# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Org.Biomol.Chem.
_journal_coden_cambridge         0177
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       jie_wu@fudan.edu.cn
_publ_contact_author_name        'Jie Wu'
loop_
_publ_author_name
'Xingxin Yu'
'Qin Yang'
'Honglei Lou'
'Yiyuan Peng'
'Jie Wu'

data_a10505c_0m
_database_code_depnum_ccdc_archive 'CCDC 826050'
#TrackingRef 'a10505c-0m.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H32 N8'
_chemical_formula_weight         528.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.636(2)
_cell_length_b                   9.930(2)
_cell_length_c                   14.630(3)
_cell_angle_alpha                88.480(2)
_cell_angle_beta                 85.747(2)
_cell_angle_gamma                80.272(2)
_cell_volume                     1375.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    3917
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SABABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6851
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.20
_reflns_number_total             4851
_reflns_number_gt                4099
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.2073P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4851
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1436
_refine_ls_wR_factor_gt          0.1335
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C28 C 0.78533(15) 0.66325(14) 0.24719(10) 0.0358(3) Uani 1 1 d . . .
C13 C 0.63842(16) -0.12205(14) 0.43393(10) 0.0399(3) Uani 1 1 d . . .
C22 C 0.55267(15) 0.59229(14) 0.25317(10) 0.0394(3) Uani 1 1 d . . .
H22 H 0.4904 0.5383 0.2801 0.047 Uiso 1 1 calc R . .
C29 C 0.74068(14) 0.75026(14) 0.17165(10) 0.0350(3) Uani 1 1 d . . .
C21 C 0.51278(15) 0.67367(14) 0.18103(10) 0.0363(3) Uani 1 1 d . . .
C23 C 0.68688(16) 0.58638(14) 0.28933(10) 0.0377(3) Uani 1 1 d . . .
C5 C 0.68747(16) 0.04933(14) 0.31920(10) 0.0411(3) Uani 1 1 d . . .
C20 C 0.37844(15) 0.68394(15) 0.13435(11) 0.0426(4) Uani 1 1 d . . .
H20A H 0.4009 0.6840 0.0686 0.051 Uiso 1 1 calc R . .
H20B H 0.3199 0.7709 0.1496 0.051 Uiso 1 1 calc R . .
C12 C 0.50284(16) -0.12292(16) 0.40068(11) 0.0437(4) Uani 1 1 d . . .
C27 C 0.91961(16) 0.65295(16) 0.28041(11) 0.0447(4) Uani 1 1 d . . .
H27 H 0.9847 0.7031 0.2524 0.054 Uiso 1 1 calc R . .
N7 N 0.69992(14) 1.00115(15) -0.00667(10) 0.0588(4) Uani 1 1 d . . .
H7A H 0.6277 1.0313 -0.0370 0.071 Uiso 1 1 calc R . .
H7B H 0.7766 1.0342 -0.0173 0.071 Uiso 1 1 calc R . .
C30 C 0.80019(15) 0.84323(15) 0.11446(10) 0.0385(3) Uani 1 1 d . . .
C31 C 0.69298(15) 0.90205(15) 0.05759(10) 0.0395(3) Uani 1 1 d . . .
C6 C 0.56037(17) 0.04844(16) 0.28694(11) 0.0467(4) Uani 1 1 d . . .
H6 H 0.5341 0.1049 0.2372 0.056 Uiso 1 1 calc R . .
C7 C 0.46413(17) -0.03577(16) 0.32595(11) 0.0462(4) Uani 1 1 d . . .
C24 C 0.72657(18) 0.50338(15) 0.36552(10) 0.0460(4) Uani 1 1 d . . .
H24 H 0.6627 0.4532 0.3949 0.055 Uiso 1 1 calc R . .
C26 C 0.95514(18) 0.56951(18) 0.35371(12) 0.0526(4) Uani 1 1 d . . .
H26 H 1.0448 0.5621 0.3749 0.063 Uiso 1 1 calc R . .
C15 C 0.84176(16) -0.13607(15) 0.50012(10) 0.0421(3) Uani 1 1 d . . .
C8 C 0.33071(18) -0.03428(19) 0.29265(13) 0.0579(5) Uani 1 1 d . . .
H8 H 0.3035 0.0223 0.2432 0.069 Uiso 1 1 calc R . .
C4 C 0.79592(18) 0.13235(16) 0.28398(11) 0.0467(4) Uani 1 1 d . . .
H4A H 0.8843 0.0710 0.2708 0.056 Uiso 1 1 calc R . .
H4B H 0.8104 0.1925 0.3323 0.056 Uiso 1 1 calc R . .
C32 C 0.93609(15) 0.87808(16) 0.11319(11) 0.0444(4) Uani 1 1 d . . .
C11 C 0.40855(18) -0.20509(19) 0.43992(13) 0.0559(4) Uani 1 1 d . . .
H11 H 0.4339 -0.2627 0.4893 0.067 Uiso 1 1 calc R . .
C19 C 0.29332(16) 0.57076(16) 0.15862(11) 0.0461(4) Uani 1 1 d . . .
H19A H 0.2820 0.5619 0.2248 0.055 Uiso 1 1 calc R . .
H19B H 0.2000 0.5968 0.1364 0.055 Uiso 1 1 calc R . .
C3 C 0.76155(18) 0.21848(16) 0.19886(11) 0.0496(4) Uani 1 1 d . . .
H3A H 0.7387 0.1607 0.1517 0.060 Uiso 1 1 calc R . .
H3B H 0.6791 0.2872 0.2132 0.060 Uiso 1 1 calc R . .
C14 C 0.71503(17) -0.18899(15) 0.50397(10) 0.0428(4) Uani 1 1 d . . .
C25 C 0.85780(19) 0.49546(17) 0.39687(11) 0.0515(4) Uani 1 1 d . . .
H25 H 0.8823 0.4402 0.4474 0.062 Uiso 1 1 calc R . .
C9 C 0.24057(19) -0.1149(2) 0.33202(14) 0.0654(5) Uani 1 1 d . . .
H9 H 0.1525 -0.1125 0.3094 0.078 Uiso 1 1 calc R . .
C10 C 0.2796(2) -0.2006(2) 0.40576(14) 0.0664(5) Uani 1 1 d . . .
H10 H 0.2175 -0.2553 0.4320 0.080 Uiso 1 1 calc R . .
C16 C 0.67750(19) -0.29100(18) 0.56569(12) 0.0528(4) Uani 1 1 d . . .
C2 C 0.8824(2) 0.28807(18) 0.16255(12) 0.0577(4) Uani 1 1 d . . .
H2A H 0.9644 0.2191 0.1475 0.069 Uiso 1 1 calc R . .
H2B H 0.9061 0.3446 0.2102 0.069 Uiso 1 1 calc R . .
C18 C 0.3594(2) 0.43343(18) 0.11942(14) 0.0618(5) Uani 1 1 d . . .
H18A H 0.3740 0.4425 0.0534 0.074 Uiso 1 1 calc R . .
H18B H 0.4509 0.4050 0.1437 0.074 Uiso 1 1 calc R . .
C17 C 0.2695(3) 0.3250(3) 0.14165(19) 0.1010(9) Uani 1 1 d . . .
H17A H 0.2499 0.3193 0.2068 0.151 Uiso 1 1 calc R . .
H17B H 0.3189 0.2384 0.1198 0.151 Uiso 1 1 calc R . .
H17C H 0.1823 0.3480 0.1125 0.151 Uiso 1 1 calc R . .
C1 C 0.8487(3) 0.3765(2) 0.07790(14) 0.0777(6) Uani 1 1 d . . .
H1A H 0.8263 0.3209 0.0302 0.117 Uiso 1 1 calc R . .
H1B H 0.9291 0.4175 0.0573 0.117 Uiso 1 1 calc R . .
H1C H 0.7695 0.4468 0.0928 0.117 Uiso 1 1 calc R . .
N3 N 0.95094(15) -0.17263(14) 0.55511(10) 0.0551(4) Uani 1 1 d . . .
H3C H 1.0256 -0.1359 0.5466 0.066 Uiso 1 1 calc R . .
H3D H 0.9450 -0.2324 0.5982 0.066 Uiso 1 1 calc R . .
N8 N 1.04512(15) 0.90936(18) 0.11106(12) 0.0675(5) Uani 1 1 d . . .
N4 N 0.6516(2) -0.37482(19) 0.61608(12) 0.0805(5) Uani 1 1 d . . .
N5 N 0.60745(12) 0.75563(12) 0.14516(8) 0.0354(3) Uani 1 1 d . . .
N1 N 0.72237(13) -0.03690(12) 0.39318(8) 0.0387(3) Uani 1 1 d . . .
N6 N 0.57598(12) 0.84918(12) 0.07539(8) 0.0406(3) Uani 1 1 d . . .
N2 N 0.84862(13) -0.04424(12) 0.43321(9) 0.0425(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C28 0.0360(7) 0.0337(7) 0.0370(7) 0.0021(6) -0.0034(6) -0.0037(6)
C13 0.0439(8) 0.0363(7) 0.0397(8) -0.0036(6) 0.0027(6) -0.0089(6)
C22 0.0393(8) 0.0375(7) 0.0426(8) 0.0077(6) -0.0009(6) -0.0117(6)
C29 0.0295(7) 0.0348(7) 0.0403(8) 0.0030(6) -0.0027(6) -0.0049(5)
C21 0.0329(7) 0.0352(7) 0.0414(8) 0.0057(6) -0.0003(6) -0.0093(6)
C23 0.0415(8) 0.0337(7) 0.0373(7) 0.0026(6) -0.0027(6) -0.0053(6)
C5 0.0460(8) 0.0346(7) 0.0423(8) 0.0003(6) -0.0052(7) -0.0047(6)
C20 0.0356(8) 0.0451(8) 0.0481(8) 0.0107(6) -0.0063(6) -0.0099(6)
C12 0.0424(8) 0.0444(8) 0.0443(8) -0.0093(7) 0.0044(7) -0.0089(7)
C27 0.0386(8) 0.0465(8) 0.0494(9) 0.0049(7) -0.0092(7) -0.0066(6)
N7 0.0375(7) 0.0680(9) 0.0728(10) 0.0390(8) -0.0102(7) -0.0181(6)
C30 0.0310(7) 0.0405(7) 0.0439(8) 0.0086(6) -0.0014(6) -0.0079(6)
C31 0.0322(7) 0.0414(8) 0.0446(8) 0.0119(6) -0.0012(6) -0.0084(6)
C6 0.0495(9) 0.0445(8) 0.0464(9) 0.0020(7) -0.0094(7) -0.0064(7)
C7 0.0423(8) 0.0467(9) 0.0495(9) -0.0090(7) -0.0036(7) -0.0056(7)
C24 0.0548(9) 0.0419(8) 0.0415(8) 0.0090(6) -0.0069(7) -0.0089(7)
C26 0.0481(9) 0.0564(10) 0.0535(10) 0.0043(8) -0.0185(8) -0.0032(7)
C15 0.0458(8) 0.0357(7) 0.0443(8) 0.0028(6) -0.0048(7) -0.0058(6)
C8 0.0470(10) 0.0643(11) 0.0630(11) -0.0080(9) -0.0104(8) -0.0072(8)
C4 0.0497(9) 0.0434(8) 0.0487(9) 0.0058(7) -0.0091(7) -0.0111(7)
C32 0.0330(8) 0.0469(8) 0.0525(9) 0.0147(7) -0.0019(6) -0.0074(6)
C11 0.0509(10) 0.0635(11) 0.0554(10) -0.0038(8) 0.0052(8) -0.0187(8)
C19 0.0346(8) 0.0565(9) 0.0498(9) 0.0121(7) -0.0063(6) -0.0157(7)
C3 0.0575(10) 0.0452(9) 0.0480(9) 0.0072(7) -0.0128(8) -0.0116(7)
C14 0.0483(9) 0.0380(8) 0.0421(8) 0.0016(6) -0.0003(7) -0.0088(6)
C25 0.0619(10) 0.0478(9) 0.0436(9) 0.0093(7) -0.0156(8) -0.0021(8)
C9 0.0423(10) 0.0820(13) 0.0744(13) -0.0160(10) -0.0038(9) -0.0155(9)
C10 0.0507(10) 0.0818(13) 0.0713(12) -0.0095(10) 0.0091(9) -0.0290(10)
C16 0.0588(10) 0.0532(10) 0.0479(9) 0.0069(7) -0.0024(8) -0.0158(8)
C2 0.0674(11) 0.0536(10) 0.0540(10) 0.0095(8) -0.0061(9) -0.0166(8)
C18 0.0624(11) 0.0546(10) 0.0727(12) 0.0031(9) -0.0177(9) -0.0173(9)
C17 0.146(3) 0.0779(15) 0.0960(18) 0.0060(13) -0.0226(17) -0.0627(17)
C1 0.1013(17) 0.0762(14) 0.0593(12) 0.0210(10) -0.0093(11) -0.0270(12)
N3 0.0531(8) 0.0526(8) 0.0616(9) 0.0195(7) -0.0167(7) -0.0125(6)
N8 0.0388(8) 0.0791(11) 0.0873(12) 0.0263(9) -0.0062(7) -0.0206(7)
N4 0.0965(14) 0.0810(12) 0.0698(11) 0.0289(9) -0.0061(10) -0.0359(10)
N5 0.0302(6) 0.0359(6) 0.0404(6) 0.0097(5) -0.0036(5) -0.0074(5)
N1 0.0412(7) 0.0352(6) 0.0405(6) 0.0006(5) -0.0045(5) -0.0082(5)
N6 0.0337(6) 0.0435(7) 0.0450(7) 0.0180(5) -0.0058(5) -0.0093(5)
N2 0.0427(7) 0.0380(6) 0.0480(7) 0.0048(5) -0.0096(6) -0.0081(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C28 C27 1.402(2) . ?
C28 C23 1.413(2) . ?
C28 C29 1.4308(19) . ?
C13 N1 1.3629(18) . ?
C13 C14 1.395(2) . ?
C13 C12 1.429(2) . ?
C22 C21 1.351(2) . ?
C22 C23 1.425(2) . ?
C29 N5 1.3605(18) . ?
C29 C30 1.3958(19) . ?
C21 N5 1.3882(17) . ?
C21 C20 1.495(2) . ?
C23 C24 1.406(2) . ?
C5 C6 1.346(2) . ?
C5 N1 1.3875(19) . ?
C5 C4 1.492(2) . ?
C20 C19 1.520(2) . ?
C12 C11 1.403(2) . ?
C12 C7 1.409(2) . ?
C27 C26 1.366(2) . ?
N7 C31 1.3493(18) . ?
C30 C32 1.409(2) . ?
C30 C31 1.414(2) . ?
C31 N6 1.3281(18) . ?
C6 C7 1.429(2) . ?
C7 C8 1.406(2) . ?
C24 C25 1.366(2) . ?
C26 C25 1.393(2) . ?
C15 N2 1.3257(19) . ?
C15 N3 1.366(2) . ?
C15 C14 1.406(2) . ?
C8 C9 1.365(3) . ?
C4 C3 1.517(2) . ?
C32 N8 1.143(2) . ?
C11 C10 1.367(3) . ?
C19 C18 1.512(3) . ?
C3 C2 1.509(2) . ?
C14 C16 1.414(2) . ?
C9 C10 1.390(3) . ?
C16 N4 1.144(2) . ?
C2 C1 1.522(2) . ?
C18 C17 1.507(3) . ?
N5 N6 1.3774(16) . ?
N1 N2 1.3790(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 C28 C23 119.87(13) . . ?
C27 C28 C29 123.01(13) . . ?
C23 C28 C29 117.12(13) . . ?
N1 C13 C14 105.21(13) . . ?
N1 C13 C12 118.99(14) . . ?
C14 C13 C12 135.79(14) . . ?
C21 C22 C23 122.21(13) . . ?
N5 C29 C30 105.43(12) . . ?
N5 C29 C28 118.96(12) . . ?
C30 C29 C28 135.56(13) . . ?
C22 C21 N5 116.69(13) . . ?
C22 C21 C20 127.19(13) . . ?
N5 C21 C20 116.12(12) . . ?
C24 C23 C28 118.23(14) . . ?
C24 C23 C22 121.87(14) . . ?
C28 C23 C22 119.88(13) . . ?
C6 C5 N1 116.66(14) . . ?
C6 C5 C4 127.26(14) . . ?
N1 C5 C4 116.08(13) . . ?
C21 C20 C19 115.14(12) . . ?
C11 C12 C7 119.78(15) . . ?
C11 C12 C13 122.71(16) . . ?
C7 C12 C13 117.51(14) . . ?
C26 C27 C28 120.20(15) . . ?
C29 C30 C32 128.86(13) . . ?
C29 C30 C31 105.70(12) . . ?
C32 C30 C31 125.41(13) . . ?
N6 C31 N7 121.28(13) . . ?
N6 C31 C30 111.46(12) . . ?
N7 C31 C30 127.24(13) . . ?
C5 C6 C7 122.68(15) . . ?
C8 C7 C12 118.40(16) . . ?
C8 C7 C6 122.22(16) . . ?
C12 C7 C6 119.38(14) . . ?
C25 C24 C23 120.82(15) . . ?
C27 C26 C25 120.34(15) . . ?
N2 C15 N3 121.06(14) . . ?
N2 C15 C14 112.24(14) . . ?
N3 C15 C14 126.68(14) . . ?
C9 C8 C7 120.81(19) . . ?
C5 C4 C3 115.74(13) . . ?
N8 C32 C30 178.29(17) . . ?
C10 C11 C12 120.12(18) . . ?
C18 C19 C20 113.89(14) . . ?
C2 C3 C4 112.26(14) . . ?
C13 C14 C15 105.61(13) . . ?
C13 C14 C16 128.36(15) . . ?
C15 C14 C16 126.02(15) . . ?
C24 C25 C26 120.52(15) . . ?
C8 C9 C10 120.42(18) . . ?
C11 C10 C9 120.47(18) . . ?
N4 C16 C14 177.8(2) . . ?
C3 C2 C1 112.85(16) . . ?
C17 C18 C19 112.48(19) . . ?
C29 N5 N6 112.77(11) . . ?
C29 N5 C21 124.81(12) . . ?
N6 N5 C21 122.39(11) . . ?
C13 N1 N2 112.95(12) . . ?
C13 N1 C5 124.77(13) . . ?
N2 N1 C5 122.28(12) . . ?
C31 N6 N5 104.62(11) . . ?
C15 N2 N1 103.99(12) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.087