#------------------------------------------------------------------------------
#$Date: 2017-10-13 09:09:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/54/2205478.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_2205478
loop_
_publ_author_name
'Kgomo, Ditebogo B.'
'Levendis, Demetrius C.'
'Gukasov, Arsen'
'Cousson, Alain'
'Schöning, Ludwig F. R.'
'Venter, Andrew M.'
_publ_section_title
;
 Low-temperature (110K) single-crystal neutron diffraction study of
 (+-)-camphoric anhydride
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1141
_journal_page_last               o1143
_journal_paper_doi               10.1107/S1600536805008950
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C10 H14 O3'
_chemical_formula_moiety         'C10 H14 O3'
_chemical_formula_sum            'C10 H14 O3'
_chemical_formula_weight         182.22
_chemical_name_systematic
;
(+-)-1,8,8-Trimethyl-3-oxabicyclo[3.2.1]octane-2,4-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 92.179(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5001(8)
_cell_length_b                   11.5624(14)
_cell_length_c                   12.7093(15)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    110
_cell_measurement_theta_max      22
_cell_measurement_theta_min      16
_cell_volume                     954.5(2)
_computing_cell_refinement       DIF4N
_computing_data_collection
'DIF4N (modified Linux version of DIF4; Stoe & Cie, 1991)'
_computing_data_reduction
'PRON98 (modified version of REDU4; Stoe & Cie, 1990; Meven, Year?)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
'a previous X-ray study gave position parameters for heavy atoms (Reference?)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
5C2 four-circle (Orphée reactor, Saclay, France)
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  Cu_(220)
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.83300
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4137
_diffrn_reflns_theta_full        39.506
_diffrn_reflns_theta_max         39.506
_diffrn_reflns_theta_min         2.792
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  450
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             128
_exptl_crystal_size_max          5.00
_exptl_crystal_size_mid          4.00
_exptl_crystal_size_min          3.00
_refine_diff_density_max         0.12
_refine_diff_density_min         -0.14
_refine_ls_extinction_coef       3.4(8)
_refine_ls_extinction_method     'Larson (1970), eq. 22'
_refine_ls_goodness_of_fit_ref   1.1006
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         1594
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000154
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial, (Watkin, 1994; Prince, 1982) W =
[weight][1-(\DF/6\sF)²]² where  [weight] = 1.0/[A₀T₀(x)+A₁T₁(x)
... +Aₙ₋₁Tₙ₋₁(x)] where x = Fcalc/Fmax and Ai are the Chebychev
coefficients  listed below: 0.703 -0.458 0.556 -0.177 0.795E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0627
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                1594
_reflns_number_total             3553
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            dn6207.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205478
_cod_database_fobs_code          2205478
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-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_occupancy
_atom_site_type_symbol
C1 0.7903(3) 0.71470(18) 0.48982(16) 0.0188 Uani 1.0000 C
C2 1.0199(3) 0.73790(19) 0.51432(16) 0.0203 Uani 1.0000 C
C3 1.0182(3) 0.87660(18) 0.36654(17) 0.0205 Uani 1.0000 C
C4 0.7950(3) 0.84498(17) 0.34358(17) 0.0194 Uani 1.0000 C
C5 0.6641(3) 0.9091(2) 0.42731(19) 0.0246 Uani 1.0000 C
C6 0.6682(3) 0.8264(2) 0.52484(17) 0.0223 Uani 1.0000 C
C7 0.7580(3) 0.71385(19) 0.36671(16) 0.0179 Uani 1.0000 C
C8 0.9082(4) 0.6336(2) 0.30866(18) 0.0245 Uani 1.0000 C
C9 0.5330(3) 0.6807(2) 0.33370(19) 0.0252 Uani 1.0000 C
C10 0.7222(4) 0.6053(2) 0.54726(19) 0.0270 Uani 1.0000 C
O1 1.1120(4) 0.8274(2) 0.4582(2) 0.0230 Uani 1.0000 O
O2 1.1304(4) 0.6881(3) 0.5787(2) 0.0298 Uani 1.0000 O
O3 1.1226(4) 0.9430(3) 0.3174(2) 0.0299 Uani 1.0000 O
H4 0.7553(9) 0.8694(5) 0.2608(4) 0.0375 Uani 1.0000 H
H51 0.5050(8) 0.9217(6) 0.3956(5) 0.0447 Uani 1.0000 H
H52 0.7279(9) 0.9952(5) 0.4473(5) 0.0415 Uani 1.0000 H
H61 0.5119(8) 0.8000(5) 0.5448(5) 0.0410 Uani 1.0000 H
H62 0.7425(9) 0.8663(5) 0.5953(4) 0.0400 Uani 1.0000 H
H81 1.0727(9) 0.6545(6) 0.3224(5) 0.0444 Uani 1.0000 H
H82 0.8782(11) 0.6388(7) 0.2230(5) 0.0512 Uani 1.0000 H
H83 0.8850(11) 0.5424(5) 0.3326(6) 0.0500 Uani 1.0000 H
H90 0.4183(8) 0.7281(6) 0.3787(6) 0.0519 Uani 1.0000 H
H91 0.5080(10) 0.5859(5) 0.3443(6) 0.0489 Uani 1.0000 H
H92 0.5043(10) 0.7008(7) 0.2502(5) 0.0531 Uani 1.0000 H
H101 0.7994(11) 0.5271(6) 0.5177(6) 0.0517 Uani 1.0000 H
H102 0.5553(9) 0.5949(6) 0.5393(5) 0.0456 Uani 1.0000 H
H103 0.7621(11) 0.6094(7) 0.6320(5) 0.0508 Uani 1.0000 H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'O   ' 0.0000 0.0000 'Varley F. Sears, Neutron News, vol 3, n3 (1992) p26-37'
'C   ' 0.0000 0.0000 'Varley F. Sears, Neutron News, vol 3, n3 (1992) p26-37'
'N   ' 0.0000 0.0000 'Varley F. Sears, Neutron News, vol 3, n3 (1992) p26-37'
'H   ' 0.0000 0.0000 'Varley F. Sears, Neutron News, vol 3, n3 (1992) p26-37'
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
C2 C1 C6 107.05(17) no
C2 C1 C7 107.15(16) no
C6 C1 C7 103.58(16) no
C2 C1 C10 110.06(17) no
C6 C1 C10 112.38(18) no
C7 C1 C10 116.04(18) no
C1 C2 O1 117.09(19) no
C1 C2 O2 126.8(2) no
O1 C2 O2 116.1(2) no
C4 C3 O1 116.22(19) no
C4 C3 O3 127.2(2) no
O1 C3 O3 116.5(2) no
C3 C4 C5 107.14(17) no
C3 C4 C7 110.55(16) no
C5 C4 C7 103.82(16) no
C3 C4 H4 107.9(3) no
C5 C4 H4 114.1(4) no
C7 C4 H4 113.1(3) no
C4 C5 C6 104.74(17) no
C4 C5 H51 109.8(4) no
C6 C5 H51 110.9(4) no
C4 C5 H52 111.9(4) no
C6 C5 H52 111.9(4) no
H51 C5 H52 107.7(5) no
C5 C6 C1 105.57(16) no
C5 C6 H61 111.4(4) no
C1 C6 H61 108.3(4) no
C5 C6 H62 112.5(4) no
C1 C6 H62 111.0(3) no
H61 C6 H62 108.0(5) no
C4 C7 C1 99.52(15) no
C4 C7 C8 112.71(16) no
C1 C7 C8 114.47(18) no
C4 C7 C9 109.76(17) no
C1 C7 C9 111.04(17) no
C8 C7 C9 109.04(18) no
C7 C8 H81 114.6(4) no
C7 C8 H82 110.2(4) no
H81 C8 H82 106.1(6) no
C7 C8 H83 110.1(4) no
H81 C8 H83 107.8(5) no
H82 C8 H83 107.7(6) no
C7 C9 H90 112.6(4) no
C7 C9 H91 110.4(4) no
H90 C9 H91 108.7(6) no
C7 C9 H92 109.4(4) no
H90 C9 H92 107.7(6) no
H91 C9 H92 107.7(6) no
C1 C10 H101 111.7(4) no
C1 C10 H102 110.5(4) no
H101 C10 H102 109.8(6) no
C1 C10 H103 111.7(4) no
H101 C10 H103 106.0(6) no
H102 C10 H103 107.0(6) no
C3 O1 C2 122.5(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.536(3) no
C1 C6 1.589(3) no
C1 C7 1.571(3) no
C1 C10 1.534(3) no
C2 O1 1.403(3) no
C2 O2 1.214(3) no
C3 C4 1.513(3) no
C3 O1 1.414(3) no
C3 O3 1.214(3) no
C4 C5 1.573(3) no
C4 C7 1.565(3) no
C4 H4 1.111(5) no
C5 C6 1.565(3) no
C5 H51 1.105(6) no
C5 H52 1.104(6) no
C6 H61 1.100(6) no
C6 H62 1.103(5) no
C7 C8 1.553(3) no
C7 C9 1.555(3) no
C8 H81 1.104(6) no
C8 H82 1.101(6) no
C8 H83 1.109(6) no
C9 H90 1.103(7) no
C9 H91 1.117(7) no
C9 H92 1.095(6) no
C10 H101 1.107(7) no
C10 H102 1.093(6) no
C10 H103 1.099(6) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C4 H4 O2 4_464 1.110(6) 2.513(6) 3.514(3) 149.4(4) yes
C5 H52 O1 2_776 1.104(6) 2.576(6) 3.655(3) 165.1(5) yes
C9 H90 O1 1_455 1.103(7) 2.541(7) 3.633(3) 170.5(5) yes
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 85566
