# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_lpf4
_database_code_depnum_ccdc_archive 'CCDC 1520157'
_audit_update_record             
;
2016-12-01 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H19 Br N2 O5 S'
_chemical_formula_weight         479.34

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   8.8208(3)
_cell_length_b                   12.8570(4)
_cell_length_c                   18.1141(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2054.30(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5745
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      26.92

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SAINT ver. 7.34; Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24921
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_av_sigmaI/netI    0.1589
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.39
_reflns_number_total             4619
_reflns_number_gt                2601
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEXII'
_computing_cell_refinement       'Bruker APEXII'
_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)+(0.0067P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(8)
_refine_ls_number_reflns         4619
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0608
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.001
_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
Br1 Br 0.02265(3) 0.80732(2) 0.815784(17) 0.06682(9) Uani 1 1 d . . .
S1 S 0.65768(7) 0.44753(5) 0.85168(4) 0.04307(19) Uani 1 1 d . . .
O1 O 0.81206(18) 0.42223(13) 0.86690(10) 0.0638(6) Uani 1 1 d . . .
O2 O 0.54663(19) 0.37022(10) 0.86656(9) 0.0584(6) Uani 1 1 d . . .
O3 O 0.1158(2) 0.60834(16) 0.52905(12) 0.0928(8) Uani 1 1 d . . .
H5B H 0.739(2) 0.4742(14) 0.6406(11) 0.042(6) Uiso 1 1 d . . .
O4 O 0.2077(3) 0.46590(17) 0.56151(14) 0.1323(10) Uani 1 1 d . . .
O5 O 0.70633(19) 0.50005(12) 0.60886(10) 0.0523(6) Uani 1 1 d . . .
N1 N 0.6376(2) 0.48093(13) 0.76252(10) 0.0384(6) Uani 1 1 d . . .
N2 N 0.2153(3) 0.55776(18) 0.55488(12) 0.0632(7) Uani 1 1 d . . .
C1 C 0.5908(2) 0.57548(16) 0.75675(12) 0.0318(7) Uani 1 1 d . . .
C2 C 0.5712(2) 0.63259(15) 0.82685(12) 0.0333(7) Uani 1 1 d . . .
C3 C 0.6055(3) 0.57012(16) 0.88629(13) 0.0369(7) Uani 1 1 d . . .
C4 C 0.5978(3) 0.60360(19) 0.95757(14) 0.0584(9) Uani 1 1 d . . .
H4A H 0.6235 0.5604 0.9968 0.070 Uiso 1 1 calc R . .
C5 C 0.5500(4) 0.70499(19) 0.96896(15) 0.0788(11) Uani 1 1 d . . .
H5A H 0.5408 0.7302 1.0169 0.095 Uiso 1 1 calc R . .
C6 C 0.5160(4) 0.76857(17) 0.91052(14) 0.0711(10) Uani 1 1 d . . .
H6A H 0.469(2) 0.8386(14) 0.9190(11) 0.052(6) Uiso 1 1 d . . .
C7 C 0.5237(3) 0.73378(16) 0.83863(13) 0.0509(8) Uani 1 1 d . . .
H7A H 0.4979 0.7769 0.7994 0.061 Uiso 1 1 calc R . .
C8 C 0.5507(2) 0.61967(14) 0.68263(13) 0.0310(6) Uani 1 1 d . . .
H8A H 0.5345(17) 0.6903(12) 0.6923(9) 0.024(4) Uiso 1 1 d . . .
C9 C 0.6773(3) 0.60799(17) 0.62487(14) 0.0409(7) Uani 1 1 d . . .
C10 C 0.6235(3) 0.65431(19) 0.55223(14) 0.0461(8) Uani 1 1 d . . .
H10B H 0.621(2) 0.7237(14) 0.5618(11) 0.040(6) Uiso 1 1 d . . .
H10A H 0.706(2) 0.6423(14) 0.5156(10) 0.036(6) Uiso 1 1 d . . .
C11 C 0.4793(3) 0.60524(18) 0.52498(13) 0.0502(8) Uani 1 1 d . . .
H11B H 0.4415(19) 0.6335(13) 0.4807(10) 0.030(6) Uiso 1 1 d . . .
H11A H 0.486(2) 0.5294(13) 0.5137(10) 0.034(5) Uiso 1 1 d . . .
C12 C 0.3550(3) 0.61388(17) 0.58285(14) 0.0421(7) Uani 1 1 d . . .
H12A H 0.3216(17) 0.6855(14) 0.5883(10) 0.027(5) Uiso 1 1 d . . .
C13 C 0.3992(2) 0.56767(16) 0.65755(13) 0.0346(7) Uani 1 1 d . . .
H13A H 0.4214(18) 0.4947(12) 0.6489(10) 0.025(5) Uiso 1 1 d . . .
C14 C 0.2797(2) 0.57712(16) 0.71623(13) 0.0361(7) Uani 1 1 d . . .
C15 C 0.2460(3) 0.49134(19) 0.75984(15) 0.0541(9) Uani 1 1 d . . .
H15A H 0.2900 0.4274 0.7491 0.065 Uiso 1 1 calc R . .
C16 C 0.1491(3) 0.4996(2) 0.81823(17) 0.0738(10) Uani 1 1 d . . .
H16A H 0.1267 0.4407 0.8460 0.089 Uiso 1 1 calc R . .
C17 C 0.0838(3) 0.5934(2) 0.83703(16) 0.0627(10) Uani 1 1 d . . .
H17A H 0.014(3) 0.5981(14) 0.8780(12) 0.059(7) Uiso 1 1 d . . .
C18 C 0.1160(2) 0.67733(18) 0.79284(14) 0.0437(8) Uani 1 1 d . . .
C19 C 0.2117(3) 0.67170(18) 0.73376(14) 0.0419(7) Uani 1 1 d . . .
H19A H 0.228(2) 0.7357(14) 0.6994(11) 0.044(6) Uiso 1 1 d . . .
C20 C 0.8231(2) 0.6608(2) 0.65135(15) 0.0636(9) Uani 1 1 d . . .
H20A H 0.7979 0.7182 0.6830 0.126(12) Uiso 1 1 calc R . .
H20B H 0.8791 0.6857 0.6095 0.151 Uiso 1 1 calc R . .
H20C H 0.8836 0.6116 0.6782 0.151 Uiso 1 1 calc R . .


_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
Br1 C18 1.909(2) . ?
S1 O2 1.4213(16) . ?
S1 O1 1.4270(17) . ?
S1 N1 1.6804(19) . ?
S1 C3 1.758(2) . ?
O3 N2 1.188(3) . ?
O4 N2 1.189(3) . ?
O5 C9 1.441(3) . ?
O5 H5B 0.726(19) . ?
N1 C1 1.288(3) . ?
N2 C12 1.515(3) . ?
C1 C2 1.477(3) . ?
C1 C8 1.500(3) . ?
C2 C3 1.377(3) . ?
C2 C7 1.383(3) . ?
C3 C4 1.363(3) . ?
C4 C5 1.386(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.371(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.379(3) . ?
C6 H6A 1.002(18) . ?
C7 H7A 0.9300 . ?
C8 C9 1.538(3) . ?
C8 C13 1.562(3) . ?
C8 H8A 0.936(15) . ?
C9 C10 1.520(3) . ?
C9 C20 1.531(3) . ?
C10 C11 1.503(4) . ?
C10 H10B 0.909(18) . ?
C10 H10A 1.000(18) . ?
C11 C12 1.521(3) . ?
C11 H11B 0.941(17) . ?
C11 H11A 0.998(16) . ?
C12 C13 1.528(3) . ?
C12 H12A 0.972(18) . ?
C13 C14 1.502(3) . ?
C13 H13A 0.972(16) . ?
C14 C15 1.389(3) . ?
C14 C19 1.393(3) . ?
C15 C16 1.364(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.378(3) . ?
C16 H16A 0.9300 . ?
C17 C18 1.374(3) . ?
C17 H17A 0.96(2) . ?
C18 C19 1.365(3) . ?
C19 H19A 1.041(19) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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
O2 S1 O1 117.49(10) . . ?
O2 S1 N1 106.77(10) . . ?
O1 S1 N1 110.14(10) . . ?
O2 S1 C3 112.26(10) . . ?
O1 S1 C3 112.68(11) . . ?
N1 S1 C3 94.94(10) . . ?
C9 O5 H5B 110.7(15) . . ?
C1 N1 S1 110.67(16) . . ?
O3 N2 O4 122.8(3) . . ?
O3 N2 C12 118.1(2) . . ?
O4 N2 C12 119.0(2) . . ?
N1 C1 C2 115.9(2) . . ?
N1 C1 C8 120.38(19) . . ?
C2 C1 C8 123.60(18) . . ?
C3 C2 C7 119.6(2) . . ?
C3 C2 C1 110.88(18) . . ?
C7 C2 C1 129.5(2) . . ?
C4 C3 C2 123.1(2) . . ?
C4 C3 S1 129.36(19) . . ?
C2 C3 S1 107.56(17) . . ?
C3 C4 C5 117.0(2) . . ?
C3 C4 H4A 121.5 . . ?
C5 C4 H4A 121.5 . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C5 C6 C7 121.7(2) . . ?
C5 C6 H6A 120.5(12) . . ?
C7 C6 H6A 117.2(12) . . ?
C6 C7 C2 117.8(2) . . ?
C6 C7 H7A 121.1 . . ?
C2 C7 H7A 121.1 . . ?
C1 C8 C9 113.60(17) . . ?
C1 C8 C13 107.48(17) . . ?
C9 C8 C13 112.45(19) . . ?
C1 C8 H8A 103.7(11) . . ?
C9 C8 H8A 109.4(10) . . ?
C13 C8 H8A 109.9(10) . . ?
O5 C9 C10 104.99(19) . . ?
O5 C9 C20 109.93(19) . . ?
C10 C9 C20 111.1(2) . . ?
O5 C9 C8 111.10(17) . . ?
C10 C9 C8 108.90(19) . . ?
C20 C9 C8 110.7(2) . . ?
C11 C10 C9 112.6(2) . . ?
C11 C10 H10B 116.9(13) . . ?
C9 C10 H10B 103.1(13) . . ?
C11 C10 H10A 109.7(11) . . ?
C9 C10 H10A 106.6(11) . . ?
H10B C10 H10A 107.3(16) . . ?
C10 C11 C12 110.7(2) . . ?
C10 C11 H11B 114.7(11) . . ?
C12 C11 H11B 107.7(11) . . ?
C10 C11 H11A 115.1(11) . . ?
C12 C11 H11A 104.9(11) . . ?
H11B C11 H11A 103.1(15) . . ?
N2 C12 C11 108.7(2) . . ?
N2 C12 C13 108.56(19) . . ?
C11 C12 C13 113.45(19) . . ?
N2 C12 H12A 103.8(10) . . ?
C11 C12 H12A 111.0(10) . . ?
C13 C12 H12A 110.8(11) . . ?
C14 C13 C12 114.60(18) . . ?
C14 C13 C8 111.10(18) . . ?
C12 C13 C8 108.02(18) . . ?
C14 C13 H13A 109.5(10) . . ?
C12 C13 H13A 106.6(11) . . ?
C8 C13 H13A 106.7(10) . . ?
C15 C14 C19 118.1(2) . . ?
C15 C14 C13 119.3(2) . . ?
C19 C14 C13 122.3(2) . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15A 119.6 . . ?
C14 C15 H15A 119.6 . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.3 . . ?
C18 C17 C16 117.2(3) . . ?
C18 C17 H17A 122.0(12) . . ?
C16 C17 H17A 120.7(12) . . ?
C19 C18 C17 122.9(2) . . ?
C19 C18 Br1 118.94(18) . . ?
C17 C18 Br1 118.19(18) . . ?
C18 C19 C14 119.4(2) . . ?
C18 C19 H19A 120.8(11) . . ?
C14 C19 H19A 119.6(11) . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 N1 C1 113.18(16) . . . . ?
O1 S1 N1 C1 -118.21(16) . . . . ?
C3 S1 N1 C1 -1.85(18) . . . . ?
S1 N1 C1 C2 2.0(2) . . . . ?
S1 N1 C1 C8 -174.28(15) . . . . ?
N1 C1 C2 C3 -1.2(3) . . . . ?
C8 C1 C2 C3 175.02(19) . . . . ?
N1 C1 C2 C7 179.8(2) . . . . ?
C8 C1 C2 C7 -4.1(4) . . . . ?
C7 C2 C3 C4 -1.3(4) . . . . ?
C1 C2 C3 C4 179.6(2) . . . . ?
C7 C2 C3 S1 178.93(18) . . . . ?
C1 C2 C3 S1 -0.3(2) . . . . ?
O2 S1 C3 C4 71.0(3) . . . . ?
O1 S1 C3 C4 -64.4(3) . . . . ?
N1 S1 C3 C4 -178.6(2) . . . . ?
O2 S1 C3 C2 -109.23(17) . . . . ?
O1 S1 C3 C2 115.40(17) . . . . ?
N1 S1 C3 C2 1.16(17) . . . . ?
C2 C3 C4 C5 1.3(4) . . . . ?
S1 C3 C4 C5 -178.9(2) . . . . ?
C3 C4 C5 C6 -1.6(4) . . . . ?
C4 C5 C6 C7 1.9(5) . . . . ?
C5 C6 C7 C2 -1.7(5) . . . . ?
C3 C2 C7 C6 1.4(4) . . . . ?
C1 C2 C7 C6 -179.6(3) . . . . ?
N1 C1 C8 C9 -53.3(3) . . . . ?
C2 C1 C8 C9 130.7(2) . . . . ?
N1 C1 C8 C13 71.7(2) . . . . ?
C2 C1 C8 C13 -104.3(2) . . . . ?
C1 C8 C9 O5 64.3(2) . . . . ?
C13 C8 C9 O5 -58.1(2) . . . . ?
C1 C8 C9 C10 179.46(18) . . . . ?
C13 C8 C9 C10 57.1(2) . . . . ?
C1 C8 C9 C20 -58.1(2) . . . . ?
C13 C8 C9 C20 179.51(18) . . . . ?
O5 C9 C10 C11 62.0(2) . . . . ?
C20 C9 C10 C11 -179.3(2) . . . . ?
C8 C9 C10 C11 -57.1(2) . . . . ?
C9 C10 C11 C12 56.4(3) . . . . ?
O3 N2 C12 C11 -100.3(3) . . . . ?
O4 N2 C12 C11 81.8(3) . . . . ?
O3 N2 C12 C13 135.8(2) . . . . ?
O4 N2 C12 C13 -42.0(3) . . . . ?
C10 C11 C12 N2 -176.58(19) . . . . ?
C10 C11 C12 C13 -55.7(3) . . . . ?
N2 C12 C13 C14 -60.2(2) . . . . ?
C11 C12 C13 C14 178.79(18) . . . . ?
N2 C12 C13 C8 175.35(17) . . . . ?
C11 C12 C13 C8 54.4(2) . . . . ?
C1 C8 C13 C14 52.2(2) . . . . ?
C9 C8 C13 C14 177.97(17) . . . . ?
C1 C8 C13 C12 178.71(18) . . . . ?
C9 C8 C13 C12 -55.5(2) . . . . ?
C12 C13 C14 C15 134.3(2) . . . . ?
C8 C13 C14 C15 -102.9(2) . . . . ?
C12 C13 C14 C19 -52.3(3) . . . . ?
C8 C13 C14 C19 70.5(3) . . . . ?
C19 C14 C15 C16 -0.1(4) . . . . ?
C13 C14 C15 C16 173.5(2) . . . . ?
C14 C15 C16 C17 -1.4(4) . . . . ?
C15 C16 C17 C18 2.3(4) . . . . ?
C16 C17 C18 C19 -2.0(4) . . . . ?
C16 C17 C18 Br1 178.2(2) . . . . ?
C17 C18 C19 C14 0.6(4) . . . . ?
Br1 C18 C19 C14 -179.62(17) . . . . ?
C15 C14 C19 C18 0.5(3) . . . . ?
C13 C14 C19 C18 -173.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.060

