#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/2/2002016.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_2002016
_journal_name_full 'Acta Crystallographica, Section C'
_journal_year 1993
_journal_volume C49
_journal_page_first 400
_journal_page_last 402
_publ_section_title
;
Structure of 1,2,2,3,3,4,4,5-Octamethyl-6,7,8-trioxabicyclo[3.2.1]octane
;
loop_
_publ_author_name
' Jerzykiewicz, Lucjan B.'
" Dziewo\'nska-Baran, Danuta"
' Baran, Janusz'
' Lis, Tadeusz'
_chemical_name_systematic
;
 1,2,2,3,3,4,4,5-octamethyl-6,7,8-trioxabicyclo[3.2.1]octane
;
_chemical_formula_sum 'C13 H24 O3'
_chemical_formula_weight 228.33
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P21/c'
_cell_length_a 14.91(2)
_cell_length_b 13.48(2)
_cell_length_c 13.010(10)
_cell_angle_alpha 90.0
_cell_angle_beta 90.47(7)
_cell_angle_gamma 90.0
_cell_volume 2615(6)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 8
_cell_measurement_theta_max 15
_cell_measurement_temperature 293.0(10)
_exptl_crystal_description 'Plate shape'
_exptl_crystal_colour 'Colourless'
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_crystal_density_diffrn 1.160(3)
_exptl_crystal_density_meas 1.18
_exptl_crystal_density_method
;
flotation in H~2~O/glycerol
;
_exptl_crystal_F_000 1008
_exptl_absorpt_coefficient_mu 0.61
_diffrn_ambient_temperature 293.0(10)
_diffrn_radiation_type 'CuK\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device
'Kuma KM4 computer-controlled four-cicle \k-axis diffractometer'
_diffrn_measurement_method \w/2\q
_diffrn_reflns_number 5537
_diffrn_reflns_av_R_equivalents '0.0090 for 58 reflections'
_diffrn_reflns_theta_min 2
_diffrn_reflns_theta_max 75
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_standards_number 3
_diffrn_standards_interval_count 50
_diffrn_standards_decay_% 89
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 -2 1
0 0 4
4 0 0
_reflns_number_total 5479
_reflns_number_observed 3523
_reflns_observed_criterion 'refl_observed_if_F_>_6_\s(F)'
_refine_ls_R_factor_obs 0.037
_refine_ls_wR_factor_obs 0.035
_refine_ls_number_reflns 3348
_refine_ls_number_parameters 481
_refine_ls_number_restraints 0
_refine_ls_number_constraints 0
_refine_ls_hydrogen_treatment 'refall'
_refine_ls_weighting_scheme '1/\s^2^(Fo)'
_refine_ls_shift/esd_max 0.03
_refine_diff_density_max 0.16
_refine_diff_density_min -0.17
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 0 International_Tables_Vol_IV_Table_2.2B
H 0 0 International_Tables_Vol_IV_Table_2.2B
O 0 0 International_Tables_Vol_IV_Table_2.2B
;
XTL/E-XTL (Syntex, 1976) (block-diagonal least squares)
;
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1A -0.03319(9) 0.10320(10) 0.18787(10)
O2A 0.03274(9) 0.02573(10) 0.16350(11)
O3A 0.07097(8) 0.16596(10) 0.08248(9)
C1A -0.06356(14) 0.25761(17) 0.11008(16)
C2A -0.00867(15) 0.27092(17) 0.33347(16)
C3A 0.10439(15) 0.33787(16) 0.21527(19)
C4A 0.08571(16) 0.09188(18) 0.37398(16)
C5A 0.20299(16) 0.2171(2)   0.36181(19)
C6A 0.25657(14) 0.15880(18) 0.15697(18)
C7A 0.21823(16) 0.00327(18) 0.24713(19)
C8A 0.14069(17) 0.01451(19) 0.03185(18)
C9A 0.00983(12) 0.19544(14) 0.15964(13)
C10A 0.06097(12) 0.24041(14) 0.25189(14)
C11A 0.13172(13) 0.16261(15) 0.29626(14)
C12A 0.17880(12) 0.10151(14) 0.20697(15)
C13A 0.10928(13) 0.07760(14) 0.12152(14)
O1B 0.46641(10) 0.75607(10) 0.71159(10)
O2B 0.45803(10) 0.83539(10) 0.78815(10)
O3B 0.50479(9) 0.90081(9) 0.63907(11)
C1B 0.53907(16) 0.75031(17) 0.55070(18)
C2B 0.33967(16) 0.71189(17) 0.53900(19)
C3B 0.38469(16) 0.87083(18) 0.46107(17)
C4B 0.26884(15) 0.79921(18) 0.72077(19)
C5B 0.22827(15) 0.9165(2)   0.5849(2)
C6B 0.36811(15) 1.05656(16) 0.63947(19)
C7B 0.31349(16) 0.98796(18) 0.80310(18)
C8B 0.51597(16) 0.99884(18) 0.7917(2)
C9B 0.46946(13) 0.80666(14) 0.61320(15)
C10B 0.37491(13) 0.81682(14) 0.56530(15)
C11B 0.31023(13) 0.87347(15) 0.64344(15)
C12B 0.36160(13) 0.95979(14) 0.70297(15)
C13B 0.45792(13) 0.92670(14) 0.72924(15)
H11A -0.1130(13) 0.2764(15) 0.1615(15)
H12A -0.0411(13) 0.3217(15) 0.0880(15)
H13A -0.0957(14) 0.2184(16) 0.0561(16)
H21A 0.0235(14) 0.2915(16) 0.3943(16)
H22A -0.0503(13) 0.2147(15) 0.3505(15)
H23A -0.0511(14) 0.3316(16) 0.3060(16)
H31A 0.1396(15) 0.3709(17) 0.2701(17)
H32A 0.1502(14) 0.3295(16) 0.1585(16)
H33A 0.0605(15) 0.3851(17) 0.1941(17)
H41A 0.1312(14) 0.0429(16) 0.4031(16)
H42A 0.0634(14) 0.1300(17) 0.4338(17)
H43A 0.0386(14) 0.0538(16) 0.3437(16)
H51A 0.2431(13) 0.1659(15) 0.3913(15)
H52A 0.1767(15) 0.2540(17) 0.4206(17)
H53A 0.2390(13) 0.2684(16) 0.3216(16)
H61A 0.3077(13) 0.1765(16) 0.2107(15)
H62A 0.2365(13) 0.2196(15) 0.1245(15)
H63A 0.2827(14) 0.1191(16) 0.1061(16)
H71A 0.2547(13) 0.0200(15) 0.3049(15)
H72A 0.1683(13) -0.0469(15) 0.2692(15)
H73A 0.2539(13) -0.0279(14) 0.1894(15)
H81A 0.1602(15) -0.0568(17) 0.0575(17)
H82A 0.1937(15) 0.0438(16) 0.0006(17)
H83A 0.0932(13) 0.0043(16) -0.0175(16)
H11B 0.5192(15) 0.6791(17) 0.5407(17)
H12B 0.5423(16) 0.7784(18) 0.4826(18)
H13B 0.5919(16) 0.7486(18) 0.5912(18)
H21B 0.2697(14) 0.7167(16) 0.5137(16)
H22B 0.3443(13) 0.6673(15) 0.5974(15)
H23B 0.3764(15) 0.6811(17) 0.4769(17)
H31B 0.3280(15) 0.8787(17) 0.4295(17)
H32B 0.4131(13) 0.9390(15) 0.4691(15)
H33B 0.4297(15) 0.8267(18) 0.4096(17)
H41B 0.2232(15) 0.8346(17) 0.7664(17)
H42B 0.2314(14) 0.7470(16) 0.6873(16)
H43B 0.3140(14) 0.7697(16) 0.7675(15)
H51B 0.1858(14) 0.9501(17) 0.6364(17)
H52B 0.1935(13) 0.8634(15) 0.5505(16)
H53B 0.2432(13) 0.9699(15) 0.5361(16)
H61B 0.3077(13) 1.0804(15) 0.6202(15)
H62B 0.4030(14) 1.0470(16) 0.5745(16)
H63B 0.4036(14) 1.1107(17) 0.6835(16)
H71B 0.2453(14) 0.9962(17) 0.7925(17)
H72B 0.3163(13) 0.9321(15) 0.8569(15)
H73B 0.3385(14) 1.0512(16) 0.8305(16)
H81B 0.4903(16) 0.9993(18) 0.8638(19)
H82B 0.5147(17) 1.0625(18) 0.7620(19)
H83B 0.5730(15) 0.9648(18) 0.8002(18)