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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_001

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 Cl N O2'
_chemical_formula_weight         367.86

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'
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'
H H 0.0000 0.0000 '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+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   7.5759(6)
_cell_length_b                   11.0478(10)
_cell_length_c                   23.488(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1965.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7315

_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      23.53


_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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 APEX-II CCD'

_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19609
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4520
_reflns_number_gt                2966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'

_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)+(0.0918P)²+0.2263P] 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   0.95(10)
_refine_ls_number_reflns         4498
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1606
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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
C1 C -0.1135(3) 0.6069(3) 0.04155(13) 0.0663(7) Uani 1 1 d . . .
C2 C -0.0449(4) 0.5379(3) -0.00180(11) 0.0630(7) Uani 1 1 d . . .
H2 H -0.0622 0.5606 -0.0395 0.076 Uiso 1 1 calc R . .
C3 C 0.0498(3) 0.4346(2) 0.01103(11) 0.0563(6) Uani 1 1 d . . .
H3 H 0.0980 0.3880 -0.0181 0.068 Uiso 1 1 calc R . .
C4 C 0.0730(3) 0.4006(2) 0.06718(10) 0.0468(5) Uani 1 1 d . . .
C5 C 0.0024(3) 0.4703(2) 0.11003(11) 0.0573(6) Uani 1 1 d . . .
H5 H 0.0176 0.4469 0.1478 0.069 Uiso 1 1 calc R . .
C6 C -0.0911(4) 0.5749(3) 0.09761(12) 0.0651(7) Uani 1 1 d . . .
H6 H -0.1377 0.6224 0.1266 0.078 Uiso 1 1 calc R . .
C7 C 0.1773(3) 0.2908(2) 0.08206(10) 0.0511(6) Uani 1 1 d . . .
C8 C 0.0979(3) 0.1835(2) 0.10168(11) 0.0552(6) Uani 1 1 d . . .
C9 C -0.0940(3) 0.1697(2) 0.10073(12) 0.0596(7) Uani 1 1 d . . .
C10 C -0.1756(4) 0.0638(3) 0.13189(16) 0.0807(9) Uani 1 1 d . . .
H10A H -0.2813 0.0922 0.1510 0.097 Uiso 1 1 calc R . .
H10B H -0.2122 0.0045 0.1038 0.097 Uiso 1 1 calc R . .
C11 C -0.0627(4) 0.0008(3) 0.17500(14) 0.0711(8) Uani 1 1 d . . .
C12 C 0.1149(4) -0.0237(3) 0.14808(16) 0.0794(9) Uani 1 1 d . . .
H12A H 0.1912 -0.0607 0.1763 0.095 Uiso 1 1 calc R . .
H12B H 0.0993 -0.0815 0.1174 0.095 Uiso 1 1 calc R . .
C13 C 0.2052(3) 0.0867(3) 0.12477(11) 0.0610(6) Uani 1 1 d . . .
C15 C 0.4512(3) 0.4113(3) 0.06727(13) 0.0673(7) Uani 1 1 d . . .
H15A H 0.3921 0.4577 0.0378 0.081 Uiso 1 1 calc R . .
H15B H 0.5675 0.3899 0.0533 0.081 Uiso 1 1 calc R . .
C16 C 0.4704(3) 0.4889(3) 0.11965(11) 0.0594(7) Uani 1 1 d . . .
C17 C 0.4333(4) 0.6093(3) 0.11775(16) 0.0830(9) Uani 1 1 d . . .
H17 H 0.3915 0.6442 0.0843 0.100 Uiso 1 1 calc R . .
C18 C 0.4584(6) 0.6796(4) 0.1660(3) 0.1180(15) Uani 1 1 d . . .
H18 H 0.4327 0.7618 0.1645 0.142 Uiso 1 1 calc R . .
C19 C 0.5198(7) 0.6313(7) 0.2155(2) 0.1244(18) Uani 1 1 d . . .
H19 H 0.5378 0.6797 0.2474 0.149 Uiso 1 1 calc R . .
C20 C 0.5531(7) 0.5144(6) 0.21723(17) 0.125(2) Uani 1 1 d . . .
H20 H 0.5926 0.4802 0.2511 0.150 Uiso 1 1 calc R . .
C21 C 0.5308(5) 0.4404(4) 0.16967(15) 0.0892(10) Uani 1 1 d . . .
H21 H 0.5569 0.3583 0.1719 0.107 Uiso 1 1 calc R . .
C22 C -0.0353(6) 0.0868(4) 0.22671(15) 0.1024(12) Uani 1 1 d . . .
H22A H 0.0183 0.1608 0.2140 0.154 Uiso 1 1 calc R . .
H22B H 0.0401 0.0484 0.2541 0.154 Uiso 1 1 calc R . .
H22C H -0.1474 0.1043 0.2439 0.154 Uiso 1 1 calc R . .
C23 C -0.1465(6) -0.1137(3) 0.1967(2) 0.1089(13) Uani 1 1 d . . .
H23A H -0.2606 -0.0954 0.2123 0.163 Uiso 1 1 calc R . .
H23B H -0.0732 -0.1484 0.2258 0.163 Uiso 1 1 calc R . .
H23C H -0.1592 -0.1702 0.1659 0.163 Uiso 1 1 calc R . .
Cl1 Cl -0.23077(14) 0.73751(9) 0.02538(5) 0.1133(4) Uani 1 1 d . . .
N1 N 0.3512(3) 0.3009(2) 0.07817(11) 0.0630(6) Uani 1 1 d . . .
O1 O -0.1930(2) 0.23653(17) 0.07495(10) 0.0778(6) Uani 1 1 d . . .
O2 O 0.3689(2) 0.0903(2) 0.12632(9) 0.0766(6) Uani 1 1 d . . .
H1N H 0.412(5) 0.229(3) 0.0868(15) 0.100(12) Uiso 1 1 d . . .


_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
C1 C2 1.374(4) . ?
C1 C6 1.374(4) . ?
C1 Cl1 1.736(3) . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(3) . ?
C4 C7 1.489(3) . ?
C5 C6 1.387(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 N1 1.326(3) . ?
C7 C8 1.407(4) . ?
C8 C13 1.449(4) . ?
C8 C9 1.462(4) . ?
C9 O1 1.214(3) . ?
C9 C10 1.512(4) . ?
C10 C11 1.497(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C23 1.504(4) . ?
C11 C12 1.511(5) . ?
C11 C22 1.556(5) . ?
C12 C13 1.502(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O2 1.241(3) . ?
C15 N1 1.459(4) . ?
C15 C16 1.506(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.360(4) . ?
C16 C21 1.370(4) . ?
C17 C18 1.387(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.362(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.317(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.394(6) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 H1N 0.94(4) . ?

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 C1 C6 121.4(3) . . ?
C2 C1 Cl1 119.5(2) . . ?
C6 C1 Cl1 119.1(2) . . ?
C1 C2 C3 119.5(2) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 C7 119.4(2) . . ?
C3 C4 C7 120.8(2) . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 118.6(3) . . ?
C1 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N1 C7 C8 121.2(2) . . ?
N1 C7 C4 116.3(2) . . ?
C8 C7 C4 122.5(2) . . ?
C7 C8 C13 120.3(2) . . ?
C7 C8 C9 120.5(2) . . ?
C13 C8 C9 119.1(2) . . ?
O1 C9 C8 123.9(3) . . ?
O1 C9 C10 117.4(2) . . ?
C8 C9 C10 118.7(2) . . ?
C11 C10 C9 117.0(2) . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C9 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C10 C11 C23 112.3(3) . . ?
C10 C11 C12 108.0(3) . . ?
C23 C11 C12 111.6(3) . . ?
C10 C11 C22 108.7(3) . . ?
C23 C11 C22 107.7(3) . . ?
C12 C11 C22 108.5(3) . . ?
C13 C12 C11 114.4(2) . . ?
C13 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O2 C13 C8 123.2(3) . . ?
O2 C13 C12 118.1(3) . . ?
C8 C13 C12 118.7(2) . . ?
N1 C15 C16 112.5(2) . . ?
N1 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N1 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C21 118.7(3) . . ?
C17 C16 C15 120.6(3) . . ?
C21 C16 C15 120.7(3) . . ?
C16 C17 C18 119.5(4) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 121.7(4) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C18 118.4(5) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
C19 C20 C21 121.8(5) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C16 C21 C20 119.9(4) . . ?
C16 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C11 C22 H22A 109.5 . . ?
C11 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C11 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C11 C23 H23A 109.5 . . ?
C11 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C11 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 N1 C15 126.8(2) . . ?
C7 N1 H1N 114(2) . . ?
C15 N1 H1N 119(2) . . ?

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
C6 C1 C2 C3 -0.6(4) . . . . ?
Cl1 C1 C2 C3 179.4(2) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 C7 -178.9(2) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C7 C4 C5 C6 178.2(2) . . . . ?
C2 C1 C6 C5 -0.2(4) . . . . ?
Cl1 C1 C6 C5 179.8(2) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C5 C4 C7 N1 -102.8(3) . . . . ?
C3 C4 C7 N1 75.8(3) . . . . ?
C5 C4 C7 C8 74.4(3) . . . . ?
C3 C4 C7 C8 -107.0(3) . . . . ?
N1 C7 C8 C13 7.7(4) . . . . ?
C4 C7 C8 C13 -169.4(2) . . . . ?
N1 C7 C8 C9 -174.3(3) . . . . ?
C4 C7 C8 C9 8.7(4) . . . . ?
C7 C8 C9 O1 13.3(4) . . . . ?
C13 C8 C9 O1 -168.6(3) . . . . ?
C7 C8 C9 C10 -168.9(3) . . . . ?
C13 C8 C9 C10 9.2(4) . . . . ?
O1 C9 C10 C11 -165.0(3) . . . . ?
C8 C9 C10 C11 17.1(4) . . . . ?
C9 C10 C11 C23 -171.3(3) . . . . ?
C9 C10 C11 C12 -47.9(4) . . . . ?
C9 C10 C11 C22 69.6(4) . . . . ?
C10 C11 C12 C13 55.4(4) . . . . ?
C23 C11 C12 C13 179.3(3) . . . . ?
C22 C11 C12 C13 -62.2(4) . . . . ?
C7 C8 C13 O2 -3.1(4) . . . . ?
C9 C8 C13 O2 178.8(3) . . . . ?
C7 C8 C13 C12 176.8(2) . . . . ?
C9 C8 C13 C12 -1.2(4) . . . . ?
C11 C12 C13 O2 147.4(3) . . . . ?
C11 C12 C13 C8 -32.5(4) . . . . ?
N1 C15 C16 C17 -131.0(3) . . . . ?
N1 C15 C16 C21 51.1(3) . . . . ?
C21 C16 C17 C18 0.4(5) . . . . ?
C15 C16 C17 C18 -177.6(3) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C17 C18 C19 C20 -1.0(7) . . . . ?
C18 C19 C20 C21 1.4(8) . . . . ?
C17 C16 C21 C20 0.0(5) . . . . ?
C15 C16 C21 C20 177.9(3) . . . . ?
C19 C20 C21 C16 -0.9(7) . . . . ?
C8 C7 N1 C15 -169.7(3) . . . . ?
C4 C7 N1 C15 7.6(4) . . . . ?
C16 C15 N1 C7 79.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O2 0.94(4) 1.82(3) 2.590(3) 137(3) .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 959044'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_001

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H21 N O4'
_chemical_formula_weight         315.36

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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   10.0101(10)
_cell_length_b                   10.7765(10)
_cell_length_c                   15.5711(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.900(3)
_cell_angle_gamma                90.00
_cell_volume                     1675.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20912
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         27.53
_reflns_number_total             3851
_reflns_number_gt                2868
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0648P)²+0.5659P] 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         3841
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
C2 C 0.70658(17) 0.12376(17) 0.01855(11) 0.0472(4) Uani 1 1 d . . .
H2 H 0.7083 0.1170 0.0782 0.057 Uiso 1 1 calc R . .
C3 C 0.66384(19) 0.02447(18) -0.03218(13) 0.0543(5) Uani 1 1 d . . .
H3 H 0.6384 -0.0487 -0.0061 0.065 Uiso 1 1 calc R . .
O4 O 1.26122(12) 0.28103(13) -0.01054(8) 0.0529(4) Uani 1 1 d . . .
H1 H 1.345(3) 0.305(2) 0.0126(15) 0.079 Uiso 1 1 d . . .
N1 N 0.92912(13) 0.35614(15) 0.04034(10) 0.0474(4) Uani 1 1 d . . .
O1 O 0.51066(10) 0.33665(12) 0.02873(7) 0.0490(3) Uani 1 1 d . . .
C14 C 0.6082(3) 0.3816(2) 0.28704(14) 0.0736(6) Uani 1 1 d . . .
H14A H 0.6623 0.3281 0.2544 0.110 Uiso 1 1 calc R . .
H14B H 0.5275 0.3391 0.2996 0.110 Uiso 1 1 calc R . .
H14C H 0.6571 0.4041 0.3399 0.110 Uiso 1 1 calc R . .
C11 C 0.57303(17) 0.49766(17) 0.23529(10) 0.0439(4) Uani 1 1 d . . .
C4 C 0.65821(17) 0.03172(18) -0.12083(12) 0.0509(4) Uani 1 1 d . . .
C18 C 0.6115(2) -0.0781(2) -0.17510(17) 0.0791(7) Uani 1 1 d . . .
H18A H 0.5867 -0.0509 -0.2327 0.119 Uiso 1 1 calc R . .
H18B H 0.5354 -0.1155 -0.1509 0.119 Uiso 1 1 calc R . .
H18C H 0.6825 -0.1378 -0.1762 0.119 Uiso 1 1 calc R . .
C16 C 1.02850(15) 0.28691(18) -0.00346(12) 0.0486(4) Uani 1 1 d . . .
H16A H 1.0187 0.3031 -0.0648 0.058 Uiso 1 1 calc R . .
H16B H 1.0171 0.1986 0.0057 0.058 Uiso 1 1 calc R . .
C15 C 0.4889(2) 0.5837(2) 0.28844(14) 0.0678(6) Uani 1 1 d . . .
H15A H 0.5400 0.6073 0.3403 0.102 Uiso 1 1 calc R . .
H15B H 0.4092 0.5412 0.3029 0.102 Uiso 1 1 calc R . .
H15C H 0.4648 0.6566 0.2555 0.102 Uiso 1 1 calc R . .
C5 C 0.69819(19) 0.14147(19) -0.15722(11) 0.0533(5) Uani 1 1 d . . .
H5 H 0.6948 0.1485 -0.2169 0.064 Uiso 1 1 calc R . .
O3 O 1.18159(13) 0.39677(19) 0.09259(11) 0.0869(6) Uani 1 1 d . . .
C12 C 0.49599(16) 0.46481(19) 0.15063(11) 0.0488(4) Uani 1 1 d . . .
H12A H 0.4195 0.4144 0.1633 0.059 Uiso 1 1 calc R . .
H12B H 0.4618 0.5410 0.1242 0.059 Uiso 1 1 calc R . .
C13 C 0.57392(15) 0.39644(15) 0.08603(10) 0.0382(4) Uani 1 1 d . . .
C8 C 0.71870(15) 0.40785(16) 0.09128(10) 0.0393(4) Uani 1 1 d . . .
C7 C 0.79943(14) 0.33631(15) 0.03792(10) 0.0376(4) Uani 1 1 d . . .
C1 C 0.74677(14) 0.23313(15) -0.01826(10) 0.0367(3) Uani 1 1 d . . .
C17 C 1.16511(16) 0.32783(18) 0.03270(11) 0.0466(4) Uani 1 1 d . . .
C10 C 0.69689(19) 0.56620(19) 0.21114(12) 0.0542(5) Uani 1 1 d . . .
H10A H 0.6696 0.6445 0.1847 0.065 Uiso 1 1 calc R . .
H10B H 0.7516 0.5849 0.2633 0.065 Uiso 1 1 calc R . .
C9 C 0.78097(17) 0.49714(17) 0.15080(11) 0.0469(4) Uani 1 1 d . . .
C6 C 0.74337(16) 0.24175(18) -0.10700(10) 0.0455(4) Uani 1 1 d . . .
H6 H 0.7711 0.3142 -0.1330 0.055 Uiso 1 1 calc R . .
H1N H 0.956(2) 0.420(2) 0.0753(15) 0.069(7) Uiso 1 1 d . . .
O2 O 0.90213(12) 0.52234(15) 0.15372(9) 0.0659(4) Uani 1 1 d . . .


_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
C2 C3 1.380(3) . ?
C2 C1 1.382(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
O4 C17 1.312(2) . ?
O4 H1 0.93(3) . ?
N1 C7 1.314(2) . ?
N1 C16 1.450(2) . ?
N1 H1N 0.91(2) . ?
O1 C13 1.2391(19) . ?
C14 C11 1.516(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11 C10 1.512(2) . ?
C11 C12 1.523(2) . ?
C11 C15 1.533(3) . ?
C4 C5 1.382(3) . ?
C4 C18 1.510(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C16 C17 1.509(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C5 C6 1.391(3) . ?
C5 H5 0.9300 . ?
O3 C17 1.195(2) . ?
C12 C13 1.507(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C8 1.451(2) . ?
C8 C7 1.425(2) . ?
C8 C9 1.447(2) . ?
C7 C1 1.489(2) . ?
C1 C6 1.383(2) . ?
C10 C9 1.501(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 O2 1.241(2) . ?
C6 H6 0.9300 . ?

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
C3 C2 C1 120.75(16) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 121.23(18) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C17 O4 H1 111.6(15) . . ?
C7 N1 C16 127.66(15) . . ?
C7 N1 H1N 113.2(14) . . ?
C16 N1 H1N 119.1(14) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C11 C14 111.73(17) . . ?
C10 C11 C12 105.88(14) . . ?
C14 C11 C12 110.73(17) . . ?
C10 C11 C15 109.17(16) . . ?
C14 C11 C15 109.18(17) . . ?
C12 C11 C15 110.10(15) . . ?
C3 C4 C5 117.72(17) . . ?
C3 C4 C18 120.4(2) . . ?
C5 C4 C18 121.91(19) . . ?
C4 C18 H18A 109.5 . . ?
C4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C16 C17 107.91(14) . . ?
N1 C16 H16A 110.1 . . ?
C17 C16 H16A 110.1 . . ?
N1 C16 H16B 110.1 . . ?
C17 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C5 C6 121.75(16) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C13 C12 C11 115.91(13) . . ?
C13 C12 H12A 108.3 . . ?
C11 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
C11 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
O1 C13 C8 122.97(14) . . ?
O1 C13 C12 118.20(13) . . ?
C8 C13 C12 118.77(14) . . ?
C7 C8 C9 119.78(14) . . ?
C7 C8 C13 121.68(14) . . ?
C9 C8 C13 118.52(14) . . ?
N1 C7 C8 119.60(14) . . ?
N1 C7 C1 116.62(14) . . ?
C8 C7 C1 123.69(13) . . ?
C2 C1 C6 118.91(15) . . ?
C2 C1 C7 119.64(14) . . ?
C6 C1 C7 121.37(15) . . ?
O3 C17 O4 124.91(16) . . ?
O3 C17 C16 123.12(15) . . ?
O4 C17 C16 111.95(15) . . ?
C9 C10 C11 114.68(15) . . ?
C9 C10 H10A 108.6 . . ?
C11 C10 H10A 108.6 . . ?
C9 C10 H10B 108.6 . . ?
C11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
O2 C9 C8 123.12(16) . . ?
O2 C9 C10 117.19(15) . . ?
C8 C9 C10 119.67(15) . . ?
C1 C6 C5 119.63(17) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?

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
C1 C2 C3 C4 -0.9(3) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C2 C3 C4 C18 179.86(19) . . . . ?
C7 N1 C16 C17 -168.87(17) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C18 C4 C5 C6 -178.89(18) . . . . ?
C10 C11 C12 C13 53.3(2) . . . . ?
C14 C11 C12 C13 -68.0(2) . . . . ?
C15 C11 C12 C13 171.18(17) . . . . ?
C11 C12 C13 O1 159.30(16) . . . . ?
C11 C12 C13 C8 -23.4(2) . . . . ?
O1 C13 C8 C7 -9.2(3) . . . . ?
C12 C13 C8 C7 173.65(16) . . . . ?
O1 C13 C8 C9 169.04(16) . . . . ?
C12 C13 C8 C9 -8.1(2) . . . . ?
C16 N1 C7 C8 174.64(17) . . . . ?
C16 N1 C7 C1 -2.0(3) . . . . ?
C9 C8 C7 N1 -3.2(2) . . . . ?
C13 C8 C7 N1 175.02(16) . . . . ?
C9 C8 C7 C1 173.20(15) . . . . ?
C13 C8 C7 C1 -8.6(2) . . . . ?
C3 C2 C1 C6 0.1(3) . . . . ?
C3 C2 C1 C7 -176.67(15) . . . . ?
N1 C7 C1 C2 106.46(18) . . . . ?
C8 C7 C1 C2 -70.0(2) . . . . ?
N1 C7 C1 C6 -70.2(2) . . . . ?
C8 C7 C1 C6 113.33(18) . . . . ?
N1 C16 C17 O3 6.4(3) . . . . ?
N1 C16 C17 O4 -172.21(15) . . . . ?
C14 C11 C10 C9 65.4(2) . . . . ?
C12 C11 C10 C9 -55.2(2) . . . . ?
C15 C11 C10 C9 -173.69(17) . . . . ?
C7 C8 C9 O2 5.7(3) . . . . ?
C13 C8 C9 O2 -172.58(18) . . . . ?
C7 C8 C9 C10 -175.88(16) . . . . ?
C13 C8 C9 C10 5.9(3) . . . . ?
C11 C10 C9 O2 -153.42(18) . . . . ?
C11 C10 C9 C8 28.0(3) . . . . ?
C2 C1 C6 C5 0.8(2) . . . . ?
C7 C1 C6 C5 177.54(15) . . . . ?
C4 C5 C6 C1 -1.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 965964'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ly140306

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Cl N O4'
_chemical_formula_weight         419.84

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'
Cl Cl 0.1484 0.1585 '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                   10.6004(18)
_cell_length_b                   13.375(2)
_cell_length_c                   16.069(2)
_cell_angle_alpha                82.836(4)
_cell_angle_beta                 71.805(5)
_cell_angle_gamma                89.343(5)
_cell_volume                     2146.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4795
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      22.51

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18337
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.1125
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7560
_reflns_number_gt                3343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.1189P)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         7256
_refine_ls_number_parameters     543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1751
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2233
_refine_ls_wR_factor_gt          0.1928
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_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
Cl1 Cl 0.52158(18) 1.33983(13) -0.01231(10) 0.1283(7) Uani 1 1 d . . .
O1 O 0.7358(3) 1.21260(19) 0.41239(19) 0.0678(9) Uani 1 1 d . . .
O2 O 0.6389(3) 1.2647(2) 0.31511(19) 0.0729(9) Uani 1 1 d . . .
O3 O 0.6101(3) 0.92009(19) 0.43174(19) 0.0711(9) Uani 1 1 d . . .
O4 O 0.6210(4) 0.5411(3) 0.1846(3) 0.1030(12) Uani 1 1 d . . .
N1 N 0.5106(4) 0.9725(2) 0.3076(2) 0.0671(10) Uani 1 1 d . . .
H1 H 0.5135 0.9315 0.3526 0.080 Uiso 1 1 d R . .
C1 C 0.5613(4) 1.0638(3) 0.3001(3) 0.0527(11) Uani 1 1 d . . .
C2 C 0.6253(4) 1.0866(3) 0.3592(2) 0.0463(10) Uani 1 1 d . . .
C3 C 0.6643(4) 1.1925(3) 0.3575(3) 0.0552(11) Uani 1 1 d . . .
C4 C 0.7726(5) 1.1384(3) 0.4672(3) 0.0593(12) Uani 1 1 d . . .
C5 C 0.7317(4) 1.0388(3) 0.4751(3) 0.0551(11) Uani 1 1 d . . .
C6 C 0.6512(4) 1.0100(3) 0.4227(3) 0.0517(11) Uani 1 1 d . . .
C7 C 0.7726(5) 0.9687(4) 0.5328(3) 0.0726(14) Uani 1 1 d . . .
H7 H 0.7484 0.9010 0.5382 0.087 Uiso 1 1 calc R . .
C8 C 0.8469(5) 0.9980(4) 0.5810(3) 0.0852(16) Uani 1 1 d . . .
H8 H 0.8709 0.9507 0.6205 0.102 Uiso 1 1 calc R . .
C9 C 0.8877(6) 1.0991(5) 0.5715(3) 0.0848(15) Uani 1 1 d . . .
H9 H 0.9402 1.1183 0.6039 0.102 Uiso 1 1 calc R . .
C10 C 0.8512(5) 1.1696(4) 0.5153(3) 0.0760(14) Uani 1 1 d . . .
H10 H 0.8778 1.2369 0.5091 0.091 Uiso 1 1 calc R . .
C11 C 0.5498(4) 1.1357(3) 0.2237(3) 0.0464(10) Uani 1 1 d . . .
C12 C 0.6576(5) 1.1528(3) 0.1501(3) 0.0657(13) Uani 1 1 d . . .
H12 H 0.7370 1.1222 0.1495 0.079 Uiso 1 1 calc R . .
C13 C 0.6508(5) 1.2153(4) 0.0761(3) 0.0785(14) Uani 1 1 d . . .
H13 H 0.7245 1.2270 0.0259 0.094 Uiso 1 1 calc R . .
C14 C 0.5308(6) 1.2598(3) 0.0790(3) 0.0722(14) Uani 1 1 d . . .
C15 C 0.4218(5) 1.2435(3) 0.1532(3) 0.0653(13) Uani 1 1 d . . .
H15 H 0.3421 1.2743 0.1547 0.078 Uiso 1 1 calc R . .
C16 C 0.4324(5) 1.1808(3) 0.2254(3) 0.0606(12) Uani 1 1 d . . .
H16 H 0.3590 1.1690 0.2758 0.073 Uiso 1 1 calc R . .
C17 C 0.4464(5) 0.9314(3) 0.2504(3) 0.0779(15) Uani 1 1 d . . .
H17A H 0.4688 0.9742 0.1942 0.093 Uiso 1 1 calc R . .
H17B H 0.3508 0.9313 0.2774 0.093 Uiso 1 1 calc R . .
C18 C 0.4886(5) 0.8264(3) 0.2349(3) 0.0568(12) Uani 1 1 d . . .
C19 C 0.6148(5) 0.8093(4) 0.1868(3) 0.0794(15) Uani 1 1 d . . .
H19 H 0.6745 0.8636 0.1632 0.095 Uiso 1 1 calc R . .
C20 C 0.6569(5) 0.7134(4) 0.1721(3) 0.0821(15) Uani 1 1 d . . .
H20 H 0.7446 0.7034 0.1398 0.099 Uiso 1 1 calc R . .
C21 C 0.5702(5) 0.6336(3) 0.2047(3) 0.0604(12) Uani 1 1 d . . .
C22 C 0.4430(5) 0.6479(3) 0.2534(3) 0.0621(12) Uani 1 1 d . . .
H22 H 0.3829 0.5936 0.2756 0.075 Uiso 1 1 calc R . .
C23 C 0.4035(4) 0.7451(3) 0.2696(3) 0.0618(12) Uani 1 1 d . . .
H23 H 0.3174 0.7549 0.3049 0.074 Uiso 1 1 calc R . .
C24 C 0.5355(7) 0.4568(4) 0.2129(4) 0.125(3) Uani 1 1 d . . .
H24A H 0.4720 0.4612 0.1813 0.188 Uiso 1 1 calc R . .
H24B H 0.4899 0.4542 0.2750 0.188 Uiso 1 1 calc R . .
H24C H 0.5858 0.3970 0.2020 0.188 Uiso 1 1 calc R . .
Cl2 Cl 1.00377(14) 0.67638(11) 1.00960(8) 0.0916(5) Uani 1 1 d . . .
O5 O 0.7630(3) 0.68611(18) 0.58987(18) 0.0658(8) Uani 1 1 d . . .
O6 O 0.8575(3) 0.7052(2) 0.6890(2) 0.0757(10) Uani 1 1 d . . .
O7 O 0.8913(3) 0.39838(19) 0.56751(17) 0.0604(8) Uani 1 1 d . . .
O8 O 0.8679(5) -0.0535(3) 0.8195(3) 0.1386(17) Uani 1 1 d . . .
N2 N 0.9879(3) 0.4102(2) 0.6934(2) 0.0606(10) Uani 1 1 d . . .
H2 H 0.9791 0.3824 0.6500 0.073 Uiso 1 1 d R . .
C25 C 0.9395(4) 0.5001(3) 0.7014(2) 0.0485(10) Uani 1 1 d . . .
C26 C 0.8727(4) 0.5426(3) 0.6423(2) 0.0440(10) Uani 1 1 d . . .
C27 C 0.8341(4) 0.6474(3) 0.6446(3) 0.0559(11) Uani 1 1 d . . .
C28 C 0.7279(4) 0.6295(3) 0.5346(3) 0.0550(11) Uani 1 1 d . . .
C29 C 0.7680(4) 0.5322(3) 0.5255(2) 0.0480(10) Uani 1 1 d . . .
C30 C 0.8490(4) 0.4860(3) 0.5780(2) 0.0497(11) Uani 1 1 d . . .
C31 C 0.7287(4) 0.4800(3) 0.4678(3) 0.0594(12) Uani 1 1 d . . .
H31 H 0.7549 0.4141 0.4612 0.071 Uiso 1 1 calc R . .
C32 C 0.6509(5) 0.5255(4) 0.4204(3) 0.0753(14) Uani 1 1 d . . .
H32 H 0.6238 0.4901 0.3823 0.090 Uiso 1 1 calc R . .
C33 C 0.6134(5) 0.6238(4) 0.4294(3) 0.0777(14) Uani 1 1 d . . .
H33 H 0.5628 0.6545 0.3960 0.093 Uiso 1 1 calc R . .
C34 C 0.6491(5) 0.6775(3) 0.4869(3) 0.0692(13) Uani 1 1 d . . .
H34 H 0.6219 0.7431 0.4937 0.083 Uiso 1 1 calc R . .
C35 C 0.9524(4) 0.5482(3) 0.7771(2) 0.0459(10) Uani 1 1 d . . .
C36 C 0.8496(4) 0.5422(3) 0.8558(3) 0.0584(11) Uani 1 1 d . . .
H36 H 0.7697 0.5107 0.8600 0.070 Uiso 1 1 calc R . .
C37 C 0.8620(5) 0.5810(3) 0.9272(3) 0.0598(12) Uani 1 1 d . . .
H37 H 0.7914 0.5774 0.9794 0.072 Uiso 1 1 calc R . .
C38 C 0.9816(5) 0.6259(3) 0.9203(3) 0.0546(11) Uani 1 1 d . . .
C39 C 1.0850(4) 0.6338(3) 0.8430(3) 0.0577(11) Uani 1 1 d . . .
H39 H 1.1643 0.6660 0.8391 0.069 Uiso 1 1 calc R . .
C40 C 1.0716(5) 0.5942(3) 0.7717(3) 0.0569(11) Uani 1 1 d . . .
H40 H 1.1424 0.5982 0.7195 0.068 Uiso 1 1 calc R . .
C41 C 1.0555(5) 0.3513(3) 0.7498(3) 0.0644(12) Uani 1 1 d . . .
H41A H 1.0375 0.3792 0.8051 0.077 Uiso 1 1 calc R . .
H41B H 1.1507 0.3553 0.7206 0.077 Uiso 1 1 calc R . .
C42 C 1.0078(5) 0.2424(3) 0.7681(3) 0.0537(11) Uani 1 1 d . . .
C43 C 1.0925(5) 0.1679(4) 0.7352(3) 0.0739(14) Uani 1 1 d . . .
H43 H 1.1798 0.1853 0.7015 0.089 Uiso 1 1 calc R . .
C44 C 1.0508(6) 0.0679(4) 0.7511(4) 0.0837(16) Uani 1 1 d . . .
H44 H 1.1090 0.0183 0.7284 0.100 Uiso 1 1 calc R . .
C45 C 0.9231(7) 0.0434(3) 0.8004(4) 0.0818(16) Uani 1 1 d . . .
C46 C 0.8344(5) 0.1180(4) 0.8351(3) 0.0850(15) Uani 1 1 d . . .
H46 H 0.7473 0.1008 0.8694 0.102 Uiso 1 1 calc R . .
C47 C 0.8786(5) 0.2162(3) 0.8176(3) 0.0636(12) Uani 1 1 d . . .
H47 H 0.8205 0.2662 0.8396 0.076 Uiso 1 1 calc R . .
C48 C 0.9535(8) -0.1346(4) 0.7948(6) 0.176(4) Uani 1 1 d . . .
H48A H 0.9877 -0.1294 0.7315 0.263 Uiso 1 1 calc R . .
H48B H 0.9048 -0.1974 0.8176 0.263 Uiso 1 1 calc R . .
H48C H 1.0258 -0.1318 0.8185 0.263 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 C14 1.734(5) . ?
O1 C4 1.379(5) . ?
O1 C3 1.381(5) . ?
O2 C3 1.189(4) . ?
O3 C6 1.260(4) . ?
O4 C21 1.378(5) . ?
O4 C24 1.392(6) . ?
N1 C1 1.316(5) . ?
N1 C17 1.461(5) . ?
N1 H1 0.8600 . ?
C1 C2 1.391(5) . ?
C1 C11 1.496(5) . ?
C2 C6 1.441(5) . ?
C2 C3 1.474(5) . ?
C4 C5 1.384(6) . ?
C4 C10 1.399(6) . ?
C5 C7 1.396(6) . ?
C5 C6 1.456(6) . ?
C7 C8 1.356(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.400(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.360(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.360(5) . ?
C11 C16 1.372(5) . ?
C12 C13 1.387(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.372(6) . ?
C15 C16 1.377(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.496(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.353(6) . ?
C18 C23 1.365(6) . ?
C19 C20 1.377(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.357(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.357(6) . ?
C22 C23 1.391(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
Cl2 C38 1.740(4) . ?
O5 C28 1.372(5) . ?
O5 C27 1.378(5) . ?
O6 C27 1.192(4) . ?
O7 C30 1.262(4) . ?
O8 C45 1.387(6) . ?
O8 C48 1.420(7) . ?
N2 C25 1.308(4) . ?
N2 C41 1.473(5) . ?
N2 H2 0.8601 . ?
C25 C26 1.414(5) . ?
C25 C35 1.488(5) . ?
C26 C30 1.438(5) . ?
C26 C27 1.458(5) . ?
C28 C29 1.375(5) . ?
C28 C34 1.401(6) . ?
C29 C31 1.389(5) . ?
C29 C30 1.463(5) . ?
C31 C32 1.377(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.382(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.378(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.382(5) . ?
C35 C40 1.385(5) . ?
C36 C37 1.360(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.376(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.369(5) . ?
C39 C40 1.368(5) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.510(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C47 1.375(6) . ?
C42 C43 1.376(6) . ?
C43 C44 1.381(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.358(7) . ?
C44 H44 0.9300 . ?
C45 C46 1.407(7) . ?
C46 C47 1.365(6) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 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
C4 O1 C3 122.9(3) . . ?
C21 O4 C24 118.3(5) . . ?
C1 N1 C17 128.6(4) . . ?
C1 N1 H1 116.5 . . ?
C17 N1 H1 114.9 . . ?
N1 C1 C2 119.7(4) . . ?
N1 C1 C11 115.9(4) . . ?
C2 C1 C11 124.4(4) . . ?
C1 C2 C6 121.7(3) . . ?
C1 C2 C3 118.6(4) . . ?
C6 C2 C3 119.7(4) . . ?
O2 C3 O1 114.8(4) . . ?
O2 C3 C2 127.5(4) . . ?
O1 C3 C2 117.7(4) . . ?
O1 C4 C5 121.5(4) . . ?
O1 C4 C10 116.4(4) . . ?
C5 C4 C10 122.1(4) . . ?
C4 C5 C7 117.7(4) . . ?
C4 C5 C6 119.9(4) . . ?
C7 C5 C6 122.4(4) . . ?
O3 C6 C2 122.0(4) . . ?
O3 C6 C5 120.1(4) . . ?
C2 C6 C5 117.8(4) . . ?
C8 C7 C5 120.9(5) . . ?
C8 C7 H7 119.5 . . ?
C5 C7 H7 119.5 . . ?
C7 C8 C9 120.3(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C4 118.4(4) . . ?
C9 C10 H10 120.8 . . ?
C4 C10 H10 120.8 . . ?
C12 C11 C16 119.8(4) . . ?
C12 C11 C1 118.6(4) . . ?
C16 C11 C1 121.5(4) . . ?
C11 C12 C13 121.0(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 118.2(4) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C15 C14 C13 121.2(4) . . ?
C15 C14 Cl1 120.0(4) . . ?
C13 C14 Cl1 118.7(4) . . ?
C14 C15 C16 118.9(4) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C11 C16 C15 120.8(4) . . ?
C11 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
N1 C17 C18 111.7(3) . . ?
N1 C17 H17A 109.3 . . ?
C18 C17 H17A 109.3 . . ?
N1 C17 H17B 109.3 . . ?
C18 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C23 117.9(4) . . ?
C19 C18 C17 120.2(4) . . ?
C23 C18 C17 121.9(5) . . ?
C18 C19 C20 121.6(4) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C19 119.9(5) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.1(4) . . ?
C20 C21 O4 115.5(5) . . ?
C22 C21 O4 124.4(5) . . ?
C21 C22 C23 119.0(4) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C18 C23 C22 121.4(4) . . ?
C18 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 O5 C27 122.3(3) . . ?
C45 O8 C48 118.2(5) . . ?
C25 N2 C41 127.7(3) . . ?
C25 N2 H2 115.8 . . ?
C41 N2 H2 116.5 . . ?
N2 C25 C26 119.2(3) . . ?
N2 C25 C35 116.2(3) . . ?
C26 C25 C35 124.5(3) . . ?
C25 C26 C30 121.2(3) . . ?
C25 C26 C27 118.6(3) . . ?
C30 C26 C27 120.1(4) . . ?
O6 C27 O5 115.0(4) . . ?
O6 C27 C26 127.1(4) . . ?
O5 C27 C26 117.9(4) . . ?
O5 C28 C29 122.6(4) . . ?
O5 C28 C34 115.7(4) . . ?
C29 C28 C34 121.8(4) . . ?
C28 C29 C31 119.1(4) . . ?
C28 C29 C30 119.0(4) . . ?
C31 C29 C30 121.8(4) . . ?
O7 C30 C26 122.8(4) . . ?
O7 C30 C29 119.7(3) . . ?
C26 C30 C29 117.4(3) . . ?
C32 C31 C29 120.2(4) . . ?
C32 C31 H31 119.9 . . ?
C29 C31 H31 119.9 . . ?
C31 C32 C33 119.8(4) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 121.6(4) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C33 C34 C28 117.6(4) . . ?
C33 C34 H34 121.2 . . ?
C28 C34 H34 121.2 . . ?
C36 C35 C40 118.7(4) . . ?
C36 C35 C25 121.0(4) . . ?
C40 C35 C25 120.2(4) . . ?
C37 C36 C35 121.8(4) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C36 C37 C38 118.3(4) . . ?
C36 C37 H37 120.9 . . ?
C38 C37 H37 120.9 . . ?
C39 C38 C37 121.2(4) . . ?
C39 C38 Cl2 118.3(4) . . ?
C37 C38 Cl2 120.4(3) . . ?
C38 C39 C40 119.9(4) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 C35 119.9(4) . . ?
C39 C40 H40 120.0 . . ?
C35 C40 H40 120.0 . . ?
N2 C41 C42 110.3(3) . . ?
N2 C41 H41A 109.6 . . ?
C42 C41 H41A 109.6 . . ?
N2 C41 H41B 109.6 . . ?
C42 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C47 C42 C43 119.0(4) . . ?
C47 C42 C41 120.4(4) . . ?
C43 C42 C41 120.6(4) . . ?
C42 C43 C44 121.5(5) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C45 C44 C43 118.7(5) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C44 C45 O8 124.5(6) . . ?
C44 C45 C46 121.0(4) . . ?
O8 C45 C46 114.5(6) . . ?
C47 C46 C45 118.8(5) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
C46 C47 C42 121.0(4) . . ?
C46 C47 H47 119.5 . . ?
C42 C47 H47 119.5 . . ?
O8 C48 H48A 109.5 . . ?
O8 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O8 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 990835'
