#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/59/2015986.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_2015986
loop_
_publ_author_name
'Branko Kaitner'
'Vladimir Stilinović'
_publ_section_title
;
 Conformational enantiomeric disorder in tripivaloylmethane
;
_journal_coeditor_code           GD3098
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o353
_journal_page_last               o354
_journal_paper_doi               10.1107/S0108270107012474
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C16 H28 O3'
_chemical_formula_moiety         'C16 H28 O3'
_chemical_formula_sum            'C16 H28 O3'
_chemical_formula_weight         268.38
_chemical_name_common            tripivaloylmethane
_chemical_name_systematic
;
4-(2,2-dimethylpropanoyl)-2,2,6,6-tetramethylheptane-3,5-dione
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.711(7)
_cell_length_b                   15.711(7)
_cell_length_c                   5.792(2)
_cell_measurement_reflns_used    1072
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      4.6
_cell_volume                     1238.1(9)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2003)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
WinGX (Farrugia, 1999) and PARST97 (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_measurement_method       'omega 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  0.0348
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3386
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         31.93
_diffrn_reflns_theta_min         4.49
_diffrn_standards_decay_%        0
_diffrn_standards_number         '4 '
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.08
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.122
_refine_diff_density_min         -0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         518
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1632P)²+0.0580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2339
_reflns_number_gt                433
_reflns_number_total             518
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gd3098.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               2015986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, z'
'-x+y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
loop_
_atom_site_type_symbol
_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_refinement_flags
_atom_site_occupancy
C C5 0.2751(5) 0.154(3) 0.8404(13) 0.142(14) Uani d P 0.5
H H5A 0.264 0.202 0.7673 0.213 Uiso calc PR 0.5
H H5B 0.2737 0.1086 0.7263 0.213 Uiso calc PR 0.5
H H5C 0.3381 0.1856 0.915 0.213 Uiso calc PR 0.5
C C4 0.2015(5) 0.1767(4) 1.1820(14) 0.137(2) Uani d . 1
H H6A 0.1385 0.1544 1.2526 0.205 Uiso calc R 1
H H6B 0.2202 0.2359 1.0968 0.205 Uiso calc R 1
H H6C 0.2495 0.1895 1.2996 0.205 Uiso calc R 1
C C1 0 0 0.9920(7) 0.0443(9) Uani d SD 1
C C3 0.1954(2) 0.09771(11) 1.0186(7) 0.0651(9) Uani d S 1
C C2 0.1002(3) 0.0802(3) 0.9009(6) 0.0507(9) Uani d P 0.5
O O1 0.1007(3) 0.1278(4) 0.7338(7) 0.0811(14) Uani d P 0.5
H H1 0 0 1.160(4) 0.066(19) Uiso d SD 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C5 0.058(3) 0.18(2) 0.096(4) -0.007(10) 0.015(3) 0.001(9)
C4 0.162(6) 0.112(4) 0.135(4) 0.068(4) -0.012(4) -0.032(3)
C1 0.0465(12) 0.0465(12) 0.0401(16) 0.0232(6) 0 0
C3 0.0483(15) 0.0738(16) 0.0647(16) 0.0241(8) -0.0025(13) -0.0013(6)
C2 0.0490(18) 0.0504(16) 0.0494(18) 0.0224(14) 0.0041(14) 0.0019(13)
O1 0.071(2) 0.086(3) 0.076(2) 0.032(2) 0.0107(17) 0.0382(19)
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 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C3 C5 H5A . . 109.5
C3 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C3 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
C3 C4 H6A . . 109.5
C3 C4 H6B . . 109.5
H6A C4 H6B . . 109.5
C3 C4 H6C . . 109.5
H6A C4 H6C . . 109.5
H6B C4 H6C . . 109.5
C2 C1 C2 4 . 108.87(19)
C2 C1 H1 4 . 110.07(19)
C2 C1 H1 3 . 110.07(19)
C2 C1 H1 5 . 110.07(18)
C2 C1 H1 . . 110.07(19)
C2 C1 H1 6 . 110.07(18)
C2 C1 H1 2 . 110.07(18)
C4 C3 C4 . 5 103.0(6)
C4 C3 C5 . . 104.7(18)
C4 C3 C5 5 . 120.9(17)
C4 C3 C5 . 5 120.9(17)
C4 C3 C5 5 5 104.7(18)
C4 C3 C2 . . 94.6(3)
C4 C3 C2 5 . 124.1(3)
C5 C3 C2 . . 104.4(9)
C5 C3 C2 5 . 110.6(6)
C4 C3 C2 . 5 124.1(3)
C4 C3 C2 5 5 94.6(3)
C5 C3 C2 . 5 110.6(6)
C5 C3 C2 5 5 104.4(9)
C2 C2 O1 5 . 127.6(3)
C2 C2 C1 5 . 72.08(16)
O1 C2 C1 . . 117.6(4)
C2 C2 C3 5 . 72.10(16)
O1 C2 C3 . . 122.3(4)
C1 C2 C3 . . 120.0(3)
C2 C2 C2 5 6 120.000(3)
O1 C2 C2 . 6 72.5(3)
C3 C2 C2 . 6 152.00(19)
C2 C2 O1 5 6 133.6(2)
C1 C2 O1 . 6 85.7(2)
C3 C2 O1 . 6 150.8(3)
O1 O1 C2 6 . 107.5(3)
C2 O1 C2 . 6 70.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C5 C3 . 1.518(11)
C5 H5A . 0.96
C5 H5B . 0.96
C5 H5C . 0.96
C4 C3 . 1.526(7)
C4 H6A . 0.96
C4 H6B . 0.96
C4 H6C . 0.96
C1 C2 . 1.537(4)
C1 H1 . 0.97(2)
C3 C4 5 1.525(7)
C3 C5 5 1.518(11)
C3 C2 . 1.538(5)
C2 O1 . 1.221(6)
