C55, C56, C57, C58, C59, C60}
{C1_12, C2_12, C3_12, C4_12, C5_12, C6_12, C7_12, C8_12, C9_12, C10_12, C11_12,
C12_12, C13_12, C14_12, C15_12, C16_12, C17_12, C18_12, C19_12, C20_12, C21_12,
C22_12, C23_12, C24_12, C25_12, C26_12, C27_12, C28_12, C29_12, C30_12}
as
{C1_11, C2_11, C3_11, C4_11, C5_11, C6_11, C7_11, C8_11, C9_11, C10_11, C11_11,
C12_11, C13_11, C14_11, C15_11, C16_11, C17_11, C18_11, C19_11, C20_11, C21_11,
C22_11, C23_11, C24_11, C25_11, C26_11, C27_11, C28_11, C29_11, C30_11} sigma
for 1-2: 0.02 1-3: 0.04
{C1_102, C2_102, C3_102, C4_102, C5_102, C6_102, C7_102}
{C1_111, C2_111, C3_111, C4_111, C5_111, C6_111, C7_111}
{C1_112, C2_112, C3_112, C4_112, C5_112, C6_112, C7_112}
{C1_121, C2_121, C3_121, C4_121, C5_121, C6_121, C7_121}
{C1_122, C2_122, C3_122, C4_122, C5_122, C6_122, C7_122}
as
{C1_101, C2_101, C3_101, C4_101, C5_101, C6_101, C7_101} sigma for 1-2: 0.02
1-3: 0.04
{C1_102, C2_102, C7_102, C6_102, C5_102, C4_102, C3_102}
{C1_111, C2_111, C7_111, C6_111, C5_111, C4_111, C3_111}
{C1_112, C2_112, C7_112, C6_112, C5_112, C4_112, C3_112}
{C1_121, C2_121, C7_121, C6_121, C5_121, C4_121, C3_121}
{C1_122, C2_122, C7_122, C6_122, C5_122, C4_122, C3_122}
as
{C1_101, C2_101, C7_101, C6_101, C5_101, C4_101, C3_101} sigma for 1-2: 0.02
1-3: 0.04
8. Others
 -1*[Sof(P51)+Sof(C52)+Sof(H52A)+Sof(H52B)+Sof(C53)+Sof(H53A)+Sof(H53B)+
 Sof(C54)+Sof(H54A)+Sof(H54B)+Sof(H54C)+Sof(C55)+Sof(H55A)+Sof(H55B)+Sof(C56)+
 Sof(H56A)+Sof(H56B)+Sof(C57)+Sof(H57A)+Sof(H57B)+Sof(H57C)+Sof(C58)+Sof(P51B)+
 Sof(C52B)+Sof(H52C)+Sof(H52D)+Sof(C53B)+Sof(H53C)+Sof(H53D)+Sof(C54B)+
 Sof(H54D)+Sof(H54E)+Sof(H54F)+Sof(C55B)+Sof(H55C)+Sof(H55D)+Sof(C56B)+
 Sof(H56C)+Sof(H56D)+Sof(C57B)+Sof(H57D)+Sof(H57E)+Sof(H57F)+Sof(C58B)+
 Sof(H58E)+Sof(H58F)+Sof(C59B)+Sof(H59E)+Sof(H59F)+Sof(C60B)+Sof(H60G)+
 Sof(H60H)+Sof(H60I)]+1*[Sof(H58A)+Sof(H58B)+Sof(C59)+Sof(H59A)+Sof(H59B)+
 Sof(C60)+Sof(H60A)+Sof(H60B)+Sof(H60C)]+1*[Sof(H58C)+Sof(H58D)+Sof(C59C)+
 Sof(H59C)+Sof(H59D)+Sof(C60C)+Sof(H60D)+Sof(H60E)+Sof(H60F)]=0 with esd of
 0.001
 1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+Sof(C8)+Sof(C9)+
 Sof(C10)+Sof(C11)+Sof(C12)+Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+Sof(C17)+
 Sof(C18)+Sof(C19)+Sof(C20)+Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+Sof(C25)+
 Sof(C26)+Sof(C27)+Sof(C28)+Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+Sof(C33)+
 Sof(C34)+Sof(C35)+Sof(C36)+Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+Sof(C41)+
 Sof(C42)+Sof(C43)+Sof(C44)+Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+Sof(C49)+
 Sof(C50)+Sof(C51)+Sof(C52)+Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+Sof(C57)+
 Sof(C58)+Sof(C59)+Sof(C60)]+1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+
 Sof(C7)+Sof(C8)+Sof(C9)+Sof(C10)+Sof(C11)+Sof(C12)+Sof(C13)+Sof(C14)+Sof(C15)+
 Sof(C16)+Sof(C17)+Sof(C18)+Sof(C19)+Sof(C20)+Sof(C21)+Sof(C22)+Sof(C23)+
 Sof(C24)+Sof(C25)+Sof(C26)+Sof(C27)+Sof(C28)+Sof(C29)+Sof(C30)+Sof(C31)+
 Sof(C32)+Sof(C33)+Sof(C34)+Sof(C35)+Sof(C36)+Sof(C37)+Sof(C38)+Sof(C39)+
 Sof(C40)+Sof(C41)+Sof(C42)+Sof(C43)+Sof(C44)+Sof(C45)+Sof(C46)+Sof(C47)+
 Sof(C48)+Sof(C49)+Sof(C50)+Sof(C51)+Sof(C52)+Sof(C53)+Sof(C54)+Sof(C55)+
 Sof(C56)+Sof(C57)+Sof(C58)+Sof(C59)+Sof(C60)]+1*[Sof(C1)+Sof(C2)+Sof(C3)+
 Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+Sof(C8)+Sof(C9)+Sof(C10)+Sof(C11)+Sof(C12)+
 Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+Sof(C17)+Sof(C18)+Sof(C19)+Sof(C20)+
 Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+Sof(C25)+Sof(C26)+Sof(C27)+Sof(C28)+
 Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+Sof(C33)+Sof(C34)+Sof(C35)+Sof(C36)+
 Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+Sof(C41)+Sof(C42)+Sof(C43)+Sof(C44)+
 Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+Sof(C49)+Sof(C50)+Sof(C51)+Sof(C52)+
 Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+Sof(C57)+Sof(C58)+Sof(C59)+Sof(C60)]=1
 with esd of 0.0005
 Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18C)=Sof(H18D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(Q1)=
 Sof(Q2)=Sof(Q3)=Sof(Q4)=Sof(Q5)=Sof(Q6)=Sof(Q7)=Sof(Q8)=Sof(Q9)=Sof(Q10)=
 Sof(Q11)=Sof(Q12)=Sof(Q13)=Sof(Q14)=Sof(Q15)=Sof(Q16)=Sof(Q17)=Sof(Q18)=
 Sof(Q19)=Sof(Q20)=Sof(Q21)=Sof(Q22)=Sof(Q23)=Sof(Q24)=Sof(Q25)=Sof(Q26)=
 Sof(Q27)=Sof(Q28)=Sof(Q29)=Sof(Q30)=Sof(Q31)=Sof(Q32)=Sof(Q33)=Sof(Q34)=
 Sof(Q35)=Sof(Q36)=Sof(Q37)=Sof(Q38)=Sof(Q39)=Sof(Q40)=Sof(Q41)=Sof(Q42)=
 Sof(Q43)=Sof(Q44)=Sof(Q45)=Sof(Q46)=Sof(Q47)=Sof(Q48)=Sof(Q49)=Sof(Q50)=1-
 FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(1)
 Sof(P31B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33C)=Sof(H33D)=
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35C)=Sof(H35D)=
 Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=
 Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(P31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(P51B)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=Sof(H53C)=Sof(H53D)=
 Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55C)=Sof(H55D)=
 Sof(C56B)=Sof(H56C)=Sof(H56D)=Sof(C57B)=Sof(H57D)=Sof(H57E)=Sof(H57F)=
 Sof(C58B)=Sof(H58E)=Sof(H58F)=Sof(C59B)=Sof(H59E)=Sof(H59F)=Sof(C60B)=
 Sof(H60G)=Sof(H60H)=Sof(H60I)=1-FVAR(3)
 Sof(P51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=FVAR(3)
 Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=FVAR(4)
 Sof(H58C)=Sof(H58D)=Sof(C59C)=Sof(H59C)=Sof(H59D)=Sof(C60C)=Sof(H60D)=
 Sof(H60E)=Sof(H60F)=FVAR(5)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=1-FVAR(6)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=FVAR(6)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=FVAR(7)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=FVAR(8)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=FVAR(9)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=1-FVAR(10)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(10)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=1-FVAR(11)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(11)
 Fixed Sof: P51C(0) C58C(0)
9.a Free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,
 C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,
 C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,C51,C52,C53,C54,C55,C56,C57,C58,C59,
 C60), C1(C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,
 C21,C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,
 C40,C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,C51,C52,C53,C54,C55,C56,C57,C58,
 C59,C60)
9.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,
 H18B), C19(H19A,H19B), C12B(H12C,H12D), C13B(H13C,H13D), C15B(H15C,H15D),
 C16B(H16C,H16D), C18B(H18C,H18D), C19B(H19C,H19D), C32(H32A,H32B), C33(H33A,
 H33B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B),
 C32B(H32C,H32D), C33B(H33C,H33D), C35B(H35C,H35D), C36B(H36C,H36D), C38B(H38C,
 H38D), C39B(H39C,H39D), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B),
 C56(H56A,H56B), C58(H58A,H58B), C59(H59A,H59B), C58C(H58C,H58D), C59C(H59C,
 H59D), C52B(H52C,H52D), C53B(H53C,H53D), C55B(H55C,H55D), C56B(H56C,H56D),
 C58B(H58E,H58F), C59B(H59E,H59F)
9.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C14B(H14D,H14E,
 H14F), C17B(H17D,H17E,H17F), C20B(H20D,H20E,H20F), C34(H34A,H34B,H34C),
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C34B(H34D,H34E,H34F), C37B(H37D,H37E,
 H37F), C40B(H40D,H40E,H40F), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C),
 C60(H60A,H60B,H60C), C60C(H60D,H60E,H60F), C54B(H54D,H54E,H54F), C57B(H57D,
 H57E,H57F), C60B(H60G,H60H,H60I)
9.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3(H3), C4(H4), C5(H5), C6(H6),
 C7(H7), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3(H3), C4(H4), C5(H5), C6(H6),
  C7(H7), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3(H3), C4(H4), C5(H5),
 C6(H6), C7(H7)
9.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1(H1A,H1B,H1C), C1(H1A,H1B,H1C), C1(H1A,H1B,H1C), C1(H1A,
 H1B,H1C)
;