# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 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_160719h
_database_code_depnum_ccdc_archive 'CCDC 1526668'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H13 Cl O2'
_chemical_formula_weight         308.74

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   9.8188(9)
_cell_length_b                   12.2691(11)
_cell_length_c                   13.2128(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.004(2)
_cell_angle_gamma                90.00
_cell_volume                     1513.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1793
_cell_measurement_theta_min      2.742
_cell_measurement_theta_max      24.691

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8978
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_process_details   sadabs

_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  '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            7452
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2672
_reflns_number_gt                1595
_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)+(0.0515P)²+0.4509P] 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         2672
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1270
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Cl1 Cl 0.11251(10) 0.67441(7) 1.11747(8) 0.0954(4) Uani 1 1 d . . .
O1 O 0.5153(2) 0.17132(18) 0.82867(16) 0.0712(6) Uani 1 1 d . . .
O2 O 0.51030(19) 0.19962(13) 1.06028(14) 0.0537(5) Uani 1 1 d . . .
C1 C 0.5029(3) 0.2654(3) 0.8039(2) 0.0594(8) Uani 1 1 d . . .
H1 H 0.5420 0.2880 0.7516 0.071 Uiso 1 1 calc R . .
C2 C 0.4305(3) 0.3487(2) 0.84947(18) 0.0438(6) Uani 1 1 d . . .
C3 C 0.3777(2) 0.32369(18) 0.93246(18) 0.0379(6) Uani 1 1 d . . .
C4 C 0.3102(2) 0.40555(18) 0.97563(18) 0.0390(6) Uani 1 1 d . . .
C5 C 0.2566(3) 0.3858(2) 1.0617(2) 0.0502(7) Uani 1 1 d . . .
H5 H 0.2622 0.3159 1.0900 0.060 Uiso 1 1 calc R . .
C6 C 0.1970(3) 0.4669(2) 1.1037(2) 0.0608(8) Uani 1 1 d . . .
H6 H 0.1636 0.4528 1.1610 0.073 Uiso 1 1 calc R . .
C7 C 0.1860(3) 0.5716(2) 1.0606(2) 0.0589(8) Uani 1 1 d . . .
C8 C 0.2346(3) 0.5954(2) 0.9782(2) 0.0542(7) Uani 1 1 d . . .
H8 H 0.2261 0.6659 0.9512 0.065 Uiso 1 1 calc R . .
C9 C 0.2983(3) 0.51290(19) 0.93290(19) 0.0430(6) Uani 1 1 d . . .
C10 C 0.3544(3) 0.5357(2) 0.8487(2) 0.0506(7) Uani 1 1 d . . .
H10 H 0.3477 0.6057 0.8206 0.061 Uiso 1 1 calc R . .
C11 C 0.4178(3) 0.4555(2) 0.8088(2) 0.0511(7) Uani 1 1 d . . .
H11 H 0.4539 0.4715 0.7531 0.061 Uiso 1 1 calc R . .
C12 C 0.4020(3) 0.21286(18) 0.98532(19) 0.0405(6) Uani 1 1 d . . .
C13 C 0.2903(3) 0.12811(18) 0.95062(18) 0.0390(6) Uani 1 1 d . . .
C14 C 0.1611(3) 0.1474(2) 0.8729(2) 0.0486(7) Uani 1 1 d . . .
H14 H 0.1443 0.2150 0.8394 0.058 Uiso 1 1 calc R . .
C15 C 0.0569(3) 0.0680(2) 0.8443(2) 0.0546(7) Uani 1 1 d . . .
H15 H -0.0297 0.0832 0.7926 0.065 Uiso 1 1 calc R . .
C16 C 0.0791(3) -0.0338(2) 0.8912(2) 0.0500(7) Uani 1 1 d . . .
C17 C 0.2083(3) -0.0530(2) 0.9682(2) 0.0556(7) Uani 1 1 d . . .
H17 H 0.2250 -0.1209 1.0010 0.067 Uiso 1 1 calc R . .
C18 C 0.3132(3) 0.02566(19) 0.9980(2) 0.0493(7) Uani 1 1 d . . .
H18 H 0.3996 0.0102 1.0498 0.059 Uiso 1 1 calc R . .
C19 C -0.0345(3) -0.1208(2) 0.8606(3) 0.0715(9) Uani 1 1 d . . .
H19A H -0.0939 -0.1163 0.9061 0.107 Uiso 1 1 calc R . .
H19B H 0.0102 -0.1912 0.8682 0.107 Uiso 1 1 calc R . .
H19C H -0.0921 -0.1104 0.7879 0.107 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
Cl1 C7 1.736(3) . ?
O1 C1 1.196(3) . ?
O2 C12 1.220(3) . ?
C1 C2 1.474(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.385(3) . ?
C2 C11 1.407(3) . ?
C3 C4 1.417(3) . ?
C3 C12 1.514(3) . ?
C4 C5 1.414(3) . ?
C4 C9 1.424(3) . ?
C5 C6 1.357(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.395(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.349(4) . ?
C8 C9 1.417(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.413(3) . ?
C10 C11 1.355(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.477(3) . ?
C13 C14 1.384(3) . ?
C13 C18 1.391(3) . ?
C14 C15 1.378(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(4) . ?
C16 C19 1.506(4) . ?
C17 C18 1.377(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 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
O1 C1 C2 125.3(3) . . ?
O1 C1 H1 117.3 . . ?
C2 C1 H1 117.3 . . ?
C3 C2 C11 119.9(2) . . ?
C3 C2 C1 121.0(2) . . ?
C11 C2 C1 119.1(2) . . ?
C2 C3 C4 119.9(2) . . ?
C2 C3 C12 121.3(2) . . ?
C4 C3 C12 118.54(19) . . ?
C5 C4 C3 122.6(2) . . ?
C5 C4 C9 118.2(2) . . ?
C3 C4 C9 119.2(2) . . ?
C6 C5 C4 121.2(2) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C8 C7 C6 121.8(3) . . ?
C8 C7 Cl1 119.3(2) . . ?
C6 C7 Cl1 118.9(2) . . ?
C7 C8 C9 119.9(2) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 121.5(2) . . ?
C10 C9 C4 119.4(2) . . ?
C8 C9 C4 119.1(2) . . ?
C11 C10 C9 120.1(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C2 121.6(2) . . ?
C10 C11 H11 119.2 . . ?
C2 C11 H11 119.2 . . ?
O2 C12 C13 122.4(2) . . ?
O2 C12 C3 117.9(2) . . ?
C13 C12 C3 119.6(2) . . ?
C14 C13 C18 118.2(2) . . ?
C14 C13 C12 122.1(2) . . ?
C18 C13 C12 119.7(2) . . ?
C15 C14 C13 121.0(2) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 121.0(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C17 C16 C15 117.9(2) . . ?
C17 C16 C19 120.9(3) . . ?
C15 C16 C19 121.3(3) . . ?
C18 C17 C16 121.8(2) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C13 120.1(2) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
O1 C1 C2 C3 4.3(4) . . . . ?
O1 C1 C2 C11 -176.9(3) . . . . ?
C11 C2 C3 C4 0.4(3) . . . . ?
C1 C2 C3 C4 179.2(2) . . . . ?
C11 C2 C3 C12 -174.0(2) . . . . ?
C1 C2 C3 C12 4.8(4) . . . . ?
C2 C3 C4 C5 -178.7(2) . . . . ?
C12 C3 C4 C5 -4.2(3) . . . . ?
C2 C3 C4 C9 -0.3(3) . . . . ?
C12 C3 C4 C9 174.3(2) . . . . ?
C3 C4 C5 C6 177.6(2) . . . . ?
C9 C4 C5 C6 -0.9(4) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C5 C6 C7 C8 -0.7(5) . . . . ?
C5 C6 C7 Cl1 -178.8(2) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
Cl1 C7 C8 C9 178.3(2) . . . . ?
C7 C8 C9 C10 -178.0(2) . . . . ?
C7 C8 C9 C4 0.0(4) . . . . ?
C5 C4 C9 C10 178.4(2) . . . . ?
C3 C4 C9 C10 -0.2(3) . . . . ?
C5 C4 C9 C8 0.4(3) . . . . ?
C3 C4 C9 C8 -178.2(2) . . . . ?
C8 C9 C10 C11 178.4(2) . . . . ?
C4 C9 C10 C11 0.5(4) . . . . ?
C9 C10 C11 C2 -0.3(4) . . . . ?
C3 C2 C11 C10 -0.2(4) . . . . ?
C1 C2 C11 C10 -179.0(2) . . . . ?
C2 C3 C12 O2 88.7(3) . . . . ?
C4 C3 C12 O2 -85.8(3) . . . . ?
C2 C3 C12 C13 -96.0(3) . . . . ?
C4 C3 C12 C13 89.5(3) . . . . ?
O2 C12 C13 C14 173.1(2) . . . . ?
C3 C12 C13 C14 -1.9(3) . . . . ?
O2 C12 C13 C18 -5.9(3) . . . . ?
C3 C12 C13 C18 179.0(2) . . . . ?
C18 C13 C14 C15 1.1(4) . . . . ?
C12 C13 C14 C15 -178.0(2) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C14 C15 C16 C17 0.7(4) . . . . ?
C14 C15 C16 C19 179.8(2) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C19 C16 C17 C18 -179.6(2) . . . . ?
C16 C17 C18 C13 0.5(4) . . . . ?
C14 C13 C18 C17 -0.8(4) . . . . ?
C12 C13 C18 C17 178.2(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.041
####################################################################### 
# 
# 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_161126a
_database_code_depnum_ccdc_archive 'CCDC 1526669'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 Cl N O'
_chemical_formula_weight         425.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   26.22(3)
_cell_length_b                   6.695(7)
_cell_length_c                   28.76(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.874(16)
_cell_angle_gamma                90.00
_cell_volume                     4542(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1085
_cell_measurement_theta_min      2.858
_cell_measurement_theta_max      28.242

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9389
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_process_details   sadabs

_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  '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            11117
_diffrn_reflns_av_R_equivalents  0.1491
_diffrn_reflns_av_sigmaI/netI    0.1341
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3981
_reflns_number_gt                1586
_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)+(0.0642P)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         3981
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2084
_refine_ls_R_factor_gt           0.0983
_refine_ls_wR_factor_ref         0.2182
_refine_ls_wR_factor_gt          0.1883
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Cl1 Cl 0.49034(7) 0.5594(3) 0.18196(8) 0.1296(8) Uani 1 1 d . . .
N1 N 0.15386(17) 0.2393(7) 0.02150(14) 0.0568(11) Uani 1 1 d . . .
O1 O 0.15658(16) -0.0840(6) -0.00709(14) 0.0804(12) Uani 1 1 d . . .
C1 C 0.1808(2) 0.0669(9) 0.0183(2) 0.0605(14) Uani 1 1 d . . .
C2 C 0.2410(2) 0.0938(8) 0.04925(18) 0.0553(13) Uani 1 1 d . . .
C3 C 0.2515(2) 0.2800(8) 0.07216(17) 0.0507(13) Uani 1 1 d . . .
C4 C 0.1959(2) 0.3874(7) 0.05686(17) 0.0533(13) Uani 1 1 d . . .
H4 H 0.1953 0.5083 0.0374 0.064 Uiso 1 1 calc R . .
C5 C 0.2851(3) -0.0346(8) 0.05504(19) 0.0634(15) Uani 1 1 d . . .
H5 H 0.2773 -0.1608 0.0401 0.076 Uiso 1 1 calc R . .
C6 C 0.3398(3) 0.0254(9) 0.0827(2) 0.0664(15) Uani 1 1 d . . .
H6 H 0.3692 -0.0600 0.0862 0.080 Uiso 1 1 calc R . .
C7 C 0.3524(2) 0.2170(9) 0.10622(19) 0.0575(14) Uani 1 1 d . . .
C8 C 0.3078(2) 0.3475(8) 0.10213(18) 0.0530(13) Uani 1 1 d . . .
C9 C 0.3227(2) 0.5364(8) 0.12692(19) 0.0619(14) Uani 1 1 d . . .
H9 H 0.2942 0.6213 0.1262 0.074 Uiso 1 1 calc R . .
C10 C 0.3781(2) 0.5958(9) 0.15192(19) 0.0691(16) Uani 1 1 d . . .
H10 H 0.3868 0.7211 0.1674 0.083 Uiso 1 1 calc R . .
C11 C 0.4215(2) 0.4697(11) 0.1544(2) 0.0755(17) Uani 1 1 d . . .
C12 C 0.4089(3) 0.2841(11) 0.1319(2) 0.0768(17) Uani 1 1 d . . .
H12 H 0.4381 0.2011 0.1337 0.092 Uiso 1 1 calc R . .
C13 C 0.0954(2) 0.2884(10) -0.00758(19) 0.0627(15) Uani 1 1 d . . .
C14 C 0.0548(3) 0.1375(10) -0.0255(2) 0.0815(18) Uani 1 1 d . . .
H14 H 0.0655 0.0050 -0.0171 0.098 Uiso 1 1 calc R . .
C15 C -0.0007(3) 0.1849(12) -0.0556(2) 0.093(2) Uani 1 1 d . . .
H15 H -0.0276 0.0834 -0.0678 0.112 Uiso 1 1 calc R . .
C16 C -0.0178(3) 0.3816(14) -0.0683(2) 0.091(2) Uani 1 1 d . . .
H16 H -0.0557 0.4121 -0.0888 0.109 Uiso 1 1 calc R . .
C17 C 0.0222(3) 0.5309(10) -0.0500(2) 0.0786(18) Uani 1 1 d . . .
H17 H 0.0111 0.6631 -0.0584 0.094 Uiso 1 1 calc R . .
C18 C 0.0779(2) 0.4877(9) -0.0198(2) 0.0667(15) Uani 1 1 d . . .
H18 H 0.1043 0.5904 -0.0073 0.080 Uiso 1 1 calc R . .
C19 C 0.18249(18) 0.4417(8) 0.10191(17) 0.0504(12) Uani 1 1 d . . .
C20 C 0.1706(2) 0.2954(8) 0.13019(19) 0.0669(15) Uani 1 1 d . . .
H20 H 0.1697 0.1620 0.1208 0.080 Uiso 1 1 calc R . .
C21 C 0.1599(2) 0.3449(9) 0.17230(19) 0.0699(16) Uani 1 1 d . . .
H21 H 0.1528 0.2429 0.1906 0.084 Uiso 1 1 calc R . .
C22 C 0.15950(18) 0.5398(8) 0.18763(16) 0.0497(12) Uani 1 1 d . . .
C23 C 0.17104(19) 0.6850(8) 0.15944(19) 0.0604(14) Uani 1 1 d . . .
H23 H 0.1721 0.8182 0.1690 0.073 Uiso 1 1 calc R . .
C24 C 0.18115(19) 0.6369(8) 0.11687(18) 0.0607(14) Uani 1 1 d . . .
H24 H 0.1872 0.7395 0.0980 0.073 Uiso 1 1 calc R . .
C25 C 0.1474(2) 0.5867(9) 0.23417(19) 0.0673(15) Uani 1 1 d . . .
C26 C 0.1922(3) 0.4864(10) 0.2823(2) 0.110(2) Uani 1 1 d . . .
H26A H 0.2291 0.5345 0.2883 0.165 Uiso 1 1 calc R . .
H26B H 0.1907 0.3444 0.2772 0.165 Uiso 1 1 calc R . .
H26C H 0.1852 0.5173 0.3115 0.165 Uiso 1 1 calc R . .
C27 C 0.0887(2) 0.5062(11) 0.2232(3) 0.117(3) Uani 1 1 d . . .
H27A H 0.0801 0.5385 0.2515 0.175 Uiso 1 1 calc R . .
H27B H 0.0882 0.3639 0.2190 0.175 Uiso 1 1 calc R . .
H27C H 0.0609 0.5659 0.1921 0.175 Uiso 1 1 calc R . .
C28 C 0.1485(3) 0.8109(10) 0.2440(3) 0.119(2) Uani 1 1 d . . .
H28A H 0.1863 0.8604 0.2548 0.179 Uiso 1 1 calc R . .
H28B H 0.1365 0.8360 0.2705 0.179 Uiso 1 1 calc R . .
H28C H 0.1234 0.8773 0.2127 0.179 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
Cl1 C11 1.731(6) . ?
N1 C1 1.378(6) . ?
N1 C13 1.428(6) . ?
N1 C4 1.501(6) . ?
O1 C1 1.246(6) . ?
C1 C2 1.444(7) . ?
C2 C3 1.381(6) . ?
C2 C5 1.393(7) . ?
C3 C8 1.420(6) . ?
C3 C4 1.508(6) . ?
C4 C19 1.527(6) . ?
C4 H4 0.9800 . ?
C5 C6 1.360(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.420(7) . ?
C6 H6 0.9300 . ?
C7 C12 1.409(7) . ?
C7 C8 1.422(7) . ?
C8 C9 1.421(7) . ?
C9 C10 1.369(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(7) . ?
C13 C18 1.404(7) . ?
C14 C15 1.368(8) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.375(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.366(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C24 1.381(6) . ?
C19 C20 1.393(6) . ?
C20 C21 1.397(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.379(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(6) . ?
C22 C25 1.536(6) . ?
C23 C24 1.399(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.525(8) . ?
C25 C28 1.525(8) . ?
C25 C27 1.529(7) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
C1 N1 C13 127.2(5) . . ?
C1 N1 C4 110.6(4) . . ?
C13 N1 C4 121.9(5) . . ?
O1 C1 N1 124.9(5) . . ?
O1 C1 C2 127.1(5) . . ?
N1 C1 C2 107.9(5) . . ?
C3 C2 C5 121.2(5) . . ?
C3 C2 C1 110.1(5) . . ?
C5 C2 C1 128.6(5) . . ?
C2 C3 C8 121.0(5) . . ?
C2 C3 C4 109.0(4) . . ?
C8 C3 C4 130.0(5) . . ?
N1 C4 C3 102.3(4) . . ?
N1 C4 C19 111.0(4) . . ?
C3 C4 C19 114.6(4) . . ?
N1 C4 H4 109.5 . . ?
C3 C4 H4 109.5 . . ?
C19 C4 H4 109.5 . . ?
C6 C5 C2 119.7(5) . . ?
C6 C5 H5 120.1 . . ?
C2 C5 H5 120.1 . . ?
C5 C6 C7 120.8(5) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C12 C7 C6 120.7(6) . . ?
C12 C7 C8 119.0(6) . . ?
C6 C7 C8 120.2(5) . . ?
C3 C8 C9 124.9(5) . . ?
C3 C8 C7 117.0(5) . . ?
C9 C8 C7 118.1(5) . . ?
C10 C9 C8 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 120.4(6) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 120.0(6) . . ?
C12 C11 Cl1 121.3(5) . . ?
C10 C11 Cl1 118.6(6) . . ?
C11 C12 C7 121.2(6) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C14 C13 C18 118.9(5) . . ?
C14 C13 N1 120.1(6) . . ?
C18 C13 N1 121.0(5) . . ?
C15 C14 C13 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 121.2(6) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 119.0(6) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C18 C17 C16 120.9(6) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C13 120.1(5) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C24 C19 C20 116.1(4) . . ?
C24 C19 C4 122.4(5) . . ?
C20 C19 C4 121.4(5) . . ?
C19 C20 C21 121.3(5) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 122.3(5) . . ?
C22 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C21 C22 C23 116.4(4) . . ?
C21 C22 C25 120.3(5) . . ?
C23 C22 C25 123.3(5) . . ?
C22 C23 C24 121.7(5) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C19 C24 C23 122.1(5) . . ?
C19 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C26 C25 C28 108.7(5) . . ?
C26 C25 C27 109.9(5) . . ?
C28 C25 C27 108.7(5) . . ?
C26 C25 C22 109.3(4) . . ?
C28 C25 C22 111.6(5) . . ?
C27 C25 C22 108.7(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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
C13 N1 C1 O1 -8.2(7) . . . . ?
C4 N1 C1 O1 177.9(4) . . . . ?
C13 N1 C1 C2 172.0(4) . . . . ?
C4 N1 C1 C2 -1.8(5) . . . . ?
O1 C1 C2 C3 -179.0(5) . . . . ?
N1 C1 C2 C3 0.8(5) . . . . ?
O1 C1 C2 C5 4.7(8) . . . . ?
N1 C1 C2 C5 -175.5(4) . . . . ?
C5 C2 C3 C8 0.5(7) . . . . ?
C1 C2 C3 C8 -176.1(4) . . . . ?
C5 C2 C3 C4 177.2(4) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
C1 N1 C4 C3 2.1(4) . . . . ?
C13 N1 C4 C3 -172.1(4) . . . . ?
C1 N1 C4 C19 -120.6(4) . . . . ?
C13 N1 C4 C19 65.1(5) . . . . ?
C2 C3 C4 N1 -1.6(4) . . . . ?
C8 C3 C4 N1 174.7(4) . . . . ?
C2 C3 C4 C19 118.7(4) . . . . ?
C8 C3 C4 C19 -65.0(6) . . . . ?
C3 C2 C5 C6 -1.6(7) . . . . ?
C1 C2 C5 C6 174.3(5) . . . . ?
C2 C5 C6 C7 0.6(7) . . . . ?
C5 C6 C7 C12 -175.7(4) . . . . ?
C5 C6 C7 C8 1.4(7) . . . . ?
C2 C3 C8 C9 179.8(5) . . . . ?
C4 C3 C8 C9 3.8(7) . . . . ?
C2 C3 C8 C7 1.5(6) . . . . ?
C4 C3 C8 C7 -174.4(4) . . . . ?
C12 C7 C8 C3 174.7(4) . . . . ?
C6 C7 C8 C3 -2.5(6) . . . . ?
C12 C7 C8 C9 -3.6(6) . . . . ?
C6 C7 C8 C9 179.2(4) . . . . ?
C3 C8 C9 C10 -175.1(4) . . . . ?
C7 C8 C9 C10 3.1(7) . . . . ?
C8 C9 C10 C11 -1.1(7) . . . . ?
C9 C10 C11 C12 -0.5(8) . . . . ?
C9 C10 C11 Cl1 175.0(4) . . . . ?
C10 C11 C12 C7 -0.1(8) . . . . ?
Cl1 C11 C12 C7 -175.4(4) . . . . ?
C6 C7 C12 C11 179.4(5) . . . . ?
C8 C7 C12 C11 2.2(7) . . . . ?
C1 N1 C13 C14 28.7(6) . . . . ?
C4 N1 C13 C14 -158.1(4) . . . . ?
C1 N1 C13 C18 -149.5(5) . . . . ?
C4 N1 C13 C18 23.7(6) . . . . ?
C18 C13 C14 C15 1.6(7) . . . . ?
N1 C13 C14 C15 -176.6(4) . . . . ?
C13 C14 C15 C16 -0.7(8) . . . . ?
C14 C15 C16 C17 -0.1(9) . . . . ?
C15 C16 C17 C18 -0.1(8) . . . . ?
C16 C17 C18 C13 1.1(8) . . . . ?
C14 C13 C18 C17 -1.8(7) . . . . ?
N1 C13 C18 C17 176.4(4) . . . . ?
N1 C4 C19 C24 -132.5(5) . . . . ?
C3 C4 C19 C24 112.2(5) . . . . ?
N1 C4 C19 C20 47.2(6) . . . . ?
C3 C4 C19 C20 -68.2(6) . . . . ?
C24 C19 C20 C21 -2.2(7) . . . . ?
C4 C19 C20 C21 178.1(4) . . . . ?
C19 C20 C21 C22 1.2(8) . . . . ?
C20 C21 C22 C23 -0.9(7) . . . . ?
C20 C21 C22 C25 179.9(4) . . . . ?
C21 C22 C23 C24 1.6(7) . . . . ?
C25 C22 C23 C24 -179.2(4) . . . . ?
C20 C19 C24 C23 2.9(7) . . . . ?
C4 C19 C24 C23 -177.4(4) . . . . ?
C22 C23 C24 C19 -2.7(7) . . . . ?
C21 C22 C25 C26 60.3(6) . . . . ?
C23 C22 C25 C26 -118.9(6) . . . . ?
C21 C22 C25 C28 -179.4(5) . . . . ?
C23 C22 C25 C28 1.4(7) . . . . ?
C21 C22 C25 C27 -59.6(6) . . . . ?
C23 C22 C25 C27 121.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_161128f
_database_code_depnum_ccdc_archive 'CCDC 1526670'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H31 N3 O'
_chemical_formula_weight         485.61

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'

_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                   10.3789(9)
_cell_length_b                   11.1013(9)
_cell_length_c                   14.0006(12)
_cell_angle_alpha                95.6210(10)
_cell_angle_beta                 103.538(2)
_cell_angle_gamma                117.117(3)
_cell_volume                     1356.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1159
_cell_measurement_theta_min      2.846
_cell_measurement_theta_max      21.08

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9731
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_process_details   sadabs

_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  '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            6964
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4722
_reflns_number_gt                2330
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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)+(0.0162P)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         4722
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
N1 N 0.4624(2) 0.1917(2) 0.14188(14) 0.0458(5) Uani 1 1 d . . .
N2 N 0.3269(2) -0.0077(2) 0.20747(15) 0.0480(6) Uani 1 1 d . . .
N3 N 0.2201(2) -0.1449(2) 0.17441(17) 0.0548(6) Uani 1 1 d . . .
O1 O 0.6886(2) 0.18803(18) 0.16526(13) 0.0600(5) Uani 1 1 d . . .
C1 C 0.6166(3) 0.2498(3) 0.15675(18) 0.0483(7) Uani 1 1 d . . .
C2 C 0.6715(3) 0.3994(3) 0.16088(18) 0.0460(7) Uani 1 1 d . . .
C3 C 0.5521(3) 0.4244(3) 0.14383(17) 0.0449(7) Uani 1 1 d . . .
C4 C 0.4054(3) 0.2914(2) 0.12895(18) 0.0443(7) Uani 1 1 d . . .
H4 H 0.3377 0.2656 0.0596 0.053 Uiso 1 1 calc R . .
C5 C 0.8226(3) 0.5066(3) 0.18075(19) 0.0590(8) Uani 1 1 d . . .
H5 H 0.9029 0.4879 0.1916 0.071 Uiso 1 1 calc R . .
C6 C 0.8476(4) 0.6388(3) 0.1835(2) 0.0673(9) Uani 1 1 d . . .
H6 H 0.9469 0.7113 0.1982 0.081 Uiso 1 1 calc R . .
C7 C 0.7259(4) 0.6685(3) 0.16469(19) 0.0568(8) Uani 1 1 d . . .
C8 C 0.5739(3) 0.5596(3) 0.14252(17) 0.0478(7) Uani 1 1 d . . .
C9 C 0.4551(4) 0.5910(3) 0.12220(18) 0.0608(8) Uani 1 1 d . . .
H9 H 0.3546 0.5201 0.1064 0.073 Uiso 1 1 calc R . .
C10 C 0.4867(4) 0.7259(4) 0.1256(2) 0.0761(10) Uani 1 1 d . . .
H10 H 0.4072 0.7457 0.1117 0.091 Uiso 1 1 calc R . .
C11 C 0.6356(5) 0.8328(3) 0.1495(2) 0.0832(11) Uani 1 1 d . . .
H11 H 0.6554 0.9239 0.1534 0.100 Uiso 1 1 calc R . .
C12 C 0.7527(4) 0.8062(3) 0.1672(2) 0.0774(10) Uani 1 1 d . . .
H12 H 0.8517 0.8788 0.1813 0.093 Uiso 1 1 calc R . .
C13 C 0.3624(3) 0.0491(3) 0.1288(2) 0.0450(7) Uani 1 1 d . . .
C14 C 0.2766(3) -0.0534(3) 0.0437(2) 0.0546(7) Uani 1 1 d . . .
H14 H 0.2761 -0.0462 -0.0220 0.065 Uiso 1 1 calc R . .
C15 C 0.1886(3) -0.1724(3) 0.0741(2) 0.0556(7) Uani 1 1 d . . .
C16 C 0.0787(3) -0.3170(3) 0.0115(2) 0.0808(10) Uani 1 1 d . . .
H16A H 0.0891 -0.3827 0.0478 0.121 Uiso 1 1 calc R . .
H16B H 0.0999 -0.3285 -0.0509 0.121 Uiso 1 1 calc R . .
H16C H -0.0235 -0.3325 -0.0026 0.121 Uiso 1 1 calc R . .
C17 C 0.3864(3) 0.0555(3) 0.3136(2) 0.0482(7) Uani 1 1 d . . .
C18 C 0.5411(3) 0.1354(3) 0.3610(2) 0.0575(8) Uani 1 1 d . . .
H18 H 0.6089 0.1485 0.3246 0.069 Uiso 1 1 calc R . .
C19 C 0.5947(4) 0.1961(3) 0.4632(2) 0.0634(8) Uani 1 1 d . . .
H19 H 0.6993 0.2510 0.4948 0.076 Uiso 1 1 calc R . .
C20 C 0.4983(4) 0.1777(3) 0.5195(2) 0.0641(8) Uani 1 1 d . . .
C21 C 0.3445(4) 0.0942(3) 0.4706(2) 0.0686(9) Uani 1 1 d . . .
H21 H 0.2771 0.0788 0.5076 0.082 Uiso 1 1 calc R . .
C22 C 0.2866(3) 0.0324(3) 0.3683(2) 0.0611(8) Uani 1 1 d . . .
H22 H 0.1821 -0.0238 0.3370 0.073 Uiso 1 1 calc R . .
C23 C 0.5565(4) 0.2448(3) 0.6312(2) 0.0957(12) Uani 1 1 d . . .
H23A H 0.6436 0.2365 0.6632 0.144 Uiso 1 1 calc R . .
H23B H 0.4777 0.1990 0.6609 0.144 Uiso 1 1 calc R . .
H23C H 0.5850 0.3415 0.6404 0.144 Uiso 1 1 calc R . .
C24 C 0.3215(3) 0.2954(2) 0.20269(18) 0.0416(6) Uani 1 1 d . . .
C25 C 0.1651(3) 0.2241(3) 0.17380(19) 0.0564(7) Uani 1 1 d . . .
H25 H 0.1098 0.1743 0.1072 0.068 Uiso 1 1 calc R . .
C26 C 0.0881(3) 0.2252(3) 0.2426(2) 0.0601(8) Uani 1 1 d . . .
H26 H -0.0180 0.1768 0.2207 0.072 Uiso 1 1 calc R . .
C27 C 0.1652(3) 0.2965(3) 0.3430(2) 0.0483(7) Uani 1 1 d . . .
C28 C 0.3226(3) 0.3667(3) 0.37057(19) 0.0538(7) Uani 1 1 d . . .
H28 H 0.3789 0.4152 0.4374 0.065 Uiso 1 1 calc R . .
C29 C 0.3986(3) 0.3669(3) 0.30185(19) 0.0518(7) Uani 1 1 d . . .
H29 H 0.5047 0.4166 0.3232 0.062 Uiso 1 1 calc R . .
C30 C 0.0774(3) 0.2961(3) 0.4171(2) 0.0588(8) Uani 1 1 d . . .
C31 C -0.0050(3) 0.3784(3) 0.3867(2) 0.0848(10) Uani 1 1 d . . .
H31A H -0.0769 0.3331 0.3200 0.127 Uiso 1 1 calc R . .
H31B H 0.0683 0.4713 0.3875 0.127 Uiso 1 1 calc R . .
H31C H -0.0580 0.3821 0.4337 0.127 Uiso 1 1 calc R . .
C32 C -0.0404(4) 0.1477(3) 0.4118(3) 0.1016(12) Uani 1 1 d . . .
H32A H -0.1154 0.1080 0.3460 0.152 Uiso 1 1 calc R . .
H32B H -0.0892 0.1483 0.4621 0.152 Uiso 1 1 calc R . .
H32C H 0.0090 0.0932 0.4240 0.152 Uiso 1 1 calc R . .
C33 C 0.1837(4) 0.3664(3) 0.5263(2) 0.0957(11) Uani 1 1 d . . .
H33A H 0.1248 0.3666 0.5699 0.143 Uiso 1 1 calc R . .
H33B H 0.2572 0.4605 0.5300 0.143 Uiso 1 1 calc R . .
H33C H 0.2355 0.3160 0.5474 0.143 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
N1 C1 1.377(3) . ?
N1 C13 1.405(3) . ?
N1 C4 1.481(3) . ?
N2 N3 1.358(2) . ?
N2 C13 1.364(3) . ?
N2 C17 1.432(3) . ?
N3 C15 1.336(3) . ?
O1 C1 1.219(3) . ?
C1 C2 1.479(3) . ?
C2 C3 1.364(3) . ?
C2 C5 1.408(3) . ?
C3 C8 1.414(3) . ?
C3 C4 1.511(3) . ?
C4 C24 1.508(3) . ?
C4 H4 0.9800 . ?
C5 C6 1.363(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.420(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.416(3) . ?
C7 C12 1.419(3) . ?
C8 C9 1.403(3) . ?
C9 C10 1.373(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.350(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.350(3) . ?
C14 C15 1.397(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.494(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C22 1.375(3) . ?
C17 C18 1.376(3) . ?
C18 C19 1.381(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.370(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(4) . ?
C20 C23 1.511(3) . ?
C21 C22 1.383(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C29 1.372(3) . ?
C24 C25 1.372(3) . ?
C25 C26 1.391(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.382(3) . ?
C27 C30 1.532(3) . ?
C28 C29 1.379(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C32 1.521(3) . ?
C30 C33 1.535(4) . ?
C30 C31 1.538(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 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
C1 N1 C13 124.5(2) . . ?
C1 N1 C4 113.7(2) . . ?
C13 N1 C4 121.5(2) . . ?
N3 N2 C13 111.1(2) . . ?
N3 N2 C17 119.29(19) . . ?
C13 N2 C17 129.6(2) . . ?
C15 N3 N2 105.14(19) . . ?
O1 C1 N1 125.9(2) . . ?
O1 C1 C2 129.0(3) . . ?
N1 C1 C2 105.1(2) . . ?
C3 C2 C5 122.0(2) . . ?
C3 C2 C1 110.1(2) . . ?
C5 C2 C1 127.9(3) . . ?
C2 C3 C8 121.3(2) . . ?
C2 C3 C4 110.2(2) . . ?
C8 C3 C4 128.5(2) . . ?
N1 C4 C24 111.64(17) . . ?
N1 C4 C3 100.92(19) . . ?
C24 C4 C3 115.1(2) . . ?
N1 C4 H4 109.6 . . ?
C24 C4 H4 109.6 . . ?
C3 C4 H4 109.6 . . ?
C6 C5 C2 117.9(3) . . ?
C6 C5 H5 121.1 . . ?
C2 C5 H5 121.1 . . ?
C5 C6 C7 121.7(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C12 118.6(3) . . ?
C8 C7 C6 120.1(3) . . ?
C12 C7 C6 121.3(3) . . ?
C9 C8 C3 123.9(3) . . ?
C9 C8 C7 119.1(2) . . ?
C3 C8 C7 117.0(3) . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 C10 120.8(3) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
C14 C13 N2 107.0(2) . . ?
C14 C13 N1 130.4(2) . . ?
N2 C13 N1 122.4(2) . . ?
C13 C14 C15 106.2(2) . . ?
C13 C14 H14 126.9 . . ?
C15 C14 H14 126.9 . . ?
N3 C15 C14 110.6(2) . . ?
N3 C15 C16 120.3(2) . . ?
C14 C15 C16 129.0(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 120.2(3) . . ?
C22 C17 N2 119.0(3) . . ?
C18 C17 N2 120.8(2) . . ?
C17 C18 C19 119.3(3) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 122.0(3) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C19 C20 C21 117.4(3) . . ?
C19 C20 C23 122.1(3) . . ?
C21 C20 C23 120.5(3) . . ?
C20 C21 C22 122.2(3) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C17 C22 C21 118.8(3) . . ?
C17 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C29 C24 C25 117.5(2) . . ?
C29 C24 C4 121.3(2) . . ?
C25 C24 C4 121.2(2) . . ?
C24 C25 C26 121.1(3) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C27 C26 C25 121.7(2) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C28 C27 C26 116.3(2) . . ?
C28 C27 C30 123.1(3) . . ?
C26 C27 C30 120.6(2) . . ?
C29 C28 C27 121.9(3) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C24 C29 C28 121.6(2) . . ?
C24 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C32 C30 C27 110.2(2) . . ?
C32 C30 C33 109.4(2) . . ?
C27 C30 C33 112.1(2) . . ?
C32 C30 C31 108.9(2) . . ?
C27 C30 C31 108.2(2) . . ?
C33 C30 C31 107.9(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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
C13 N2 N3 C15 -0.6(3) . . . . ?
C17 N2 N3 C15 -179.7(2) . . . . ?
C13 N1 C1 O1 -3.5(4) . . . . ?
C4 N1 C1 O1 -176.9(2) . . . . ?
C13 N1 C1 C2 177.1(2) . . . . ?
C4 N1 C1 C2 3.7(3) . . . . ?
O1 C1 C2 C3 177.6(2) . . . . ?
N1 C1 C2 C3 -3.0(3) . . . . ?
O1 C1 C2 C5 -3.4(4) . . . . ?
N1 C1 C2 C5 175.9(2) . . . . ?
C5 C2 C3 C8 1.8(4) . . . . ?
C1 C2 C3 C8 -179.2(2) . . . . ?
C5 C2 C3 C4 -177.7(2) . . . . ?
C1 C2 C3 C4 1.3(3) . . . . ?
C1 N1 C4 C24 -125.6(2) . . . . ?
C13 N1 C4 C24 60.8(3) . . . . ?
C1 N1 C4 C3 -2.9(2) . . . . ?
C13 N1 C4 C3 -176.5(2) . . . . ?
C2 C3 C4 N1 0.8(2) . . . . ?
C8 C3 C4 N1 -178.6(2) . . . . ?
C2 C3 C4 C24 121.2(2) . . . . ?
C8 C3 C4 C24 -58.3(3) . . . . ?
C3 C2 C5 C6 0.6(4) . . . . ?
C1 C2 C5 C6 -178.2(2) . . . . ?
C2 C5 C6 C7 -1.6(4) . . . . ?
C5 C6 C7 C8 0.2(4) . . . . ?
C5 C6 C7 C12 -179.7(2) . . . . ?
C2 C3 C8 C9 177.9(2) . . . . ?
C4 C3 C8 C9 -2.7(4) . . . . ?
C2 C3 C8 C7 -3.1(3) . . . . ?
C4 C3 C8 C7 176.3(2) . . . . ?
C12 C7 C8 C9 1.1(4) . . . . ?
C6 C7 C8 C9 -178.8(2) . . . . ?
C12 C7 C8 C3 -178.0(2) . . . . ?
C6 C7 C8 C3 2.1(3) . . . . ?
C3 C8 C9 C10 177.9(2) . . . . ?
C7 C8 C9 C10 -1.1(4) . . . . ?
C8 C9 C10 C11 -0.3(4) . . . . ?
C9 C10 C11 C12 1.8(5) . . . . ?
C10 C11 C12 C7 -1.9(5) . . . . ?
C8 C7 C12 C11 0.4(4) . . . . ?
C6 C7 C12 C11 -179.8(3) . . . . ?
N3 N2 C13 C14 0.2(3) . . . . ?
C17 N2 C13 C14 179.2(2) . . . . ?
N3 N2 C13 N1 175.6(2) . . . . ?
C17 N2 C13 N1 -5.3(4) . . . . ?
C1 N1 C13 C14 -92.2(4) . . . . ?
C4 N1 C13 C14 80.7(3) . . . . ?
C1 N1 C13 N2 93.5(3) . . . . ?
C4 N1 C13 N2 -93.6(3) . . . . ?
N2 C13 C14 C15 0.3(3) . . . . ?
N1 C13 C14 C15 -174.7(2) . . . . ?
N2 N3 C15 C14 0.8(3) . . . . ?
N2 N3 C15 C16 177.5(2) . . . . ?
C13 C14 C15 N3 -0.6(3) . . . . ?
C13 C14 C15 C16 -177.1(3) . . . . ?
N3 N2 C17 C22 -47.3(3) . . . . ?
C13 N2 C17 C22 133.8(3) . . . . ?
N3 N2 C17 C18 131.2(2) . . . . ?
C13 N2 C17 C18 -47.8(4) . . . . ?
C22 C17 C18 C19 -2.2(4) . . . . ?
N2 C17 C18 C19 179.3(2) . . . . ?
C17 C18 C19 C20 0.8(4) . . . . ?
C18 C19 C20 C21 0.9(4) . . . . ?
C18 C19 C20 C23 -179.5(3) . . . . ?
C19 C20 C21 C22 -1.3(4) . . . . ?
C23 C20 C21 C22 179.2(2) . . . . ?
C18 C17 C22 C21 1.9(4) . . . . ?
N2 C17 C22 C21 -179.6(2) . . . . ?
C20 C21 C22 C17 -0.1(4) . . . . ?
N1 C4 C24 C29 78.0(3) . . . . ?
C3 C4 C24 C29 -36.2(3) . . . . ?
N1 C4 C24 C25 -100.0(3) . . . . ?
C3 C4 C24 C25 145.8(2) . . . . ?
C29 C24 C25 C26 0.3(4) . . . . ?
C4 C24 C25 C26 178.4(2) . . . . ?
C24 C25 C26 C27 -0.7(4) . . . . ?
C25 C26 C27 C28 0.2(4) . . . . ?
C25 C26 C27 C30 179.9(2) . . . . ?
C26 C27 C28 C29 0.6(4) . . . . ?
C30 C27 C28 C29 -179.1(2) . . . . ?
C25 C24 C29 C28 0.5(4) . . . . ?
C4 C24 C29 C28 -177.6(2) . . . . ?
C27 C28 C29 C24 -1.0(4) . . . . ?
C28 C27 C30 C32 -129.2(3) . . . . ?
C26 C27 C30 C32 51.1(3) . . . . ?
C28 C27 C30 C33 -7.1(4) . . . . ?
C26 C27 C30 C33 173.2(3) . . . . ?
C28 C27 C30 C31 111.7(3) . . . . ?
C26 C27 C30 C31 -67.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.036
