# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_140623D
_database_code_depnum_ccdc_archive 'CCDC 1012979'
_audit_update_record             
;
2014-07-09 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H66 Br2 N6 O7'
_chemical_formula_weight         1179.02

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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.6110(16)
_cell_length_b                   14.920(2)
_cell_length_c                   12.644(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.924(8)
_cell_angle_gamma                90.00
_cell_volume                     2907.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1908
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      19.16

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5806
_exptl_absorpt_correction_T_max  0.6229
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16139
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5093
_reflns_number_gt                2544
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0943P)²+0.0000P] where P=(Fo²+2Fc²)/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         5093
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1858
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.002
_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
O1 O 0.1041(2) -0.9806(3) 0.1029(3) 0.0704(10) Uani 1 1 d . . .
O2 O 0.1911(2) -0.6137(3) -0.0755(4) 0.0888(13) Uani 1 1 d . . .
O3 O 0.1997(2) -0.3165(2) -0.0665(4) 0.0862(13) Uani 1 1 d . . .
N1 N 0.3517(2) -0.5492(3) 0.0282(3) 0.0517(10) Uani 1 1 d . . .
N2 N 0.3535(2) -0.4024(3) 0.0351(3) 0.0518(10) Uani 1 1 d . . .
N3 N 0.2337(3) -0.0270(3) -0.1113(3) 0.0522(10) Uani 1 1 d . . .
C1 C 0.1530(4) -1.0349(4) 0.1999(5) 0.091(2) Uani 1 1 d . . .
H1A H 0.1194 -1.0866 0.2029 0.136 Uiso 1 1 calc R . .
H1B H 0.1660 -1.0005 0.2684 0.136 Uiso 1 1 calc R . .
H1C H 0.2060 -1.0538 0.1930 0.136 Uiso 1 1 calc R . .
C2 C 0.1405(3) -0.9042(3) 0.0843(4) 0.0531(13) Uani 1 1 d . . .
C3 C 0.0920(3) -0.8559(4) -0.0116(4) 0.0576(14) Uani 1 1 d . . .
H3A H 0.0373 -0.8763 -0.0581 0.069 Uiso 1 1 calc R . .
C4 C 0.1238(3) -0.7787(4) -0.0387(4) 0.0555(13) Uani 1 1 d . . .
H4A H 0.0898 -0.7463 -0.1026 0.067 Uiso 1 1 calc R . .
C5 C 0.2070(3) -0.7471(3) 0.0280(4) 0.0509(13) Uani 1 1 d . . .
C6 C 0.2539(3) -0.7961(3) 0.1255(5) 0.0641(15) Uani 1 1 d . . .
H6A H 0.3086 -0.7764 0.1728 0.077 Uiso 1 1 calc R . .
C7 C 0.2206(3) -0.8732(4) 0.1531(4) 0.0671(15) Uani 1 1 d . . .
H7A H 0.2527 -0.9045 0.2190 0.081 Uiso 1 1 calc R . .
C8 C 0.2387(3) -0.6643(4) -0.0037(4) 0.0580(14) Uani 1 1 d . . .
C9 C 0.3351(3) -0.6409(4) 0.0505(5) 0.0634(15) Uani 1 1 d . . .
H9A H 0.3550 -0.6501 0.1322 0.076 Uiso 1 1 calc R . .
H9B H 0.3677 -0.6807 0.0208 0.076 Uiso 1 1 calc R . .
C10 C 0.3820(3) -0.5192(4) -0.0546(4) 0.0549(14) Uani 1 1 d . . .
C11 C 0.4110(3) -0.5660(4) -0.1300(5) 0.0704(16) Uani 1 1 d . . .
H11A H 0.4128 -0.6283 -0.1327 0.084 Uiso 1 1 calc R . .
C12 C 0.4371(4) -0.5106(7) -0.2005(5) 0.088(2) Uani 1 1 d . . .
H12A H 0.4575 -0.5371 -0.2523 0.105 Uiso 1 1 calc R . .
C13 C 0.4339(4) -0.4167(6) -0.1967(6) 0.091(2) Uani 1 1 d . . .
H13A H 0.4503 -0.3833 -0.2475 0.110 Uiso 1 1 calc R . .
C14 C 0.4078(3) -0.3737(5) -0.1219(5) 0.0697(16) Uani 1 1 d . . .
H14A H 0.4072 -0.3115 -0.1182 0.084 Uiso 1 1 calc R . .
C15 C 0.3818(3) -0.4261(4) -0.0507(4) 0.0535(13) Uani 1 1 d . . .
C16 C 0.3345(3) -0.4769(4) 0.0791(4) 0.0511(13) Uani 1 1 d . . .
C17 C 0.2986(4) -0.4801(4) 0.1698(5) 0.0816(18) Uani 1 1 d . . .
H17A H 0.2919 -0.4202 0.1930 0.122 Uiso 1 1 calc R . .
H17B H 0.3375 -0.5128 0.2340 0.122 Uiso 1 1 calc R . .
H17C H 0.2432 -0.5094 0.1414 0.122 Uiso 1 1 calc R . .
C18 C 0.3452(3) -0.3106(3) 0.0670(5) 0.0610(14) Uani 1 1 d . . .
H18A H 0.3954 -0.2764 0.0691 0.073 Uiso 1 1 calc R . .
H18B H 0.3430 -0.3094 0.1425 0.073 Uiso 1 1 calc R . .
C19 C 0.2623(3) -0.2677(4) -0.0189(5) 0.0614(14) Uani 1 1 d . . .
C20 C 0.2708(3) -0.1737(3) -0.0334(5) 0.0602(14) Uani 1 1 d . . .
H20A H 0.3230 -0.1484 0.0140 0.072 Uiso 1 1 calc R . .
C21 C 0.2130(3) -0.1153(3) -0.1070(4) 0.0488(12) Uani 1 1 d . . .
C22 C 0.1211(3) -0.1307(3) -0.1932(4) 0.0537(13) Uani 1 1 d . . .
C23 C 0.0598(3) -0.1578(4) -0.1343(5) 0.0733(17) Uani 1 1 d . . .
H23A H 0.0624 -0.1139 -0.0775 0.110 Uiso 1 1 calc R . .
H23B H 0.0769 -0.2152 -0.0985 0.110 Uiso 1 1 calc R . .
H23C H 0.0016 -0.1613 -0.1896 0.110 Uiso 1 1 calc R . .
C24 C 0.1199(4) -0.1985(4) -0.2844(5) 0.0728(17) Uani 1 1 d . . .
H24A H 0.1592 -0.1794 -0.3196 0.109 Uiso 1 1 calc R . .
H24B H 0.0623 -0.2025 -0.3411 0.109 Uiso 1 1 calc R . .
H24C H 0.1375 -0.2561 -0.2498 0.109 Uiso 1 1 calc R . .
C25 C 0.0989(3) -0.0386(3) -0.2451(4) 0.0556(13) Uani 1 1 d . . .
C26 C 0.0233(4) -0.0070(4) -0.3304(5) 0.0841(19) Uani 1 1 d . . .
H26A H -0.0246 -0.0170 -0.3055 0.101 Uiso 1 1 calc R . .
H26B H 0.0126 -0.0435 -0.3978 0.101 Uiso 1 1 calc R . .
C27 C 0.0212(5) 0.0831(5) -0.3628(6) 0.091(2) Uani 1 1 d . . .
H27A H -0.0291 0.1059 -0.4180 0.109 Uiso 1 1 calc R . .
C28 C 0.0911(5) 0.1386(5) -0.3151(6) 0.0834(19) Uani 1 1 d . . .
H28A H 0.0881 0.1976 -0.3400 0.100 Uiso 1 1 calc R . .
C29 C 0.1665(4) 0.1079(4) -0.2300(5) 0.0681(15) Uani 1 1 d . . .
H29A H 0.2145 0.1450 -0.1977 0.082 Uiso 1 1 calc R . .
C30 C 0.1673(3) 0.0199(4) -0.1954(4) 0.0546(13) Uani 1 1 d . . .
C31 C 0.3150(4) 0.0131(4) -0.0360(5) 0.0785(17) Uani 1 1 d . . .
H31A H 0.3501 -0.0317 0.0149 0.118 Uiso 1 1 calc R . .
H31B H 0.3029 0.0604 0.0075 0.118 Uiso 1 1 calc R . .
H31C H 0.3456 0.0372 -0.0808 0.118 Uiso 1 1 calc R . .
Br1 Br 0.55540(4) -0.18346(4) 0.12110(5) 0.0810(3) Uani 1 1 d . . .
O4 O 0.4836(6) -0.3259(6) 0.3256(7) 0.091(3) Uani 0.50 1 d P . .
C32 C 0.4681(9) -0.4226(15) 0.3777(13) 0.132(7) Uani 0.50 1 d P . .


_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
O1 C2 1.353(6) . ?
O1 C1 1.441(6) . ?
O2 C8 1.218(6) . ?
O3 C19 1.228(6) . ?
N1 C16 1.341(6) . ?
N1 C10 1.395(6) . ?
N1 C9 1.444(6) . ?
N2 C16 1.333(6) . ?
N2 C15 1.380(6) . ?
N2 C18 1.448(6) . ?
N3 C21 1.367(6) . ?
N3 C30 1.400(6) . ?
N3 C31 1.460(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C7 1.369(6) . ?
C2 C3 1.382(7) . ?
C3 C4 1.363(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.404(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.395(6) . ?
C5 C8 1.457(7) . ?
C6 C7 1.376(7) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.528(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.389(7) . ?
C10 C11 1.404(7) . ?
C11 C12 1.399(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.403(9) . ?
C12 H12A 0.9300 . ?
C13 C14 1.342(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.378(7) . ?
C14 H14A 0.9300 . ?
C16 C17 1.477(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.539(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.427(7) . ?
C20 C21 1.371(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.526(6) . ?
C22 C25 1.508(7) . ?
C22 C23 1.523(7) . ?
C22 C24 1.529(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C30 1.384(7) . ?
C25 C26 1.396(7) . ?
C26 C27 1.402(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.369(9) . ?
C27 H27A 0.9300 . ?
C28 C29 1.389(8) . ?
C28 H28A 0.9300 . ?
C29 C30 1.383(7) . ?
C29 H29A 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
O4 C32 1.65(2) . ?

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
C2 O1 C1 118.3(4) . . ?
C16 N1 C10 107.7(4) . . ?
C16 N1 C9 125.3(4) . . ?
C10 N1 C9 126.9(5) . . ?
C16 N2 C15 108.5(4) . . ?
C16 N2 C18 127.6(4) . . ?
C15 N2 C18 123.9(4) . . ?
C21 N3 C30 111.9(4) . . ?
C21 N3 C31 123.7(4) . . ?
C30 N3 C31 124.4(4) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C7 124.5(5) . . ?
O1 C2 C3 116.1(4) . . ?
C7 C2 C3 119.4(5) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C3 C4 C5 121.3(5) . . ?
C3 C4 H4A 119.4 . . ?
C5 C4 H4A 119.4 . . ?
C6 C5 C4 117.0(5) . . ?
C6 C5 C8 123.3(4) . . ?
C4 C5 C8 119.7(4) . . ?
C7 C6 C5 121.2(5) . . ?
C7 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
C2 C7 C6 120.6(5) . . ?
C2 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
O2 C8 C5 122.0(5) . . ?
O2 C8 C9 118.2(5) . . ?
C5 C8 C9 119.8(5) . . ?
N1 C9 C8 112.0(4) . . ?
N1 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C15 C10 N1 106.7(4) . . ?
C15 C10 C11 121.9(5) . . ?
N1 C10 C11 131.4(6) . . ?
C12 C11 C10 113.9(6) . . ?
C12 C11 H11A 123.1 . . ?
C10 C11 H11A 123.1 . . ?
C11 C12 C13 122.9(6) . . ?
C11 C12 H12A 118.5 . . ?
C13 C12 H12A 118.5 . . ?
C14 C13 C12 121.8(7) . . ?
C14 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
C13 C14 C15 116.9(7) . . ?
C13 C14 H14A 121.6 . . ?
C15 C14 H14A 121.6 . . ?
C14 C15 N2 130.5(6) . . ?
C14 C15 C10 122.5(6) . . ?
N2 C15 C10 107.0(4) . . ?
N2 C16 N1 110.1(4) . . ?
N2 C16 C17 125.3(5) . . ?
N1 C16 C17 124.5(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 110.5(4) . . ?
N2 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O3 C19 C20 128.7(5) . . ?
O3 C19 C18 118.0(5) . . ?
C20 C19 C18 113.3(4) . . ?
C21 C20 C19 129.3(5) . . ?
C21 C20 H20A 115.3 . . ?
C19 C20 H20A 115.3 . . ?
N3 C21 C20 121.1(4) . . ?
N3 C21 C22 108.4(4) . . ?
C20 C21 C22 130.5(5) . . ?
C25 C22 C23 110.8(4) . . ?
C25 C22 C21 101.0(4) . . ?
C23 C22 C21 111.3(4) . . ?
C25 C22 C24 110.0(4) . . ?
C23 C22 C24 111.7(4) . . ?
C21 C22 C24 111.5(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 119.1(5) . . ?
C30 C25 C22 110.5(4) . . ?
C26 C25 C22 130.3(5) . . ?
C25 C26 C27 117.8(6) . . ?
C25 C26 H26A 107.9 . . ?
C27 C26 H26A 107.9 . . ?
C25 C26 H26B 107.9 . . ?
C27 C26 H26B 107.9 . . ?
H26A C26 H26B 107.2 . . ?
C28 C27 C26 121.8(6) . . ?
C28 C27 H27A 119.1 . . ?
C26 C27 H27A 119.1 . . ?
C27 C28 C29 120.9(6) . . ?
C27 C28 H28A 119.6 . . ?
C29 C28 H28A 119.6 . . ?
C30 C29 C28 117.2(6) . . ?
C30 C29 H29A 121.4 . . ?
C28 C29 H29A 121.4 . . ?
C25 C30 C29 123.1(5) . . ?
C25 C30 N3 108.1(4) . . ?
C29 C30 N3 128.8(5) . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.061
