#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/73/2007303.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007303
loop_
_publ_author_name
'Luccioni-Houzé, Barbara'
'Giusti, Gerard'
'Pèpe, Gérard'
_publ_section_title
;5'-[2-(N-tert-Butylethanal
 nitrone)]-1,3,3-trimethylspiro[indoline-2,3'-naphtho[2,1-b][1,4]oxazine]
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              824
_journal_page_last               825
_journal_paper_doi               10.1107/S0108270197012882
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C27 H29 N3 O2'
_chemical_formula_sum            'C27 H29 N3 O2'
_chemical_formula_weight         427.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 98.57(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5800(10)
_cell_length_b                   13.901(2)
_cell_length_c                   19.977(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      5
_cell_volume                     2356.1(6)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1977)'
_computing_data_reduction        'DATARED (Pèpe, 1979)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.1446
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4732
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        'none; variation <3%'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pseudo-hexagonal prism'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.09
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.923
_refine_ls_goodness_of_fit_obs   0.991
_refine_ls_hydrogen_treatment
'H atoms refined with fixed values for  d = 1\%A and U = 0.05\%A^2^'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.936
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_obs          .036
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0036P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.066
_refine_ls_wR_factor_obs         .065
_reflns_number_observed          2038
_reflns_number_total             4732
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1178.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0036P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0036P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2007303
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'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
C1 -.1152(2) .4124(2) .43312(11) .0409(6) Uani d . 1 . C
C2 -.1903(2) .4201(2) .49165(12) .0493(6) Uani d D 1 . C
C3 -.2879(2) .5005(2) .4965(2) .0587(8) Uani d D 1 . C
C4 -.3083(2) .5709(2) .44689(15) .0586(7) Uani d D 1 . C
C5 -.2368(2) .5650(2) .39080(13) .0492(6) Uani d D 1 . C
C6 -.1411(2) .4830(2) .38257(11) .0388(5) Uani d . 1 . C
C7 -.0653(2) .4727(2) .32262(11) .0395(6) Uani d . 1 . C
C8 .0252(2) .3931(2) .31827(11) .0367(5) Uani d . 1 . C
C9 .0608(2) .3249(2) .36991(11) .0390(5) Uani d . 1 . C
C10 -.0132(2) .3336(2) .42771(12) .0431(6) Uani d D 1 . C
C11 .1887(2) .2580(2) .36269(12) .0376(5) Uani d D 1 . C
N12 .2557(2) .20047(13) .40862(10) .0430(5) Uani d . 1 . N
O13 .2101(2) .18476(14) .46564(8) .0654(5) Uani d . 1 . O
C14 .4098(2) .1477(2) .40018(12) .0460(6) Uani d . 1 . C
C15 .4485(3) .1602(2) .32924(14) .0590(7) Uani d D 1 . C
C16 .5353(3) .1930(3) .4545(2) .0833(11) Uani d D 1 . C
C17 .3848(3) .0456(2) .4160(2) .0695(8) Uani d D 1 . C
O18 .08515(13) .37693(10) .25964(7) .0415(4) Uani d . 1 . O
C19 .1159(2) .4590(2) .21862(11) .0385(5) Uani d . 1 . C
C20 -.0089(2) .5332(2) .22224(12) .0452(6) Uani d D 1 . C
N21 -.0893(2) .54141(15) .27286(10) .0511(5) Uani d . 1 . N
N22 .2742(2) .49573(14) .24297(10) .0469(5) Uani d . 1 . N
C23 .3751(2) .4307(2) .21629(11) .0407(6) Uani d . 1 . C
C24 .3013(2) .3842(2) .16233(11) .0385(5) Uani d . 1 . C
C25 .1285(2) .4195(2) .14894(11) .0429(6) Uani d . 1 . C
C26 .0083(2) .3389(2) .12413(13) .0594(8) Uani d D 1 . C
C27 .1171(3) .5009(2) .09444(14) .0583(7) Uani d D 1 . C
C28 .3146(3) .5343(2) .3102(2) .0617(8) Uani d D 1 . C
C29 .5382(2) .4109(2) .24416(13) .0499(6) Uani d D 1 . C
C30 .6117(2) .3445(2) .20806(15) .0590(8) Uani d D 1 . C
C31 .5383(2) .2992(2) .15217(14) .0538(7) Uani d D 1 . C
C32 .3751(2) .3184(2) .12709(13) .0484(6) Uani d D 1 . C
H2 -.170(2) .3585(14) .5223(10) .050 Uiso d D 1 . H
H3 -.326(2) .5167(15) .5378(10) .050 Uiso d D 1 . H
H4 -.353(2) .6322(14) .4625(10) .050 Uiso d D 1 . H
H5 -.241(2) .6207(14) .3555(10) .050 Uiso d D 1 . H
H10 .011(2) .2833(14) .4629(10) .050 Uiso d D 1 . H
H11 .221(2) .2727(14) .3177(10) .050 Uiso d D 1 . H
H151 .362(2) .1501(15) .2923(10) .050 Uiso d D 1 . H
H152 .468(2) .2348(14) .3087(10) .050 Uiso d D 1 . H
H153 .543(2) .1103(14) .3193(10) .050 Uiso d D 1 . H
H161 .547(2) .2590(14) .4375(11) .050 Uiso d D 1 . H
H162 .526(2) .2001(16) .5007(10) .050 Uiso d D 1 . H
H163 .620(2) .1499(14) .4553(10) .050 Uiso d D 1 . H
H171 .344(2) .0416(14) .4671(9) .050 Uiso d D 1 . H
H172 .295(2) .0083(14) .3764(10) .050 Uiso d D 1 . H
H173 .491(2) .0043(14) .4115(9) .050 Uiso d D 1 . H
H20 -.018(2) .5801(14) .1790(10) .050 Uiso d D 1 . H
H261 -.003(2) .2771(14) .1642(10) .050 Uiso d D 1 . H
H262 -.110(2) .3747(14) .1235(9) .050 Uiso d D 1 . H
H263 .011(2) .3278(15) .0780(10) .050 Uiso d D 1 . H
H271 .008(2) .5365(14) .0747(9) .050 Uiso d D 1 . H
H272 .179(2) .5623(14) .1175(10) .050 Uiso d D 1 . H
H273 .121(2) .4663(14) .0440(10) .050 Uiso d D 1 . H
H281 .227(2) .5824(14) .3243(10) .050 Uiso d D 1 . H
H282 .318(2) .4784(15) .3360(11) .050 Uiso d D 1 . H
H283 .377(2) .5923(14) .2988(10) .050 Uiso d D 1 . H
H29 .591(2) .4539(14) .2888(10) .050 Uiso d D 1 . H
H30 .708(2) .3207(14) .2409(9) .050 Uiso d D 1 . H
H31 .575(2) .2496(14) .1233(10) .050 Uiso d D 1 . H
H32 .363(2) .2774(15) .0875(10) .050 Uiso d D 1 . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C10 121.3(2) ?
C6 C1 C2 119.9(2) ?
C10 C1 C2 118.8(2) ?
C3 C2 C1 117.6(2) ?
C2 C3 C4 121.6(2) ?
C5 C4 C3 121.6(2) ?
C4 C5 C6 118.8(2) ?
C1 C6 C5 120.5(2) ?
C1 C6 C7 118.9(2) ?
C5 C6 C7 120.6(2) ?
C8 C7 N21 123.0(2) yes
C8 C7 C6 117.5(2) ?
N21 C7 C6 119.5(2) ?
C7 C8 O18 118.6(2) yes
C7 C8 C9 124.5(2) ?
O18 C8 C9 116.8(2) ?
C10 C9 C8 118.2(2) ?
C10 C9 C11 125.0(2) ?
C8 C9 C11 116.3(2) ?
C9 C10 C1 119.3(2) ?
N12 C11 C9 126.0(2) ?
O13 N12 C11 125.3(2) yes
O13 N12 C14 113.4(2) yes
C11 N12 C14 121.2(2) yes
C17 C14 C15 111.7(2) ?
C17 C14 C16 110.5(2) ?
C15 C14 C16 112.5(2) ?
C17 C14 N12 106.3(2) ?
C15 C14 N12 111.0(2) ?
C16 C14 N12 104.4(2) ?
C8 O18 C19 118.6(2) yes
O18 C19 N22 108.9(2) ?
O18 C19 C20 108.8(2) yes
N22 C19 C20 112.2(2) ?
O18 C19 C25 106.1(2) ?
N22 C19 C25 104.0(2) yes
C20 C19 C25 116.3(2) ?
N21 C20 C19 124.0(2) ?
C20 N21 C7 117.3(2) yes
C23 N22 C28 121.0(2) ?
C23 N22 C19 104.0(2) ?
C28 N22 C19 121.5(2) ?
C24 C23 N22 111.8(2) ?
C24 C23 C29 122.1(2) ?
N22 C23 C29 125.9(2) ?
C23 C24 C32 122.7(2) ?
C23 C24 C25 108.3(2) ?
C32 C24 C25 129.0(2) ?
C19 C25 C26 114.8(2) ?
C19 C25 C27 111.9(2) ?
C26 C25 C27 109.3(2) ?
C19 C25 C24 98.8(2) ?
C26 C25 C24 113.5(2) ?
C27 C25 C24 108.0(2) ?
C30 C29 C23 114.5(2) ?
C31 C30 C29 123.3(2) ?
C30 C31 C32 120.7(2) ?
C24 C32 C31 116.5(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.402(3) ?
C1 C10 . 1.417(3) ?
C1 C2 . 1.421(3) ?
C2 C3 . 1.409(3) ?
C3 C4 . 1.386(4) ?
C4 C5 . 1.358(3) ?
C5 C6 . 1.429(3) ?
C6 C7 . 1.452(3) ?
C7 C8 . 1.363(3) ?
C7 N21 . 1.371(3) yes
C8 O18 . 1.366(2) yes
C8 C9 . 1.401(3) ?
C9 C10 . 1.404(3) ?
C9 C11 . 1.462(3) ?
C11 N12 . 1.287(3) yes
N12 O13 . 1.277(2) yes
N12 C14 . 1.543(2) ?
C14 C17 . 1.477(3) ?
C14 C15 . 1.513(3) ?
C14 C16 . 1.545(3) ?
O18 C19 . 1.452(2) yes
C19 N22 . 1.464(2) yes
C19 C20 . 1.497(3) yes
C19 C25 . 1.515(3) yes
C20 N21 . 1.311(3) yes
N22 C23 . 1.410(2) ?
N22 C28 . 1.440(3) ?
C23 C24 . 1.333(3) ?
C23 C29 . 1.453(2) ?
C24 C32 . 1.366(3) ?
C24 C25 . 1.547(2) ?
C25 C26 . 1.553(3) ?
C25 C27 . 1.563(3) ?
C29 C30 . 1.381(3) ?
C30 C31 . 1.353(3) ?
C31 C32 . 1.440(3) ?
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_publ_flag
C6 C1 C2 C3 -0.7(3) ?
C10 C1 C2 C3 178.4(2) ?
C1 C2 C3 C4 -1.2(3) ?
C2 C3 C4 C5 0.9(4) ?
C3 C4 C5 C6 1.3(4) ?
C10 C1 C6 C5 -176.2(2) ?
C2 C1 C6 C5 2.9(3) ?
C10 C1 C6 C7 2.1(3) ?
C2 C1 C6 C7 -178.9(2) ?
C4 C5 C6 C1 -3.2(3) ?
C4 C5 C6 C7 178.6(2) ?
C1 C6 C7 C8 1.3(3) ?
C5 C6 C7 C8 179.6(2) ?
C1 C6 C7 N21 -179.8(2) ?
C5 C6 C7 N21 -1.6(3) ?
N21 C7 C8 O18 -5.1(3) ?
C6 C7 C8 O18 173.7(2) ?
N21 C7 C8 C9 175.5(2) ?
C6 C7 C8 C9 -5.7(3) ?
C7 C8 C9 C10 6.4(3) ?
O18 C8 C9 C10 -173.0(2) ?
C7 C8 C9 C11 -165.7(2) ?
O18 C8 C9 C11 14.9(3) ?
C8 C9 C10 C1 -2.7(3) ?
C11 C9 C10 C1 168.7(2) ?
C6 C1 C10 C9 -1.4(3) ?
C2 C1 C10 C9 179.6(2) ?
C10 C9 C11 N12 -2.9(3) ?
C8 C9 C11 N12 168.6(2) yes
C9 C11 N12 O13 8.2(3) yes
C9 C11 N12 C14 -168.0(2) yes
O13 N12 C14 C17 52.2(3) ?
C11 N12 C14 C17 -131.2(2) ?
O13 N12 C14 C15 173.9(2) ?
C11 N12 C14 C15 -9.5(3) ?
O13 N12 C14 C16 -64.7(3) ?
C11 N12 C14 C16 111.9(3) ?
C7 C8 O18 C19 28.3(2) ?
C9 C8 O18 C19 -152.2(2) ?
C8 O18 C19 N22 86.7(2) ?
C8 O18 C19 C20 -36.0(2) ?
C8 O18 C19 C25 -161.87(14) ?
O18 C19 C20 N21 25.4(3) ?
N22 C19 C20 N21 -95.2(3) ?
C25 C19 C20 N21 145.1(2) ?
C19 C20 N21 C7 -5.3(3) ?
C8 C7 N21 C20 -6.4(3) ?
C6 C7 N21 C20 174.8(2) ?
O18 C19 N22 C23 77.7(2) ?
C20 C19 N22 C23 -161.7(2) ?
C25 C19 N22 C23 -35.1(2) ?
O18 C19 N22 C28 -63.1(3) ?
C20 C19 N22 C28 57.5(3) ?
C25 C19 N22 C28 -176.0(2) ?
C28 N22 C23 C24 163.4(2) ?
C19 N22 C23 C24 22.3(2) ?
C28 N22 C23 C29 -13.9(3) ?
C19 N22 C23 C29 -154.9(2) ?
N22 C23 C24 C32 179.0(2) ?
C29 C23 C24 C32 -3.6(3) ?
N22 C23 C24 C25 -0.1(2) ?
C29 C23 C24 C25 177.3(2) ?
O18 C19 C25 C26 39.6(2) ?
N22 C19 C25 C26 154.4(2) ?
C20 C19 C25 C26 -81.6(3) ?
O18 C19 C25 C27 164.90(14) ?
N22 C19 C25 C27 -80.2(2) ?
C20 C19 C25 C27 43.7(2) ?
O18 C19 C25 C24 -81.5(2) ?
N22 C19 C25 C24 33.3(2) ?
C20 C19 C25 C24 157.3(2) ?
C23 C24 C25 C19 -20.9(2) ?
C32 C24 C25 C19 160.0(2) ?
C23 C24 C25 C26 -143.0(2) ?
C32 C24 C25 C26 37.9(3) ?
C23 C24 C25 C27 95.6(2) ?
C32 C24 C25 C27 -83.5(3) ?
C24 C23 C29 C30 3.5(3) ?
N22 C23 C29 C30 -179.5(2) ?
C23 C29 C30 C31 -1.6(4) ?
C29 C30 C31 C32 -0.2(4) ?
C23 C24 C32 C31 1.6(3) ?
C25 C24 C32 C31 -179.5(2) ?
C30 C31 C32 C24 0.4(4) ?
