#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:19:53 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180500 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/69/7216916.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7216916
loop_
_publ_author_name
'Opris, Dorina'
'Grosu, Ion'
'Toupet, Loïc'
'Plé, Gérard'
'Terec, Anamaria'
'Mager, Sorin'
'Muntean, Luminita'
_publ_section_title
;
 Synthesis and stereochemistry of new tetraspiro-1,3-dioxanes
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2413
_journal_paper_doi               10.1039/b104604g
_journal_year                    2001
_chemical_formula_sum            'C12 H20 O2'
_chemical_formula_weight         196.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.588(2)
_cell_angle_beta                 100.393(2)
_cell_angle_gamma                112.749(3)
_cell_formula_units_Z            2
_cell_length_a                   7.1914(2)
_cell_length_b                   7.6935(3)
_cell_length_c                   10.8709(5)
_cell_measurement_temperature    293(2)
_cell_volume                     531.89(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2398
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.081
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.000(19)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.211
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0424P)²+0.2172P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                2055
_reflns_number_total             2398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104604g.txt
_cod_data_source_block           gr11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216916
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 0.44356(11) 0.50777(10) 0.14793(7) 0.0127(2) Uani 1 1 d .
O2 O 0.31078(11) 0.33037(10) 0.29596(7) 0.0144(2) Uani 1 1 d .
C1 C 0.74560(18) 0.44531(17) 0.32574(12) 0.0195(3) Uani 1 1 d .
H1A H 0.6569 0.3182 0.3323 0.023 Uiso 1 1 calc R
H1B H 0.8803 0.4876 0.3835 0.023 Uiso 1 1 calc R
H1C H 0.7598 0.4423 0.2394 0.023 Uiso 1 1 calc R
C2 C 0.64992(16) 0.58498(15) 0.36062(10) 0.0142(3) Uani 1 1 d .
H2 H 0.6420 0.5887 0.4499 0.017 Uiso 1 1 calc R
C3 C 0.78725(17) 0.79040(16) 0.35178(11) 0.0168(3) Uani 1 1 d .
H3A H 0.9247 0.8331 0.4086 0.020 Uiso 1 1 calc R
H3B H 0.8027 0.7892 0.2649 0.020 Uiso 1 1 calc R
C4 C 0.69578(18) 0.93303(16) 0.38790(11) 0.0193(3) Uani 1 1 d .
H4A H 0.7825 1.0590 0.3759 0.023 Uiso 1 1 calc R
H4B H 0.6948 0.9458 0.4777 0.023 Uiso 1 1 calc R
C5 C 0.47380(17) 0.86483(16) 0.30573(11) 0.0180(3) Uani 1 1 d .
H5A H 0.4763 0.8650 0.2168 0.022 Uiso 1 1 calc R
H5B H 0.4156 0.9531 0.3337 0.022 Uiso 1 1 calc R
C6 C 0.33678(17) 0.66084(15) 0.31676(11) 0.0158(3) Uani 1 1 d .
H6A H 0.1978 0.6182 0.2621 0.019 Uiso 1 1 calc R
H6B H 0.3258 0.6629 0.4045 0.019 Uiso 1 1 calc R
C7 C 0.42825(16) 0.51837(15) 0.27738(10) 0.0122(2) Uani 1 1 d .
C8 C 0.10885(16) 0.22766(15) 0.20829(10) 0.0144(2) Uani 1 1 d .
H8A H 0.0221 0.2941 0.2236 0.017 Uiso 1 1 calc R
H8B H 0.0439 0.0990 0.2238 0.017 Uiso 1 1 calc R
C9 C 0.24628(16) 0.41686(15) 0.05512(10) 0.0133(2) Uani 1 1 d .
H9A H 0.2686 0.4131 -0.0304 0.016 Uiso 1 1 calc R
H9B H 0.1672 0.4927 0.0663 0.016 Uiso 1 1 calc R
C10 C 0.12123(15) 0.21129(14) 0.06809(10) 0.0122(2) Uani 1 1 d .
C11 C 0.22997(15) 0.08182(15) 0.03216(10) 0.0138(2) Uani 1 1 d .
H11A H 0.2622 0.0982 -0.0496 0.017 Uiso 1 1 calc R
H11B H 0.3606 0.1234 0.0961 0.017 Uiso 1 1 calc R
C12 C 0.09789(16) -0.13269(15) 0.02268(11) 0.0145(2) Uani 1 1 d .
H12A H 0.0843 -0.1518 0.1076 0.017 Uiso 1 1 calc R
H12B H 0.1702 -0.2068 -0.0070 0.017 Uiso 1 1 calc R
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'
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
C7 O1 C9 113.83(8) . .
C7 O2 C8 114.63(8) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C1 C2 C7 112.10(9) . .
C1 C2 C3 111.23(9) . .
C7 C2 C3 110.21(9) . .
C1 C2 H2 107.7 . .
C7 C2 H2 107.7 . .
C3 C2 H2 107.7 . .
C4 C3 C2 112.11(9) . .
C4 C3 H3A 109.2 . .
C2 C3 H3A 109.2 . .
C4 C3 H3B 109.2 . .
C2 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
C3 C4 C5 110.88(9) . .
C3 C4 H4A 109.5 . .
C5 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
C4 C5 C6 110.50(9) . .
C4 C5 H5A 109.5 . .
C6 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
C6 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
C5 C6 C7 110.97(9) . .
C5 C6 H6A 109.4 . .
C7 C6 H6A 109.4 . .
C5 C6 H6B 109.4 . .
C7 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
O1 C7 O2 110.39(8) . .
O1 C7 C2 106.48(8) . .
O2 C7 C2 106.10(8) . .
O1 C7 C6 111.43(8) . .
O2 C7 C6 111.74(8) . .
C2 C7 C6 110.43(8) . .
O2 C8 C10 111.90(8) . .
O2 C8 H8A 109.2 . .
C10 C8 H8A 109.2 . .
O2 C8 H8B 109.2 . .
C10 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
O1 C9 C10 111.55(8) . .
O1 C9 H9A 109.3 . .
C10 C9 H9A 109.3 . .
O1 C9 H9B 109.3 . .
C10 C9 H9B 109.3 . .
H9A C9 H9B 108.0 . .
C9 C10 C8 106.11(8) . .
C9 C10 C11 109.97(8) . .
C8 C10 C11 111.82(9) . .
C9 C10 C12 108.49(8) . 2
C8 C10 C12 110.55(8) . 2
C11 C10 C12 109.80(8) . 2
C12 C11 C10 113.08(8) . .
C12 C11 H11A 109.0 . .
C10 C11 H11A 109.0 . .
C12 C11 H11B 109.0 . .
C10 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C11 C12 C10 113.71(9) . 2
C11 C12 H12A 108.8 . .
C10 C12 H12A 108.8 2 .
C11 C12 H12B 108.8 . .
C10 C12 H12B 108.8 2 .
H12A C12 H12B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C7 1.4253(12) .
O1 C9 1.4317(12) .
O2 C7 1.4284(12) .
O2 C8 1.4338(12) .
C1 C2 1.5265(15) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C7 1.5323(14) .
C2 C3 1.5328(14) .
C2 H2 0.9800 .
C3 C4 1.5260(16) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.5282(15) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.5312(15) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.5339(14) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C8 C10 1.5342(15) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.5279(14) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.5382(14) .
C10 C12 1.5385(14) 2
C11 C12 1.5310(14) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C10 1.5385(14) 2
C12 H12A 0.9700 .
C12 H12B 0.9700 .
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_4
C1 C2 C3 C4 -179.29(9) . .
C7 C2 C3 C4 55.74(12) . .
C2 C3 C4 C5 -55.55(12) . .
C3 C4 C5 C6 55.72(12) . .
C4 C5 C6 C7 -57.36(12) . .
C9 O1 C7 O2 55.38(10) . .
C9 O1 C7 C2 170.12(8) . .
C9 O1 C7 C6 -69.40(10) . .
C8 O2 C7 O1 -54.00(11) . .
C8 O2 C7 C2 -168.98(8) . .
C8 O2 C7 C6 70.60(11) . .
C1 C2 C7 O1 -59.71(11) . .
C3 C2 C7 O1 64.76(10) . .
C1 C2 C7 O2 57.91(11) . .
C3 C2 C7 O2 -177.62(8) . .
C1 C2 C7 C6 179.17(9) . .
C3 C2 C7 C6 -56.36(11) . .
C5 C6 C7 O1 -60.24(11) . .
C5 C6 C7 O2 175.74(8) . .
C5 C6 C7 C2 57.89(11) . .
C7 O2 C8 C10 55.15(11) . .
C7 O1 C9 C10 -58.21(11) . .
O1 C9 C10 C8 54.24(10) . .
O1 C9 C10 C11 -66.86(11) . .
O1 C9 C10 C12 173.04(8) . 2
O2 C8 C10 C9 -52.71(11) . .
O2 C8 C10 C11 67.19(11) . .
O2 C8 C10 C12 -170.15(8) . 2
C9 C10 C11 C12 -171.14(9) . .
C8 C10 C11 C12 71.25(11) . .
C12 C10 C11 C12 -51.84(13) 2 .
C10 C11 C12 C10 53.90(13) . 2
