#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2009138.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_2009138
loop_
_publ_author_name
'Zimmer, R.'
'Zahn, G.'
'Khan, F. A.'
'Reissig, H.-U.'
_publ_section_title
;
 Configurational analysis of
 14,14-dimethyl-12-oxatricyclo[9.2.1.0^3,8^]tetradeca-3,5,7-trien-13-one
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1941
_journal_page_last               1943
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'C15 H18 O2'
_chemical_formula_moiety         'C15 H18 O2'
_chemical_formula_sum            'C15 H18 O2'
_chemical_formula_weight         230.29
_chemical_name_systematic
; 14,14-Dimethyl-12-oxa-tricyclo[9.2.1.03,8]tetradeca-
3,5,7-trien-13-one
;
_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'
_audit_creation_method           'manual editing of a SHELXL97.cif'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.043(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.7311(7)
_cell_length_b                   23.123(2)
_cell_length_c                   11.0657(8)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      10.1
_cell_volume                     2545.1(3)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe & Cie, 1997)'
_computing_data_reduction        'XRED (Stoe & Cie, 1996)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe Stadi4'
_diffrn_measurement_method       '\w-\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5857
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             992
_exptl_crystal_size_max          1.06
_exptl_crystal_size_mid          0.87
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.151
_refine_ls_extinction_coef       0.0133(8)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                3727
_reflns_number_total             5571
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    ja1001.cif
_[local]_cod_data_source_block   s091
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_cod_database_code               2009138
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_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
O1 0.61528(13) 0.73219(6) 0.96370(11) 0.0555(4) Uani d 1 O
O2 0.51614(14) 0.81536(6) 0.88088(13) 0.0568(4) Uani d 1 O
C1 0.56884(17) 0.77127(8) 0.86694(17) 0.0450(4) Uani d 1 C
C2 0.59080(18) 0.74975(8) 0.74796(17) 0.0447(4) Uani d 1 C
C3 0.45528(19) 0.72588(9) 0.64888(17) 0.0474(4) Uani d 1 C
C4 0.35305(17) 0.70770(8) 0.70530(16) 0.0434(4) Uani d 1 C
C5 0.23994(19) 0.74204(9) 0.6827(2) 0.0534(5) Uani d 1 C
C6 0.1446(2) 0.72811(11) 0.7340(3) 0.0680(6) Uani d 1 C
C7 0.1610(2) 0.67973(11) 0.8095(3) 0.0738(7) Uani d 1 C
C8 0.2712(2) 0.64478(10) 0.8314(2) 0.0664(6) Uani d 1 C
C9 0.36779(19) 0.65764(8) 0.77967(18) 0.0500(5) Uani d 1 C
C10 0.4826(2) 0.61633(10) 0.8010(2) 0.0619(6) Uani d 1 C
C11 0.6117(2) 0.62829(10) 0.9184(2) 0.0662(6) Uani d 1 C
C12 0.6862(2) 0.68478(9) 0.92797(19) 0.0554(5) Uani d 1 C
C13 0.71284(18) 0.70923(9) 0.81037(18) 0.0515(5) Uani d 1 C
C14 0.8388(2) 0.74779(14) 0.8634(3) 0.0752(7) Uani d 1 C
C15 0.7383(3) 0.66384(12) 0.7223(3) 0.0662(6) Uani d 1 C
O3 0.08033(13) 0.62868(5) 0.19761(12) 0.0525(3) Uani d 1 O
O4 -0.06419(14) 0.58653(7) 0.02069(13) 0.0681(4) Uani d 1 O
C16 0.03252(18) 0.58262(8) 0.12044(18) 0.0473(4) Uani d 1 C
C17 0.11461(18) 0.52991(8) 0.17992(18) 0.0472(4) Uani d 1 C
C18 0.0406(2) 0.49375(9) 0.2505(2) 0.0544(5) Uani d 1 C
C19 -0.0614(2) 0.52566(8) 0.2890(2) 0.0517(5) Uani d 1 C
C20 -0.1972(2) 0.51875(11) 0.2139(3) 0.0704(6) Uani d 1 C
C21 -0.2950(3) 0.54637(14) 0.2443(4) 0.0905(9) Uani d 1 C
C22 -0.2590(3) 0.58210(14) 0.3506(4) 0.0977(11) Uani d 1 C
C23 -0.1251(3) 0.59039(11) 0.4252(3) 0.0809(8) Uani d 1 C
C24 -0.0239(2) 0.56270(8) 0.3967(2) 0.0579(5) Uani d 1 C
C25 0.1208(3) 0.57260(11) 0.4811(2) 0.0658(6) Uani d 1 C
C26 0.1945(3) 0.61893(11) 0.4350(2) 0.0641(6) Uani d 1 C
C27 0.2083(2) 0.61462(9) 0.30408(18) 0.0532(5) Uani d 1 C
C28 0.25077(18) 0.55789(9) 0.25846(18) 0.0537(5) Uani d 1 C
C29 0.3169(3) 0.57371(16) 0.1612(3) 0.0779(7) Uani d 1 C
C30 0.3516(3) 0.52164(15) 0.3666(3) 0.0796(8) Uani d 1 C
H2 0.6169(17) 0.7823(8) 0.7062(17) 0.048(5) Uiso d 1 H
H3A 0.4136(19) 0.7564(9) 0.5832(19) 0.062(6) Uiso d 1 H
H3B 0.4774(18) 0.6930(8) 0.5997(18) 0.055(5) Uiso d 1 H
H5 0.229(2) 0.7766(9) 0.628(2) 0.065(6) Uiso d 1 H
H6 0.067(2) 0.7530(10) 0.717(2) 0.074(7) Uiso d 1 H
H7 0.096(2) 0.6680(10) 0.847(2) 0.090(8) Uiso d 1 H
H8 0.284(2) 0.6092(11) 0.883(2) 0.090(8) Uiso d 1 H
H10A 0.504(2) 0.6149(9) 0.719(2) 0.063(6) Uiso d 1 H
H10B 0.453(2) 0.5792(10) 0.812(2) 0.076(7) Uiso d 1 H
H11A 0.676(2) 0.5986(10) 0.926(2) 0.079(7) Uiso d 1 H
H11B 0.594(2) 0.6257(9) 1.002(2) 0.074(7) Uiso d 1 H
H12 0.7702(19) 0.6823(8) 1.0007(19) 0.050(5) Uiso d 1 H
H14A 0.830(2) 0.7774(10) 0.928(2) 0.078(7) Uiso d 1 H
H14B 0.917(2) 0.7244(10) 0.910(2) 0.082(7) Uiso d 1 H
H14C 0.853(3) 0.7687(12) 0.789(3) 0.106(10) Uiso d 1 H
H15A 0.659(2) 0.6392(10) 0.672(2) 0.075(7) Uiso d 1 H
H15B 0.811(2) 0.6395(10) 0.771(2) 0.082(7) Uiso d 1 H
H15C 0.768(3) 0.6831(12) 0.658(3) 0.106(10) Uiso d 1 H
H17 0.1215(17) 0.5067(8) 0.1109(18) 0.045(5) Uiso d 1 H
H18A -0.008(2) 0.4613(9) 0.190(2) 0.069(6) Uiso d 1 H
H18B 0.105(2) 0.4750(9) 0.325(2) 0.060(6) Uiso d 1 H
H20 -0.221(2) 0.4929(11) 0.137(2) 0.086(8) Uiso d 1 H
H21 -0.391(3) 0.5415(12) 0.187(3) 0.109(10) Uiso d 1 H
H22 -0.328(3) 0.5997(14) 0.369(3) 0.135(12) Uiso d 1 H
H23 -0.093(3) 0.6140(12) 0.501(3) 0.096(9) Uiso d 1 H
H25A 0.173(2) 0.5354(10) 0.494(2) 0.072(7) Uiso d 1 H
H25B 0.124(2) 0.5853(10) 0.568(2) 0.083(7) Uiso d 1 H
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'