Electronic Supplementary Material for CrystEngComm
This Journal is (c) The Royal Society of Chemistry 2006

data_global

_journal_name_full               Chem.Commun.
_journal_coden_Cambridge         0182
#=======================================================================
# start Validation Reply Form
#=======================================================================

_vrf_ATOM007_06isis018_h         
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: isotropic atom refinement only, due to level of diorder in
system
;
#=======================================================================
# end Validation Reply Form
#=======================================================================

_publ_contact_author_name        'Alastair J. Florence'
_publ_contact_author_email       alastair.florence@strath.ac.uk
_publ_contact_author_fax         '+44 (0)141 552 6443'
_publ_contact_author_phone       '+44 (0)141 548 4877'
_publ_contact_author_address     
; Solid-State Research Group,
Department of Pharmaceutical Sciences,
University of Strathclyde,
27 Taylor St,
Glasgow G4 0NR
United Kingdom
;

loop_
_publ_author_name
_publ_author_address
A.J.Florence
; Solid-State Research Group
Pharmaceutical Sciences
University of Strathclyde,
27 Taylor St,
Glasgow G4 0NR
United Kingdom
;
C.K.Broder
; ISIS Facility
Rutherford Appleton Laboratory
Chilton, Didcot
Oxon, OX11 0QX
United Kingdom
;
N.Shankland
; Solid-State Research Group
Pharmaceutical Sciences
University of Strathclyde,
27 Taylor St,
Glasgow G4 0NR
United Kingdom
;
K.Shankland
; ISIS Facility
Rutherford Appleton Laboratory
Chilton, Didcot
Oxon, OX11 0QX
United Kingdom
;
A.Johnston
; Solid-State Research Group
Pharmaceutical Sciences
University of Strathclyde,
27 Taylor St,
Glasgow G4 0NR
United Kingdom
;
#=======================================================================
#data_06isis018_h
#=======================================================================

data_06isis018_h
_database_code_depnum_ccdc_archive 'CCDC 609185'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
5H-dibenz[b,f]azepine-5-carboxamide 10,11-dihydro-5H-dibenz[b,f]azepine-
5-carboxamide (1/1)
;
_chemical_name_common            
;
5H-dibenz(b,f)azepine-5-carboxamide 10,11-dihydro-5H-
dibenz(b,f)azepine-5-carboxamide (1/1)
;
_chemical_melting_point          ?
_chemical_formula_moiety         '0.5(C15 H12 N2 O1), 0.5(C15 H14 N2 O1)'
_chemical_formula_sum            'C15 H13 N2 O'
_chemical_formula_weight         237.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   9.088(2)
_cell_length_b                   10.425(4)
_cell_length_c                   25.005(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2369.0(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1608
_cell_measurement_theta_min      3.5323
_cell_measurement_theta_max      73.4341

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_exptl_crystal_preparation       'crystallised from MeOH solution'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 15.9745
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12425
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         74.42
_reflns_number_total             2368
_reflns_number_gt                1400
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Structure solution using direct methods resulted in a structure (Av)
that was an average between the known molecular structure of
carbamazapine(CBZ) and dihydrocarbamazapine (DHCBZ), characterised
by a C7-C8 bond length of 1.45 rather than the expected double bond
for CBZ or single bond for DHCBZ. This average structure (Av) exhibited
unusully large anisotropic displacement parameters. Generation of a
fourier difference map from this data dataset with the model for
DHCBZ form II, which has almost identical unit cell
dimentions, produced peaks of residual electron density in the CBZ moiety
position. The final disorded model was obtained by the refinement of
the DHCBZ form II model and the averaged structure model Av as a 50:50
system this resulted in the average structure model Av refining to the
CBZ molecular structure as defined by a C7-C8 bond lenght of 1.36(1)
with the corrisponding bond in the DHCBZ moiety equal to 1.52(1).
A free refinement of the CBZ to DHCBZ ratio gave 0.48 so the ratio was
fixed to be 0.5 in the final refinement. When either the CBZ moiety or
the DHCBZ moiety was removed from the disordered structure the remaining
moiety refined to the average structure Av coordinates. but when both
moietys were present in the model the refinement remained stable.
Constraints have been used to fix the hydrogen atoms to geometrically
sencible positions and to reduce the number of parameters required
to define the aromatic rings. Without these constraints a chemically
resonable refinable model was obtained but the data to parameter ratio
was low.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR
and goodness of fit S are based on F^2^, conventional R-factors R are
based on F, with F set to zero for negative F^2^. The threshold
expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt)
etc. and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large as
those based on F, and R-factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2368
_refine_ls_number_parameters     145
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_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
O1 O 0.1556(7) 0.8281(6) 0.4636(2) 0.0329(17) Uiso 0.50 1 d P A 1
N2 N -0.0723(10) 0.7643(8) 0.4915(3) 0.035(2) Uiso 0.50 1 d P A 1
H2A H -0.1681 0.7601 0.4866 0.052 Uiso 0.50 1 calc PR A 1
H2C H -0.0321 0.7268 0.5194 0.052 Uiso 0.50 1 calc PR A 1
N1 N -0.0337(12) 0.8856(12) 0.4145(5) 0.047(4) Uiso 0.50 1 d P A 1
C1 C 0.0424(13) 0.9389(12) 0.3709(4) 0.039(4) Uiso 0.50 1 d P A 1
C2 C 0.1356(17) 1.0447(17) 0.3838(5) 0.054(5) Uiso 0.50 1 d P A 1
H2 H 0.1356 1.0800 0.4189 0.065 Uiso 0.50 1 calc PR A 1
C3 C 0.2278(9) 1.0957(9) 0.3437(3) 0.040(2) Uiso 0.50 1 d P A 1
H3 H 0.2902 1.1667 0.3510 0.048 Uiso 0.50 1 calc PR A 1
C4 C 0.2253(9) 1.0393(8) 0.2927(3) 0.046(2) Uiso 0.50 1 d P A 1
H4 H 0.2852 1.0722 0.2648 0.055 Uiso 0.50 1 calc PR A 1
C5 C 0.1374(9) 0.9386(8) 0.2840(3) 0.050(2) Uiso 0.50 1 d P A 1
H5 H 0.1420 0.8996 0.2496 0.059 Uiso 0.50 1 calc PR A 1
C6 C 0.0389(13) 0.8854(10) 0.3212(5) 0.044(3) Uiso 0.50 1 d P A 1
C7 C -0.0466(8) 0.7730(8) 0.3098(3) 0.0449(19) Uiso 0.50 1 d P A 1
H7 H -0.0060 0.7153 0.2843 0.054 Uiso 0.50 1 calc PR A 1
C8 C -0.1791(9) 0.7391(9) 0.3310(3) 0.050(2) Uiso 0.50 1 d P A 1
H8 H -0.2165 0.6582 0.3201 0.059 Uiso 0.50 1 calc PR A 1
C9 C -0.2722(11) 0.8121(10) 0.3690(4) 0.039(3) Uiso 0.50 1 d P A 1
C10 C -0.2111(11) 0.8906(11) 0.4059(4) 0.029(3) Uiso 0.50 1 d P A 1
C11 C -0.3009(11) 0.9734(10) 0.4363(4) 0.030(3) Uiso 0.50 1 d P A 1
H11 H -0.2650 1.0295 0.4633 0.036 Uiso 0.50 1 calc PR A 1
C12 C -0.4462(12) 0.9632(11) 0.4223(4) 0.047(3) Uiso 0.50 1 d P A 1
H12 H -0.5154 1.0187 0.4390 0.056 Uiso 0.50 1 calc PR A 1
C13 C -0.4963(10) 0.8758(8) 0.3851(3) 0.039(2) Uiso 0.50 1 d P A 1
H13 H -0.5984 0.8706 0.3773 0.047 Uiso 0.50 1 calc PR A 1
C14 C -0.3978(9) 0.7954(9) 0.3591(3) 0.037(3) Uiso 0.50 1 d P A 1
H14 H -0.4295 0.7309 0.3349 0.044 Uiso 0.50 1 calc PR A 1
C15 C 0.0090(11) 0.8252(12) 0.4577(4) 0.042(4) Uiso 0.50 1 d P A 1
O1B O 0.1564(8) 0.8054(6) 0.4585(3) 0.039(2) Uiso 0.50 1 d P B 2
N1B N -0.0505(9) 0.8926(9) 0.4152(3) 0.020(2) Uiso 0.50 1 d P B 2
N2B N -0.0683(9) 0.7845(7) 0.4962(3) 0.034(2) Uiso 0.50 1 d P B 2
H2D H -0.0369 0.7410 0.5241 0.051 Uiso 0.50 1 calc PR B 2
H2E H -0.1624 0.8025 0.4928 0.051 Uiso 0.50 1 calc PR B 2
C1B C 0.0507(10) 0.9493(10) 0.3767(4) 0.025(3) Uiso 0.50 1 d P B 2
C2B C 0.1429(11) 1.0469(11) 0.3895(4) 0.026(3) Uiso 0.50 1 d P B 2
H2B H 0.1468 1.0726 0.4259 0.031 Uiso 0.50 1 calc PR B 2
C3B C 0.2289(9) 1.1100(8) 0.3548(3) 0.036(2) Uiso 0.50 1 d P B 2
H3B H 0.2930 1.1762 0.3665 0.043 Uiso 0.50 1 calc PR B 2
C4B C 0.2217(7) 1.0758(7) 0.3009(3) 0.0325(16) Uiso 0.50 1 d P B 2
H4B H 0.2820 1.1189 0.2756 0.039 Uiso 0.50 1 calc PR B 2
C5B C 0.1263(8) 0.9783(7) 0.2836(3) 0.0357(17) Uiso 0.50 1 d P B 2
H5B H 0.1180 0.9585 0.2467 0.043 Uiso 0.50 1 calc PR B 2
C6B C 0.0425(10) 0.9097(10) 0.3219(4) 0.031(3) Uiso 0.50 1 d P B 2
C7B C -0.0567(7) 0.8026(7) 0.2979(2) 0.0345(15) Uiso 0.50 1 d P B 2
H7B H -0.1270 0.8435 0.2729 0.041 Uiso 0.50 1 calc PR B 2
H7C H 0.0066 0.7448 0.2765 0.041 Uiso 0.50 1 calc PR B 2
C8B C -0.1443(8) 0.7205(7) 0.3368(3) 0.0338(16) Uiso 0.50 1 d PD B 2
H8B H -0.2005 0.6546 0.3170 0.041 Uiso 0.50 1 calc PR B 2
H8C H -0.0764 0.6763 0.3617 0.041 Uiso 0.50 1 calc PR B 2
C9B C -0.2473(9) 0.8036(9) 0.3676(3) 0.027(2) Uiso 0.50 1 d PD B 2
C10B C -0.1886(11) 0.8904(11) 0.4074(4) 0.030(3) Uiso 0.50 1 d P B 2
C11B C -0.2774(11) 0.9718(12) 0.4350(4) 0.042(3) Uiso 0.50 1 d P B 2
H11B H -0.2318 1.0309 0.4587 0.050 Uiso 0.50 1 calc PR B 2
C12B C -0.4358(9) 0.9750(9) 0.4309(3) 0.033(2) Uiso 0.50 1 d P B 2
H12B H -0.4917 1.0316 0.4527 0.039 Uiso 0.50 1 calc PR B 2
C13B C -0.5049(9) 0.8946(8) 0.3949(3) 0.033(2) Uiso 0.50 1 d P B 2
H13B H -0.6091 0.8948 0.3919 0.039 Uiso 0.50 1 calc PR B 2
C14B C -0.4210(9) 0.8137(9) 0.3632(3) 0.034(2) Uiso 0.50 1 d P B 2
H14B H -0.4700 0.7617 0.3376 0.041 Uiso 0.50 1 calc PR B 2
C15B C 0.0317(9) 0.8252(9) 0.4570(3) 0.020(2) Uiso 0.50 1 d P B 2

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s.
planes) are estimated using the full covariance matrix. The cell
esds are taken into account individually in the estimation of esds in
distances, angles and torsion angles; correlations between esds in
cell parameters are only used when they are defined by crystal
symmetry. An approximate (isotropic) treatment of cell esds is used
for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C15 1.341(12) . ?
N2 C15 1.289(14) . ?
N2 H2A 0.8800 . ?
N2 H2C 0.8800 . ?
N1 C15 1.309(15) . ?
N1 C1 1.406(16) . ?
N1 C10 1.627(15) . ?
C1 C6 1.364(15) . ?
C1 C2 1.43(2) . ?
C2 C3 1.412(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.405(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.337(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.434(13) . ?
C7 C8 1.362(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.482(12) . ?
C8 H8 0.9500 . ?
C9 C14 1.180(12) . ?
C9 C10 1.353(14) . ?
C10 C11 1.411(14) . ?
C11 C12 1.370(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(12) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
O1B C15B 1.152(11) . ?
N1B C10B 1.270(13) . ?
N1B C1B 1.457(12) . ?
N1B C15B 1.465(11) . ?
N2B C15B 1.401(12) . ?
N2B H2D 0.8800 . ?
N2B H2E 0.8800 . ?
C1B C2B 1.357(17) . ?
C1B C6B 1.433(13) . ?
C2B C3B 1.340(14) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.395(9) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.404(10) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.416(12) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.556(12) . ?
C7B C8B 1.521(9) . ?
C7B H7B 0.9900 . ?
C7B H7C 0.9900 . ?
C8B C9B 1.489(9) . ?
C8B H8B 0.9900 . ?
C8B H8C 0.9900 . ?
C9B C10B 1.447(13) . ?
C9B C14B 1.586(12) . ?
C10B C11B 1.360(15) . ?
C11B C12B 1.444(13) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.381(12) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.387(12) . ?
C13B H13B 0.9500 . ?
C14B H14B 0.9500 . ?

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
C15 N2 H2A 120.0 . . ?
C15 N2 H2C 120.0 . . ?
H2A N2 H2C 120.0 . . ?
C15 N1 C1 133.2(11) . . ?
C15 N1 C10 114.7(10) . . ?
C1 N1 C10 111.8(9) . . ?
C6 C1 N1 122.3(11) . . ?
C6 C1 C2 122.5(12) . . ?
N1 C1 C2 114.9(11) . . ?
C3 C2 C1 118.8(11) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C4 C3 C2 118.5(10) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 119.2(8) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 125.6(9) . . ?
C4 C5 H5 117.2 . . ?
C6 C5 H5 117.2 . . ?
C1 C6 C5 115.3(10) . . ?
C1 C6 C7 121.9(10) . . ?
C5 C6 C7 122.4(9) . . ?
C8 C7 C6 127.8(8) . . ?
C8 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C7 C8 C9 128.4(8) . . ?
C7 C8 H8 115.8 . . ?
C9 C8 H8 115.8 . . ?
C14 C9 C10 128.9(10) . . ?
C14 C9 C8 110.1(9) . . ?
C10 C9 C8 120.8(9) . . ?
C9 C10 C11 120.0(9) . . ?
C9 C10 N1 118.5(9) . . ?
C11 C10 N1 121.4(9) . . ?
C12 C11 C10 111.8(9) . . ?
C12 C11 H11 124.1 . . ?
C10 C11 H11 124.1 . . ?
C11 C12 C13 122.8(10) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C14 120.1(9) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C9 C14 C13 115.9(9) . . ?
C9 C14 H14 122.1 . . ?
C13 C14 H14 122.1 . . ?
N2 C15 N1 127.4(11) . . ?
N2 C15 O1 120.6(10) . . ?
N1 C15 O1 112.0(10) . . ?
C10B N1B C1B 122.0(8) . . ?
C10B N1B C15B 127.2(8) . . ?
C1B N1B C15B 110.2(7) . . ?
C15B N2B H2D 120.0 . . ?
C15B N2B H2E 120.0 . . ?
H2D N2B H2E 120.0 . . ?
C2B C1B C6B 118.3(9) . . ?
C2B C1B N1B 122.5(9) . . ?
C6B C1B N1B 118.9(9) . . ?
C3B C2B C1B 125.1(10) . . ?
C3B C2B H2B 117.4 . . ?
C1B C2B H2B 117.4 . . ?
C2B C3B C4B 118.2(9) . . ?
C2B C3B H3B 120.9 . . ?
C4B C3B H3B 120.9 . . ?
C3B C4B C5B 120.7(7) . . ?
C3B C4B H4B 119.6 . . ?
C5B C4B H4B 119.6 . . ?
C4B C5B C6B 119.3(7) . . ?
C4B C5B H5B 120.3 . . ?
C6B C5B H5B 120.3 . . ?
C5B C6B C1B 118.2(9) . . ?
C5B C6B C7B 114.4(7) . . ?
C1B C6B C7B 127.3(8) . . ?
C8B C7B C6B 117.4(6) . . ?
C8B C7B H7B 108.0 . . ?
C6B C7B H7B 108.0 . . ?
C8B C7B H7C 108.0 . . ?
C6B C7B H7C 108.0 . . ?
H7B C7B H7C 107.2 . . ?
C9B C8B C7B 109.4(6) . . ?
C9B C8B H8B 109.8 . . ?
C7B C8B H8B 109.8 . . ?
C9B C8B H8C 109.8 . . ?
C7B C8B H8C 109.8 . . ?
H8B C8B H8C 108.2 . . ?
C10B C9B C8B 119.1(8) . . ?
C10B C9B C14B 111.9(7) . . ?
C8B C9B C14B 129.0(7) . . ?
N1B C10B C11B 119.8(10) . . ?
N1B C10B C9B 118.8(9) . . ?
C11B C10B C9B 121.4(10) . . ?
C10B C11B C12B 124.8(11) . . ?
C10B C11B H11B 117.6 . . ?
C12B C11B H11B 117.6 . . ?
C13B C12B C11B 119.0(9) . . ?
C13B C12B H12B 120.5 . . ?
C11B C12B H12B 120.5 . . ?
C12B C13B C14B 119.5(8) . . ?
C12B C13B H13B 120.3 . . ?
C14B C13B H13B 120.3 . . ?
C13B C14B C9B 123.3(7) . . ?
C13B C14B H14B 118.4 . . ?
C9B C14B H14B 118.4 . . ?
O1B C15B N2B 124.1(8) . . ?
O1B C15B N1B 127.7(8) . . ?
N2B C15B N1B 108.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        74.42
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.046


