Self-Assembly of Goldberg Polyhedra from a Concave [WV<sub>5</sub>O<sub>11</sub>(RCO<sub>2</sub>)<sub>5</sub>(SO<sub>4</sub>)]<sup>3-</sup> Building Block with 5-Fold Symmetry.
Zhang, Yuteng; Gan, Hongmei; Qin, Chao; Wang, Xinlong; Su, Zhongmin; Zaworotko, Michael J.; Journal of the American Chemical Society 140 (2018) 17365–17368; doi:10.1021/jacs.8b10866

data_4133537
_publ_section_title
;
 Self-Assembly of Goldberg Polyhedra from a Concave
 [WV<sub>5</sub>O<sub>11</sub>(RCO<sub>2</sub>)<sub>5</sub>(SO<sub>4</sub>)]<sup>3-</sup>
 Building Block with 5-Fold Symmetry.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17365
_journal_page_last               17368
_journal_paper_doi               10.1021/jacs.8b10866
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C480 H240 N60 O324 S10 V60 W12, C60'
_chemical_formula_sum            'C540 H240 N60 O324 S10 V60 W12'
_chemical_formula_weight         18335.11
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   41.893(3)
_cell_length_b                   41.893(3)
_cell_length_c                   53.783(4)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.470
_cell_measurement_theta_min      2.497
_cell_volume                     94390(12)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            120615
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        57.470
_diffrn_reflns_theta_max         57.470
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.095
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17840
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.711
_refine_diff_density_min         -2.366
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.000009(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1355
_refine_ls_number_reflns         32010
_refine_ls_number_restraints     15002
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.2185
_refine_ls_R_factor_gt           0.1385
_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^)+(0.3500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3897
_refine_ls_wR_factor_ref         0.4988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14639
_reflns_number_total             32010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10866_si_002.cif
_cod_data_source_block           GMOP-4.C60
_cod_original_cell_volume        94393(15)
_cod_database_code               4133537
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 W1-O1 = W2-O37 = W3-O14
 2.2 with sigma of 0.02
 S3-S4 = V1-O45 = V6-O47 = S2-O45 = S2-O47
 1.45 with sigma of 0.02
 S2-O45 = S2-O14 = S2-O47 = S2-S1
 1.45 with sigma of 0.02
 S3-O1 = S3-S4
 1.45 with sigma of 0.01
 S3-S4 = S3-O1 = S3-O42 = S3-O41
 1.45 with sigma of 0.02
 S1-O14 = S1-O40 = S1-O48
 1.45 with sigma of 0.02
 S5-O47 = S5-O14 = S5-O48
 1.45 with sigma of 0.02
 S6-O37 = S6-O46 = S6-O44
 1.45 with sigma of 0.02
 S4-O1 = S4-O49
 1.45 with sigma of 0.02
 C65-C64_$1 = C65-C64 = C64-C62 = C62-C61_$2 = C62_$1-C61_$2 = C64_$1-C62_$1
 1.38 with sigma of 0.01
 C65-C31 = C63_$2-C61_$2
 1.45 with sigma of 0.02
 N3_$1-C38_$1 = N9-C38_$1 = N9-C38 = N3-C38 = N3-C31 = N3_$1-C31
 1.38 with sigma of 0.01
 C60-C55 = C60-C58 = C58-C56 = C59-C56 = C59-C57 = C57-C55
 1.38 with sigma of 0.01
 N7-C47 = N7-C47_$3 = N2_$3-C47_$3 = N2_$3-C42 = N2-C42 = N2-C47
 1.38 with sigma of 0.01
 N7-C42
 2.75 with sigma of 0.02
 C47-N2_$3
 2.75 with sigma of 0.02
 N2-C47_$3
 2.75 with sigma of 0.02
 N2-N2_$3
 2.38 with sigma of 0.01
 N2_$3-N7
 2.38 with sigma of 0.01
 N2-N7
 2.38 with sigma of 0.01
 C47-C47_$3
 2.38 with sigma of 0.01
 C1F-C1E \\sim C1H-C1G \\sim C1I-C1A \\sim C1K-C1J \\sim C1L-C1B \\sim C1M-C1N
\\sim C1O-C1C \\sim C1Q-C1P
 \\sim C1R-C1D \\sim C1S-C1T \\sim C1V-C1W \\sim C1X-C1Y \\sim C1Z-C2A \\sim
C2B-C2C \\sim C2D-C2E \\sim C2G-
 C2F \\sim C2I-C2H \\sim C2K-C2J \\sim C2M-C2L \\sim C2N-C1U \\sim C2P-C2O
\\sim C2R-C2S \\sim C2T-C3F ~
 C2U-C2V \\sim C2Y-C2X \\sim C2Z-C3H \\sim C3B-C3A \\sim C3C-C3D \\sim C3E-C2Q
\\sim C3G-C2W
 with sigma of 0.02
 C1A-C1E \\sim C1B-C1A \\sim C1C-C1D \\sim C1C-C1B \\sim C1E-C1D \\sim C1F-C1T
\\sim C1G-C1F \\sim C1G-C1V
 \\sim C1H-C1Y \\sim C1I-C1H \\sim C1J-C1I \\sim C1J-C1Z \\sim C1K-C2C \\sim
C1L-C1K \\sim C1M-C2D \\sim C1M-
 C1L \\sim C1N-C2G \\sim C1O-C1P \\sim C1O-C1N \\sim C1Q-C2K \\sim C1R-C1Q
\\sim C1S-C2L \\sim C1S-C1R ~
 C1T-C1U \\sim C1V-C1U \\sim C1W-C1X \\sim C1Z-C1Y \\sim C2A-C2B \\sim C2D-C2C
\\sim C2E-C2V \\sim C2E-C2F
 \\sim C2H-C1P \\sim C2H-C2G \\sim C2I-C2J \\sim C2L-C2K \\sim C2M-C2N \\sim
C2N-C2O \\sim C2P-C1W \\sim C2P-
 C2Q \\sim C2R-C1X \\sim C2R-C2Q \\sim C2S-C2T \\sim C2S-C2A \\sim C2T-C2U
\\sim C2U-C2B \\sim C2V-C2W ~
 C2X-C2W \\sim C2X-C2F \\sim C2Y-C2I \\sim C2Z-C2Y \\sim C3A-C2Z \\sim C3A-C2J
\\sim C3B-C2M \\sim C3C-C3B
 \\sim C3C-C2O \\sim C3E-C3F \\sim C3E-C3D \\sim C3G-C3H \\sim C3G-C3F \\sim
C3H-C3D
 with sigma of 0.02
 C1B-C1E \\sim C1H-C1J \\sim C1M-C2C \\sim C1O-C2H \\sim C1R-C2K \\sim C1T-C1V
\\sim C1X-C2Q \\sim C2A-C2T
 \\sim C2F-C2V \\sim C2M-C2O \\sim C2Y-C3A \\sim C3D-C3G \\sim C1B-C1D \\sim
C1C-C1E \\sim C1F-C1V \\sim C1G-
 C1T \\sim C1H-C1Z \\sim C1J-C1Y \\sim C1K-C1M \\sim C1L-C2C \\sim C1N-C2H
\\sim C1O-C2G \\sim C1R-C2L ~
 C1S-C2K \\sim C1W-C2Q \\sim C1X-C2P \\sim C2A-C2U \\sim C2B-C2T \\sim C2F-C2W
\\sim C2I-C3A \\sim C2J-C2Y
 \\sim C2M-C3C \\sim C2O-C3B \\sim C2V-C2X \\sim C3D-C3F \\sim C3E-C3G \\sim
C1A-C1C \\sim C1A-C1D \\sim C1F-
 C1U \\sim C1G-C1U \\sim C1I-C1Y \\sim C1I-C1Z \\sim C1K-C2D \\sim C1L-C2D
\\sim C1N-C1P \\sim C1P-C2G ~
 C1Q-C2L \\sim C1Q-C1S \\sim C1W-C2R \\sim C2B-C2S \\sim C2E-C2W \\sim C2E-C2X
\\sim C2I-C2Z \\sim C2J-C2Z
 \\sim C2N-C3B \\sim C2N-C3C \\sim C2P-C2R \\sim C2S-C2U \\sim C3E-C3H \\sim
C3F-C3H
 with sigma of 0.04
 C1A-C1L \\sim C1A-C1F \\sim C1B-C1O \\sim C1B-C1M \\sim C1C-C1P \\sim C1D-C1Q
\\sim C1E-C1T \\sim C1E-C1R
 \\sim C1G-C1I \\sim C1H-C1V \\sim C1H-C1X \\sim C1I-C1K \\sim C1J-C2A \\sim
C1J-C2C \\sim C1M-C1O \\sim C1N-
 C2D \\sim C1P-C2I \\sim C1Q-C2J \\sim C1R-C1T \\sim C1S-C1U \\sim C1U-C1W
\\sim C1V-C1X \\sim C1Y-C2R ~
 C1Z-C2S \\sim C2A-C2C \\sim C2B-C2D \\sim C2E-C2U \\sim C2E-C2G \\sim C2F-C2H
\\sim C2F-C2Y \\sim C2H-C2Y
 \\sim C2K-C3A \\sim C2K-C2M \\sim C2L-C2N \\sim C2M-C3A \\sim C2N-C2P \\sim
C2O-C3D \\sim C2O-C2Q \\sim C2Q-
 C3D \\sim C2R-C3E \\sim C2S-C3F \\sim C2T-C2V \\sim C2T-C3G \\sim C2V-C3G
\\sim C2W-C3H \\sim C2X-C2Z ~
 C2Z-C3B \\sim C3C-C3H \\sim C1A-C1H \\sim C1A-C1J \\sim C1B-C1K \\sim C1B-C1I
\\sim C1C-C1R \\sim C1D-C1O
 \\sim C1E-C1I \\sim C1E-C1G \\sim C1F-C1H \\sim C1J-C1L \\sim C1M-C2E \\sim
C1M-C2G \\sim C1N-C2F \\sim C1O-
 C1Q \\sim C1P-C2K \\sim C1P-C1R \\sim C1Q-C2H \\sim C1S-C2M \\sim C1T-C2L
\\sim C1T-C2N \\sim C1U-C2M ~
 C1U-C2O \\sim C1V-C2P \\sim C1V-C2N \\sim C1W-C2O \\sim C1X-C2S \\sim C1X-C1Z
\\sim C1Y-C2A \\sim C2A-C2R
 \\sim C2B-C2V \\sim C2C-C2U \\sim C2C-C2E \\sim C2D-C2V \\sim C2D-C2F \\sim
C2H-C2J \\sim C2I-C2K \\sim C2Q-
 C2S \\sim C2Q-C3F \\sim C2R-C2T \\sim C2T-C3E \\sim C2W-C2Y \\sim C2X-C3G
\\sim C2Y-C3H \\sim C2Z-C3D ~
 C2Z-C3G \\sim C3A-C3C \\sim C3A-C3H \\sim C3B-C3D \\sim C1C-C1L \\sim C1C-C1N
\\sim C1D-C1S \\sim C1D-C1F
 \\sim C1F-C1S \\sim C1G-C1W \\sim C1G-C1Y \\sim C1K-C2B \\sim C1K-C1Z \\sim
C1L-C1N \\sim C1W-C1Y \\sim C1Z-
 C2B \\sim C2G-C2I \\sim C2G-C2X \\sim C2I-C2X \\sim C2J-C2L \\sim C2J-C3B
\\sim C2L-C3B \\sim C2P-C3C ~
 C2P-C3E \\sim C2U-C2W \\sim C2U-C3F \\sim C2W-C3F \\sim C3C-C3E
 with sigma of 0.04
3. Restrained planarity
 C65, C64, C62, C61_$2, C62_$1, C64_$1
 with sigma of 0.1
 N3_$1, C38_$1, N9, C38, N3, C31
 with sigma of 0.1
 C55, C60, C58, C56, C59, C57
 with sigma of 0.1
 N7, C47_$3, N2_$3, C42, N2, C47
 with sigma of 0.1
 C21, C49, C52, C46, C22, C26, N7, C47, N2, C42, C37, C45, C36, C13
 with sigma of 0.05
 C1A, C1E, C1F, C1I
 with sigma of 0.1
 C1A, C1B, C1C, C1E
 with sigma of 0.1
 C1A, C1B, C1K, C1L
 with sigma of 0.1
 C1A, C1E, C1F, C1G
 with sigma of 0.1
 C1B, C1J, C1K, C1L
 with sigma of 0.1
 C1D, C1E, C1F, C1R
 with sigma of 0.1
 C1E, C1F, C1G, C1H
 with sigma of 0.1
 C1F, C1G, C1T, C1U
 with sigma of 0.1
 C1G, C1H, C1V, C1W
 with sigma of 0.1
 C1H, C1I, C1J, C1Y
 with sigma of 0.1
 C1H, C1I, C1Y, C1Z
 with sigma of 0.1
 C1K, C1M, C2C, C2D
 with sigma of 0.1
 C1K, C1L, C2C, C2D
 with sigma of 0.1
 C1N, C1O, C2G, C2H
 with sigma of 0.1
 C1N, C1O, C1P, C2G
 with sigma of 0.1
 C1Q, C1R, C1S, C2K
 with sigma of 0.1
 C1Q, C1R, C2K, C2L
 with sigma of 0.1
 C1X, C1Y, C1Z, C2R
 with sigma of 0.1
 C1Y, C1Z, C2A, C2S
 with sigma of 0.1
 C2A, C2B, C2S, C2T
 with sigma of 0.1
 C2A, C2S, C2T, C2U
 with sigma of 0.1
 C2E, C2V, C2W, C2X
 with sigma of 0.1
 C2F, C2G, C2X, C2Y
 with sigma of 0.1
 C2F, C2V, C2W, C2X
 with sigma of 0.1
 C2H, C2I, C2X, C2Y
 with sigma of 0.1
 C2J, C2Y, C2Z, C3A
 with sigma of 0.1
 C2M, C2N, C3B, C3C
 with sigma of 0.1
 C2M, C2N, C2O, C3B
 with sigma of 0.1
 C2O, C2P, C3C, C3D
 with sigma of 0.1
 C2O, C2P, C2Q, C3E
 with sigma of 0.1
 C2T, C2U, C2V, C3F
 with sigma of 0.1
 C2T, C2U, C2V, C2W
 with sigma of 0.1
 C2W, C2Z, C3G, C3H
 with sigma of 0.1
 C2X, C2Y, C2Z, C3H
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C32 \\sim C51
\\sim C33 \\sim C43 \\sim C50 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28
\\sim C29 \\sim C30 \\sim C31 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38
\\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C44 \\sim C45 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G
\\sim C1H \\sim C1I \\sim C1J \\sim C1K \\sim C1L \\sim C1M \\sim C1N \\sim C1O
\\sim C1P \\sim C1Q \\sim C1R \\sim C1S \\sim C1T \\sim C1U \\sim C1V \\sim C1W
\\sim C1X \\sim C1Y \\sim C1Z \\sim C2A \\sim C2B \\sim C2C \\sim C2D \\sim C2E
\\sim C2F \\sim C2G \\sim C2H \\sim C2I \\sim C2J \\sim C2K \\sim C2L \\sim C2M
\\sim C2N \\sim C2O \\sim C2P \\sim C2Q \\sim C2R \\sim C2S \\sim C2T \\sim C2U
\\sim C2V \\sim C2W \\sim C2X \\sim C2Y \\sim C2Z \\sim C3A \\sim C3B \\sim C3C
\\sim C3D \\sim C3E \\sim C3F \\sim C3G \\sim C3H \\sim O1 \\sim O2 \\sim O3
\\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim
O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim
O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim
O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim
O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim
O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim N1 \\sim N2 \\sim
N3 \\sim N7 \\sim N8 \\sim N9 \\sim N4 \\sim N5 \\sim N6 \\sim S1 \\sim S2
\\sim S3 \\sim S4 \\sim S5 \\sim S6: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.03
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G \\sim C1H \\sim
C1I \\sim C1J \\sim C1K \\sim C1L \\sim C1M \\sim C1N \\sim C1O \\sim C1P \\sim
C1Q \\sim C1R \\sim C1S \\sim C1T \\sim C1U \\sim C1V \\sim C1W \\sim C1X \\sim
C1Y \\sim C1Z \\sim C2A \\sim C2B \\sim C2C \\sim C2D \\sim C2E \\sim C2F \\sim
C2G \\sim C2H \\sim C2I \\sim C2J \\sim C2K \\sim C2L \\sim C2M \\sim C2N \\sim
C2O \\sim C2P \\sim C2Q \\sim C2R \\sim C2S \\sim C2T \\sim C2U \\sim C2V \\sim
C2W \\sim C2X \\sim C2Y \\sim C2Z \\sim C3A \\sim C3B \\sim C3C \\sim C3D \\sim
C3E \\sim C3F \\sim C3G \\sim C3H: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C31) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G, C1H, C1I, C1J, C1K, C1L, C1M, C1N, C1O,
 C1P, C1Q, C1R, C1S, C1T, C1U, C1V, C1W, C1X, C1Y, C1Z, C2A, C2B, C2C, C2D, C2E,
  C2F, C2G, C2H, C2I, C2J, C2K, C2L, C2M, C2N, C2O, C2P, C2Q, C2R, C2S, C2T,
 C2U, C2V, C2W, C2X, C2Y, C2Z, C3A, C3B, C3C, C3D, C3E, C3F, C3G, C3H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: S1(0.125) S2(0.25) S3(0.25) S4(0.25) S5(0.125) S6(0.25) C1A(0.125)
 C1B(0.125) C1C(0.125) C1D(0.125) C1E(0.125) C1F(0.125) C1G(0.125) C1H(0.125)
 C1I(0.125) C1J(0.125) C1K(0.125) C1L(0.125) C1M(0.125) C1N(0.125) C1O(0.125)
 C1P(0.125) C1Q(0.125) C1R(0.125) C1S(0.125) C1T(0.125) C1U(0.125) C1V(0.125)
 C1W(0.125) C1X(0.125) C1Y(0.125) C1Z(0.125) C2A(0.125) C2B(0.125) C2C(0.125)
 C2D(0.125) C2E(0.125) C2F(0.125) C2G(0.125) C2H(0.125) C2I(0.125) C2J(0.125)
 C2K(0.125) C2L(0.125) C2M(0.125) C2N(0.125) C2O(0.125) C2P(0.125) C2Q(0.125)
 C2R(0.125) C2S(0.125) C2T(0.125) C2U(0.125) C2V(0.125) C2W(0.125) C2X(0.125)
 C2Y(0.125) C2Z(0.125) C3A(0.125) C3B(0.125) C3C(0.125) C3D(0.125) C3E(0.125)
 C3F(0.125) C3G(0.125) C3H(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C32(H32),
 C51(H51), C43(H43), C50(H50), C24(H24), C26(H26), C27(H27), C28(H28), C30(H30),
  C35(H35), C36(H36), C39(H39), C41(H41), C44(H44), C45(H45), C49(H49),
 C52(H52), C53(H53), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C64(H64)
7.b Fitted hexagon refined as free rotating group:
 C10(N4,C11,N5,C12,N6), C14(C15,C16,C17,C18,C19), C23(C32,C51,C33,C43,C50)
;