Structural Evolution of Atomically Precise Thiolated Bimetallic [Au12+nCu32(SR)30+n](4-) (n = 0, 2, 4, 6) Nanoclusters.
Yang, Huayan; Wang, Yu; Yan, Juanzhu; Chen, Xi; Zhang, Xin; Häkkinen, Hannu; Zheng, Nanfeng; Journal of the American Chemical Society 136 (2014) 7197–7200; doi:10.1021/ja501811j

data_4121794
_publ_section_title
;
 Structural Evolution of Atomically Precise Thiolated Bimetallic
 [Au12+nCu32(SR)30+n](4-) (n = 0, 2, 4, 6) Nanoclusters.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7197
_journal_page_last               7200
_journal_paper_doi               10.1021/ja501811j
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C224 H128 Au14 Cu32 F96 S32, 4(C16 H36 N)'
_chemical_formula_sum            'C290 H272 Au14 Cl4 Cu32 F96 N4 O6 S32'
_chemical_formula_weight         11691.65
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                108.611(3)
_cell_angle_beta                 105.491(3)
_cell_angle_gamma                107.174(3)
_cell_formula_units_Z            1
_cell_length_a                   20.7601(7)
_cell_length_b                   23.6955(7)
_cell_length_c                   23.7758(7)
_cell_measurement_reflns_used    18921
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.2118
_cell_measurement_theta_min      3.2590
_cell_volume                     9710.3(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.9860
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_details
;
  1 omega  -64.00   32.00   0.6000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   57.0000  -90.0000 160

  2 omega -109.00  -10.60   0.6000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424  -57.0000  120.0000 164

  3 omega  -38.00   19.00   0.6000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000   60.0000 95

  4 omega -133.00  -76.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000  -60.0000 95

  5 omega  -24.00    3.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000  -30.0000 45

  6 omega -145.00  -88.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -94.0000 -150.0000 95

  7 omega  -96.00  -51.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  125.0000  -30.0000 75

  8 omega   94.00  165.40   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000 -180.0000 119

  9 omega   60.00  120.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000   30.0000 100

 10 omega   39.00   87.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -45.0000 -120.0000 81

 11 omega   36.00   63.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000 -120.0000 46

 12 omega   84.00  114.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000 -120.0000 50

 13 omega   33.00   97.80   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000  -90.0000 108

 14 omega   50.00  172.40   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   15.0000  -60.0000 204

 15 omega   35.00   89.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000    0.0000 90

 16 omega   41.00   89.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  -90.0000 80

 17 omega   40.00  139.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -61.0000    0.0000 165

 18 omega   77.00  113.00   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -106.0000   99.0000 60

 19 omega   31.00   67.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  -30.0000 61

 20 omega  118.00  163.60   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  125.0000 -120.0000 76

 21 omega   34.00  122.20   0.6000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -61.0000  120.0000 147
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0099284000
_diffrn_orient_matrix_UB_12      -0.0010762000
_diffrn_orient_matrix_UB_13      -0.0622174000
_diffrn_orient_matrix_UB_21      0.0840876000
_diffrn_orient_matrix_UB_22      0.0300485000
_diffrn_orient_matrix_UB_23      0.0368731000
_diffrn_orient_matrix_UB_31      -0.0021072000
_diffrn_orient_matrix_UB_32      -0.0692154000
_diffrn_orient_matrix_UB_33      -0.0181884000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62770
_diffrn_reflns_theta_full        61.17
_diffrn_reflns_theta_max         61.17
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5566
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
SQUEEZE removed two disordered dichloromethane and six disordered water molecules per formula unit.
;
_refine_diff_density_max         4.468
_refine_diff_density_min         -3.979
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2010
_refine_ls_number_reflns         29663
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.712
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2785
_reflns_number_gt                21085
_reflns_number_total             29663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja501811j_si_003.cif
_cod_data_source_block           Au12@Cu32@Au2
_cod_depositor_comments
'Adding full bibliography for 4121793--4121797.cif.'
_cod_original_cell_volume        9710.2(5)
_cod_database_code               4121794
_chemical_oxdiff_formula         Au14Cu32S32F9N4Cl4C290H276N4
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 F1-C7 = F2-C7 = F3-C7
 1.4 with sigma of 0.02
 F1-F3
 2.4 with sigma of 0.02
 F3-F2
 2.4 with sigma of 0.02
 F2-F1
 2.4 with sigma of 0.02
 F7-C21 = F8-C21 = F9-C21
 1.4 with sigma of 0.02
 F7-F8
 2.4 with sigma of 0.02
 F8-F9
 2.4 with sigma of 0.02
 F9-F7
 2.4 with sigma of 0.02
 N2-C141 = N2-C137 = N2-C133 = C135-C134 = C135-C136 = C129-C130 = N2-C129 =
 C131-C130 = C131-C132 = C141-C142 = C143-C142 = C144-C143 = C138-C137 = C139-
 C138 = C139-C140
 1.5 with sigma of 0.02
 N2-C130
 2.5 with sigma of 0.02
 C129-C131
 2.5 with sigma of 0.02
 C130-C132
 2.5 with sigma of 0.02
 N2-C134
 2.5 with sigma of 0.02
 C133-C135
 2.5 with sigma of 0.02
 C134-C136
 2.5 with sigma of 0.02
 N2-C138
 2.5 with sigma of 0.02
 C137-C139
 2.5 with sigma of 0.02
 C138-C140
 2.5 with sigma of 0.02
 N2-C142
 2.5 with sigma of 0.02
 C141-C143
 2.5 with sigma of 0.02
 C142-C144
 2.5 with sigma of 0.02
 F30-C70 = F29-C70
 1.5 with sigma of 0.02
 F29-F30
 2.5 with sigma of 0.02
 C11-C14
 1.5 with sigma of 0.02
 F5-C14 = F4-C14 = F6-C14
 1.5 with sigma of 0.02
 F6-F4
 2.5 with sigma of 0.02
 F4-F5
 2.5 with sigma of 0.02
 F5-F6
 2.5 with sigma of 0.02
 F6-C14 = F5-C14 = F4-C14
 1.4 with sigma of 0.02
 F6-F4
 2.4 with sigma of 0.02
 F4-F5
 2.4 with sigma of 0.02
 F5-F6
 2.4 with sigma of 0.02
 F17-C42 = F16-C42 = F18-C42
 1.4 with sigma of 0.02
 F18-F17
 2.4 with sigma of 0.02
 F17-F16
 2.4 with sigma of 0.02
 F16-F18
 2.4 with sigma of 0.02
 F48-C112 = F46-C112 = F47-C112
 1.4 with sigma of 0.02
 F47-F48
 2.4 with sigma of 0.02
 F48-F46
 2.4 with sigma of 0.02
 F46-F47
 2.4 with sigma of 0.02
 F30-C70 = F29-C70 = F28-C70
 1.4 with sigma of 0.02
 F30-F29
 2.4 with sigma of 0.02
 F29-F28
 2.4 with sigma of 0.02
 F28-F30
 2.4 with sigma of 0.02
 C120-C119
 1.5 with sigma of 0.02
 C120-C119
 1.5 with sigma of 0.02
 C134-C133
 1.5 with sigma of 0.02
 N2-C133 = C134-C133 = C135-C134 = C136-C135 = N2-C129 = C130-C129 = C131-C130
 = C132-C131 = N2-C141 = C142-C141 = C143-C142 = C144-C143 = N2-C137 = C138-
 C137 = C139-C138 = C140-C139
 1.5 with sigma of 0.02
 C133-C129
 2.5 with sigma of 0.02
 C141-C133
 2.5 with sigma of 0.02
 C141-C137
 2.5 with sigma of 0.02
 C137-C129
 2.5 with sigma of 0.02
 C133-C135
 2.5 with sigma of 0.02
 C134-C136
 2.5 with sigma of 0.02
 N2-C130
 2.5 with sigma of 0.02
 C129-C131
 2.5 with sigma of 0.02
 C130-C132
 2.5 with sigma of 0.02
 N2-C142
 2.5 with sigma of 0.02
 C141-C143
 2.5 with sigma of 0.02
 C144-C142
 2.5 with sigma of 0.02
 N2-C138
 2.5 with sigma of 0.02
 C139-C137
 2.5 with sigma of 0.02
 C140-C138
 2.5 with sigma of 0.02
 C137-N2
 1.55 with sigma of 0.02
 C137-C133
 2.6 with sigma of 0.02
 C133-C129
 2.6 with sigma of 0.02
 C129-C141
 2.6 with sigma of 0.02
 C130-C129 = C131-C130 = C134-C133 = C142-C141 = C138-C137
 1.5 with sigma of 0.02
 F7-C21 = F8-C21 = F9-C21 = F18-C42 = F17-C42 = F16-C42 = F12-C28
 1.35 with sigma of 0.02
 C7-C3
 2.8 with sigma of 0.02
 C7-C5
 2.8 with sigma of 0.02
 C7-C4
 1.8 with sigma of 0.02
3. Rigid bond restraints
 F3, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F16, C42
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C135, C136
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F2, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C119, C120
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F1, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F4, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F10, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F12, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F4, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F7, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F10, C28
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F12, C28
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F17, C42
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F24, C56
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F25, C63
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F28, C70
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F30, C70
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F33, C77
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F38, C91
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F41, C98
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F43, C105
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F44, C105
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F47, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F48, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C2, C3
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C10, C11
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C15, C16
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C18, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C22, C23
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C26, C27
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C29, C30
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C29, C34
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C38, C39
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C39, C42
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C43, C44
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C43, C48
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C45, C46
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C57, C62
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C61, C62
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C71, C76
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C73, C74
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C85, C90
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C88, C89
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C106, C107
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 107
 C115, C116
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C123, C124
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C131, C132
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C137, C138
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C141, C142
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C142, C143
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C143, C144
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S10, C64
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F9, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F17, C42
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F30, C70
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F46, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C11, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C19, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C25, C26
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C32, C33
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C33, C34
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C33, C34
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C43, C44
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C43, C48
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C57, C62
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C71, C76
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C73, C74
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C85, C90
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C88, C87
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C101, C102
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C109, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C137, C138
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C117, C138
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S8, C8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 S10, C64
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F5, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F47, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F48, C112
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C4, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C5, C6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C8, C9
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C18, C19
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C18, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C78, C79
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C85, C90
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C102, C103
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C135 \\sim C136 \\sim C134: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C130 \\sim C129 \\sim C131: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
N2 \\sim C133 \\sim C129 \\sim C137 \\sim C141: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C134 \\sim C133 \\sim C135: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C130 \\sim C129 \\sim C131: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C139 \\sim C138 \\sim C140: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C13 \\sim C11: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C89 \\sim C90 \\sim C88: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C141 \\sim C142 \\sim N2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C109 \\sim C110 \\sim C108 \\sim C112: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C142 \\sim C143 \\sim C141: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C119 \\sim C120 \\sim C118: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C131 \\sim C132 \\sim C130: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C143 \\sim C144 \\sim C142: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C130) \\sim Ueq, Uanis(C129) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C112) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C137) = Uanis(C134) = Uanis(N2)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11A,H11B), C141(H14A,H14B), C113(H11C,H11D), C122(H12A,H12B), C143(H14C,
 H14D), C114(H11E,H11F), C121(H12C,H12D), C123(H12E,H12F), C125(H12G,H12H),
 C142(H14H,H14I), C115(H11J,H11K), C134(H13A,H13B), C126(H12I,H12J), C118(H11L,
 H11M), C127(H12K,H12L), C130(H13C,H13D), C137(H13E,H13F), C119(H11N,H11O),
 C138(H13J,H13K), C139(H13L,H13M), C129(H12V,H12W), C131(H13Q,H13R), C135(H13S,
 H13T), C133(H13U,H13V)
5.b Aromatic/amide H refined with riding coordinates:
 C69(H69), C37(H37), C38(H38), C40(H40), C41(H41), C62(H62), C68(H68),
 C51(H51), C61(H61), C44(H44), C45(H45), C47(H47), C48(H48), C65(H65),
 C104(H104), C79(H79), C93(H93), C97(H97), C100(H100), C66(H66), C52(H52),
 C31(H31), C33(H33), C34(H34), C30(H30), C59(H59), C111(H111), C94(H94),
 C23(H23), C107(H107), C108(H108), C27(H27), C103(H103), C58(H58), C83(H83),
 C20(H20), C26(H26), C16(H16), C24(H24), C19(H19), C82(H82), C101(H101),
 C110(H110), C55(H55), C96(H96), C17(H17), C80(H80), C73(H73), C75(H75),
 C76(H76), C72(H72), C5(H5), C6(H6), C2(H2), C3(H3), C54(H54), C86(H86),
 C87(H87), C89(H89), C90(H90), C9(H9), C13(H13), C12(H12), C10(H10)
5.c Fitted hexagon refined as free rotating group:
 C36(C37,C38,C39,C40,C41), C44(C45,C46,C47,C48,C43), C31(C32,C33,C34,C29,C30),
 C73(C74,C75,C76,C71,C72), C5(C6,C1,C2,C3,C4), C86(C87,C88,C89,C90,C85), C9(C8,
 C13,C12,C11,C10)
5.d Idealised Me refined as rotating group:
 C116(H11G,H11H,H11I), C144(H14E,H14F,H14G), C124(H12M,H12N,H12O), C136(H13G,
 H13H,H13I), C128(H12P,H12Q,H12R), C140(H14J,H14K,H14L), C132(H13N,H13O,H13P),
 C120(H12S,H12T,H12U)
;