# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2009
data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Mercedes Alvarez'
_publ_contact_author_email       MERCEDES.ALVAREZ@IRBBARCELONA.ORG

_publ_section_title              
;
Synthesis of the Pyrrolo[2,3-c]carbazole Core of the
Dictyodendrins
;
loop_
_publ_author_name
'Mercedes Alvarez'
'Fernando Albericio'
'Carles Ayats'
'Roger Soley'

data_camm66a
_database_code_depnum_ccdc_archive 'CCDC 704582'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'0.9(C25 H22 Br1 N O4 S) 0.1(C25 H21 Br2 N O4 S)'
_chemical_formula_sum            'C25 H21.90 Br1.10 N O4 S'
_chemical_formula_weight         520.30

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   11.180(7)
_cell_length_b                   17.516(8)
_cell_length_c                   13.175(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.18(3)
_cell_angle_gamma                90.00
_cell_volume                     2389(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1922
_cell_measurement_theta_min      24298
_cell_measurement_theta_max      7455

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1062
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24156
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         32.33
_reflns_number_total             7270
_reflns_number_gt                3503
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MARXDS
_computing_cell_refinement       AUTOMAR
_computing_data_reduction        MARSCALE
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'

_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^)+(0.0874P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0104(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         7270
_refine_ls_number_parameters     299
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1857
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.016
_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 0.38292(4) 0.15841(2) 0.51666(3) 0.09380(19) Uani 1 1 d . . .
Br2 Br 0.2255(3) 0.38442(18) 0.6109(2) 0.0753(7) Uani 0.10 1 d P . .
S S 0.26669(9) 0.39503(5) 0.21294(7) 0.0864(3) Uani 1 1 d . . .
O1 O 0.2703(2) 0.31309(15) 0.21898(19) 0.0936(6) Uani 1 1 d . . .
O2 O 0.1704(3) 0.43169(16) 0.1228(2) 0.1058(8) Uani 1 1 d . . .
O3 O 0.4583(2) 0.31157(15) 0.4616(2) 0.0955(6) Uani 1 1 d U . .
O4 O -0.2616(2) 0.21587(16) 0.3511(2) 0.1059(7) Uani 1 1 d . . .
N1 N 0.2484(3) 0.42620(15) 0.3257(2) 0.0845(7) Uani 1 1 d . . .
C1 C 0.4168(4) 0.4278(2) 0.2202(3) 0.0890(9) Uani 1 1 d . . .
C2 C 0.5253(4) 0.3818(2) 0.2661(3) 0.0915(9) Uani 1 1 d . . .
H2 H 0.5185 0.3356 0.2981 0.110 Uiso 1 1 calc R . .
C3 C 0.6428(4) 0.4042(2) 0.2645(3) 0.1024(11) Uani 1 1 d . . .
H3 H 0.7148 0.3730 0.2955 0.123 Uiso 1 1 calc R . .
C4 C 0.6540(5) 0.4732(3) 0.2164(4) 0.1120(12) Uani 1 1 d U . .
C5 C 0.5450(6) 0.5192(3) 0.1709(5) 0.1498(19) Uani 1 1 d U . .
H5 H 0.5512 0.5658 0.1394 0.180 Uiso 1 1 calc R . .
C6 C 0.4278(5) 0.4957(3) 0.1725(4) 0.1176(13) Uani 1 1 d . . .
H6 H 0.3553 0.5263 0.1407 0.141 Uiso 1 1 calc R . .
C7 C 0.7827(6) 0.4965(4) 0.2105(5) 0.156(2) Uani 1 1 d . . .
H7A H 0.7736 0.5452 0.1749 0.235 Uiso 1 1 calc R . .
H7B H 0.8084 0.4590 0.1695 0.235 Uiso 1 1 calc R . .
H7C H 0.8473 0.4999 0.2833 0.235 Uiso 1 1 calc R . .
C8 C 0.1919(3) 0.4969(2) 0.3338(3) 0.0844(8) Uani 1 1 d . . .
C9 C 0.1621(4) 0.5610(2) 0.2662(4) 0.1020(11) Uani 1 1 d . . .
H9 H 0.1780 0.5617 0.2019 0.122 Uiso 1 1 calc R . .
C10 C 0.1084(5) 0.6236(3) 0.2966(5) 0.1279(16) Uani 1 1 d . . .
H10 H 0.0879 0.6669 0.2525 0.154 Uiso 1 1 calc R . .
C11 C 0.0848(5) 0.6223(3) 0.3926(5) 0.1315(17) Uani 1 1 d . . .
H11 H 0.0482 0.6650 0.4113 0.158 Uiso 1 1 calc R . .
C12 C 0.1142(4) 0.5593(3) 0.4617(4) 0.1182(14) Uani 1 1 d . . .
H12 H 0.0977 0.5592 0.5259 0.142 Uiso 1 1 calc R . .
C13 C 0.1689(3) 0.4964(2) 0.4318(3) 0.0913(9) Uani 1 1 d . . .
C14 C 0.2132(3) 0.4244(2) 0.4829(3) 0.0918(9) Uani 1 1 d U . .
H14 H 0.2102 0.4087 0.5493 0.110 Uiso 0.90 1 calc PR . .
C15 C 0.2604(3) 0.38225(19) 0.4194(3) 0.0797(7) Uani 1 1 d U . .
C16 C 0.3297(3) 0.3098(2) 0.4483(2) 0.0793(7) Uani 1 1 d U . .
C17 C 0.5375(5) 0.3652(3) 0.5410(4) 0.1268(15) Uani 1 1 d . . .
H17A H 0.6245 0.3625 0.5439 0.190 Uiso 1 1 calc R . .
H17B H 0.5365 0.3531 0.6118 0.190 Uiso 1 1 calc R . .
H17C H 0.5044 0.4158 0.5205 0.190 Uiso 1 1 calc R . .
C18 C 0.2754(3) 0.24514(19) 0.4611(2) 0.0791(8) Uani 1 1 d . . .
C19 C 0.1344(3) 0.23324(18) 0.4317(3) 0.0789(8) Uani 1 1 d . . .
C20 C 0.0457(3) 0.2544(2) 0.3288(3) 0.0878(9) Uani 1 1 d . . .
H20 H 0.0751 0.2737 0.2765 0.105 Uiso 1 1 calc R . .
C21 C -0.0844(3) 0.2471(2) 0.3040(3) 0.0884(9) Uani 1 1 d . . .
H21 H -0.1425 0.2613 0.2350 0.106 Uiso 1 1 calc R . .
C22 C -0.1304(3) 0.2188(2) 0.3814(3) 0.0844(8) Uani 1 1 d . . .
C23 C -0.0432(3) 0.19634(19) 0.4831(2) 0.0799(8) Uani 1 1 d . . .
H23 H -0.0728 0.1768 0.5350 0.096 Uiso 1 1 calc R . .
C24 C 0.0879(3) 0.2031(2) 0.5075(3) 0.0872(9) Uani 1 1 d . . .
H24 H 0.1460 0.1873 0.5756 0.105 Uiso 1 1 calc R . .
C25 C -0.3119(4) 0.1928(3) 0.4334(4) 0.1243(14) Uani 1 1 d . . .
H25A H -0.4046 0.1933 0.4019 0.186 Uiso 1 1 calc R . .
H25B H -0.2821 0.2277 0.4941 0.186 Uiso 1 1 calc R . .
H25C H -0.2822 0.1423 0.4587 0.186 Uiso 1 1 calc R . .

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
Br1 0.0921(3) 0.0902(3) 0.0956(3) 0.00650(16) 0.0314(2) 0.00963(16)
Br2 0.0824(17) 0.0724(17) 0.0734(15) -0.0091(12) 0.0318(13) 0.0032(13)
S 0.0885(5) 0.0801(5) 0.0854(5) -0.0020(4) 0.0268(4) -0.0035(4)
O1 0.0999(16) 0.0828(15) 0.0969(15) -0.0064(12) 0.0359(13) -0.0091(13)
O2 0.1045(17) 0.1062(18) 0.0936(15) 0.0038(13) 0.0226(13) 0.0022(14)
O3 0.0809(11) 0.0955(16) 0.1069(16) 0.0022(13) 0.0316(12) 0.0019(12)
O4 0.0881(15) 0.116(2) 0.1082(17) 0.0059(15) 0.0311(13) -0.0040(14)
N1 0.0887(17) 0.0751(16) 0.0876(15) 0.0012(13) 0.0310(13) 0.0055(13)
C1 0.095(2) 0.083(2) 0.0875(18) 0.0015(16) 0.0321(17) -0.0043(18)
C2 0.096(2) 0.089(2) 0.090(2) 0.0029(17) 0.0373(18) -0.0019(19)
C3 0.105(3) 0.102(3) 0.098(2) -0.002(2) 0.035(2) -0.007(2)
C4 0.115(3) 0.110(3) 0.113(3) -0.009(2) 0.045(2) -0.020(2)
C5 0.141(4) 0.123(4) 0.188(5) 0.028(4) 0.065(4) 0.000(3)
C6 0.118(3) 0.101(3) 0.136(3) 0.014(3) 0.050(3) 0.002(3)
C7 0.148(5) 0.165(5) 0.172(5) 0.000(4) 0.078(4) -0.028(4)
C8 0.0778(18) 0.078(2) 0.088(2) -0.0014(15) 0.0211(15) 0.0014(15)
C9 0.102(3) 0.086(2) 0.108(2) 0.0047(19) 0.029(2) 0.007(2)
C10 0.128(4) 0.096(3) 0.141(4) -0.008(3) 0.029(3) 0.010(3)
C11 0.117(3) 0.107(4) 0.155(5) -0.021(3) 0.034(3) 0.005(3)
C12 0.115(3) 0.102(3) 0.130(3) -0.019(3) 0.036(3) 0.004(2)
C13 0.084(2) 0.087(2) 0.095(2) -0.0080(17) 0.0242(17) -0.0027(17)
C14 0.088(2) 0.091(2) 0.091(2) -0.0067(16) 0.0283(16) 0.0014(17)
C15 0.0752(18) 0.0752(19) 0.0802(17) -0.0014(13) 0.0197(13) -0.0026(14)
C16 0.0752(12) 0.0791(18) 0.0755(16) -0.0017(14) 0.0195(14) -0.0020(15)
C17 0.108(3) 0.139(4) 0.125(3) -0.010(3) 0.034(3) -0.018(3)
C18 0.0738(16) 0.084(2) 0.0753(15) 0.0021(14) 0.0235(14) 0.0011(15)
C19 0.0749(17) 0.0748(19) 0.0822(17) -0.0008(14) 0.0243(14) -0.0023(14)
C20 0.0817(19) 0.094(2) 0.0830(18) 0.0078(16) 0.0256(15) -0.0007(16)
C21 0.0784(19) 0.099(2) 0.0790(18) 0.0033(16) 0.0192(15) 0.0058(17)
C22 0.0797(19) 0.085(2) 0.0849(19) -0.0017(16) 0.0268(16) -0.0043(15)
C23 0.0797(18) 0.083(2) 0.0744(16) 0.0015(14) 0.0255(14) -0.0052(15)
C24 0.084(2) 0.087(2) 0.0850(19) 0.0043(16) 0.0254(16) -0.0011(16)
C25 0.101(3) 0.143(4) 0.131(3) -0.001(3) 0.047(3) -0.009(3)

_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 1.904(3) . ?
Br2 C14 1.783(5) . ?
S O2 1.420(3) . ?
S O1 1.437(3) . ?
S N1 1.666(3) . ?
S C1 1.742(4) . ?
O3 C16 1.381(4) . ?
O3 C17 1.436(5) . ?
O4 C22 1.368(4) . ?
O4 C25 1.455(5) . ?
N1 C8 1.412(4) . ?
N1 C15 1.418(4) . ?
C1 C6 1.372(6) . ?
C1 C2 1.390(5) . ?
C2 C3 1.378(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(7) . ?
C4 C7 1.525(7) . ?
C5 C6 1.381(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.393(5) . ?
C8 C13 1.408(5) . ?
C9 C10 1.379(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.428(5) . ?
C14 C15 1.362(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.460(5) . ?
C16 C18 1.326(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.489(5) . ?
C19 C24 1.391(5) . ?
C19 C20 1.394(5) . ?
C20 C21 1.371(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.395(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.383(4) . ?
C23 C24 1.383(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 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 S O1 119.64(15) . . ?
O2 S N1 106.72(17) . . ?
O1 S N1 106.76(15) . . ?
O2 S C1 107.91(18) . . ?
O1 S C1 108.64(16) . . ?
N1 S C1 106.45(16) . . ?
C16 O3 C17 115.6(3) . . ?
C22 O4 C25 117.8(3) . . ?
C8 N1 C15 108.0(3) . . ?
C8 N1 S 124.3(2) . . ?
C15 N1 S 126.5(2) . . ?
C6 C1 C2 119.2(4) . . ?
C6 C1 S 120.8(3) . . ?
C2 C1 S 119.8(3) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 C7 120.3(5) . . ?
C5 C4 C7 120.8(5) . . ?
C6 C5 C4 120.1(5) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C1 C6 C5 121.0(5) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 120.5(4) . . ?
C9 C8 N1 131.7(4) . . ?
C13 C8 N1 107.8(3) . . ?
C10 C9 C8 118.7(5) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 120.3(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 122.2(5) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 117.6(5) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
C12 C13 C8 120.6(4) . . ?
C12 C13 C14 132.7(4) . . ?
C8 C13 C14 106.7(3) . . ?
C15 C14 C13 109.6(3) . . ?
C15 C14 Br2 117.3(3) . . ?
C13 C14 Br2 133.0(3) . . ?
C15 C14 H14 125.2 . . ?
C13 C14 H14 125.2 . . ?
Br2 C14 H14 8.4 . . ?
C14 C15 N1 108.0(3) . . ?
C14 C15 C16 127.0(3) . . ?
N1 C15 C16 124.4(3) . . ?
C18 C16 O3 120.5(3) . . ?
C18 C16 C15 123.5(3) . . ?
O3 C16 C15 116.0(3) . . ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 C19 125.3(3) . . ?
C16 C18 Br1 118.5(2) . . ?
C19 C18 Br1 116.2(2) . . ?
C24 C19 C20 118.6(3) . . ?
C24 C19 C18 120.8(3) . . ?
C20 C19 C18 120.6(3) . . ?
C21 C20 C19 120.5(3) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 120.7(3) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
O4 C22 C23 123.9(3) . . ?
O4 C22 C21 116.8(3) . . ?
C23 C22 C21 119.3(3) . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C19 121.1(3) . . ?
C23 C24 H24 119.5 . . ?
C19 C24 H24 119.5 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.852
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.061