#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/03/2200352.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_2200352
loop_
_publ_author_name
'Simon Fielder'
'Daryl D. Rowan'
'Michael S. Sherburn'
'Anthony K. Burrell'
_publ_section_title
;
 1-(Cholest-4-en-3β-yl)-2,2,2-trichloroethanimidate tert-butyl
 methyl ether hemisolvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o533
_journal_page_last               o534
_journal_paper_doi               10.1107/S160053680100825X
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C29 H45 Cl3 N O, 0.5C5 H12 O1'
_chemical_formula_moiety         'C29 H45 Cl3 N O, 0.5C5 H12 O1'
_chemical_formula_sum            'C31.5 H51 Cl3 N O1.5'
_chemical_formula_weight         574.08
_chemical_name_common            'Cholesteryl Trichloroacetimidate'
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 109.14(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.037(13)
_cell_length_b                   9.072(6)
_cell_length_c                   12.628(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     3143(3)
_computing_cell_refinement       CAD-4/PC
_computing_data_collection       'CAD-4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'XCAD4B (Harms, 1994)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 '
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_sigmaI/netI    .024
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3008
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .318
_exptl_absorpt_correction_T_max  .911
_exptl_absorpt_correction_T_min  .857
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .30
_refine_diff_density_max         .97
_refine_diff_density_min         -.72
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .00(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          .086
_refine_ls_R_factor_gt           .078
_refine_ls_shift/su_max          .048
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1249P)²+13.5363P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .221
_reflns_number_gt                2640
_reflns_number_total             2926
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk6022.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C31.50 H51 Cl3 N O1.50'
_cod_database_code               2200352
_cod_database_fobs_code          2200352
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cl11 .01083(10) .0125(3) .3192(2) .0697(8) Uani d . 1 . . Cl
Cl12 .00509(11) -.2983(3) .3199(3) .0861(10) Uani d . 1 . . Cl
Cl13 .07229(9) -.1487(5) .50617(18) .0843(9) Uani d . 1 . . Cl
O1 .07050(19) -.1069(6) .2047(4) .0447(13) Uani d . 1 . . O
N1 .1259(3) -.2227(10) .3493(7) .062(2) Uani d . 1 . . N
C28 .0834(3) -.1651(10) .3022(6) .050(2) Uani d . 1 . . C
C1 .1044(2) -.1309(9) -.0568(6) .0371(15) Uani d . 1 . . C
H1C .1171 -.2330 -.0463 .045 Uiso calc R 1 . . H
H1D .0842 -.1198 -.1365 .045 Uiso calc R 1 . . H
C2 .0719(2) -.1086(9) .0158(6) .0415(17) Uani d . 1 . . C
H2A .0565 -.0101 .0014 .050 Uiso calc R 1 . . H
H2B .0459 -.1841 -.0026 .050 Uiso calc R 1 . . H
C3 .1029(3) -.1215(8) .1368(6) .0398(17) Uani d . 1 . . C
H3A .1186 -.2211 .1499 .048 Uiso calc R 1 . . H
C4 .1418(3) -.0057(9) .1692(6) .0402(16) Uani d . 1 . . C
H4A .1619 -.0183 .2489 .048 Uiso calc R 1 . . H
H4B .1266 .0931 .1603 .048 Uiso calc R 1 . . H
C5 .1741(3) -.0175(7) .0962(5) .0328(14) Uani d . 1 . . C
C6 .2215(2) -.0192(7) .1417(5) .0326(14) Uani d . 1 . . C
H6A .2348 -.0157 .2212 .039 Uiso calc R 1 . . H
C7 .2566(2) -.0265(8) .0764(5) .0331(15) Uani d . 1 . . C
H7A .2727 -.1242 .0886 .040 Uiso calc R 1 . . H
H7B .2822 .0491 .1059 .040 Uiso calc R 1 . . H
C8 .2323(2) -.0022(7) -.0501(5) .0275(13) Uani d . 1 . . C
H8A .2268 .1058 -.0647 .033 Uiso calc R 1 . . H
C9 .1830(2) -.0811(8) -.0907(5) .0289(13) Uani d . 1 . . C
H9A .1897 -.1867 -.0682 .035 Uiso calc R 1 . . H
C10 .1474(2) -.0242(8) -.0314(5) .0308(14) Uani d . 1 . . C
C11 .1608(2) -.0798(9) -.2208(5) .0355(15) Uani d . 1 . . C
H11A .1315 -.1434 -.2435 .043 Uiso calc R 1 . . H
H11B .1502 .0218 -.2459 .043 Uiso calc R 1 . . H
C12 .1963(2) -.1336(9) -.2812(5) .0340(14) Uani d . 1 . . C
H12A .2041 -.2389 -.2636 .041 Uiso calc R 1 . . H
H12B .1806 -.1242 -.3633 .041 Uiso calc R 1 . . H
C13 .2431(2) -.0428(7) -.2438(5) .0268(13) Uani d . 1 . . C
C14 .2645(2) -.0593(7) -.1145(5) .0271(13) Uani d . 1 . . C
H14A .2687 -.1674 -.0988 .033 Uiso calc R 1 . . H
C15 .3155(2) .0053(8) -.0864(5) .0327(14) Uani d . 1 . . C
H15A .3375 -.0344 -.0146 .039 Uiso calc R 1 . . H
H15B .3148 .1141 -.0816 .039 Uiso calc R 1 . . H
C16 .3318(2) -.0453(8) -.1867(5) .0347(15) Uani d . 1 . . C
H16A .3567 -.1241 -.1625 .042 Uiso calc R 1 . . H
H16B .3461 .0385 -.2154 .042 Uiso calc R 1 . . H
C17 .2854(2) -.1040(7) -.2800(5) .0295(14) Uani d . 1 . . C
H17A .2851 -.2138 -.2730 .035 Uiso calc R 1 . . H
C18 .2331(3) .1197(8) -.2805(6) .0365(16) Uani d . 1 . . C
H18A .2195 .1248 -.3624 .055 Uiso calc R 1 . . H
H18B .2636 .1756 -.2547 .055 Uiso calc R 1 . . H
H18C .2098 .1618 -.2476 .055 Uiso calc R 1 . . H
C19 .1284(3) .1321(9) -.0713(6) .0413(17) Uani d . 1 . . C
H19A .1061 .1642 -.0319 .062 Uiso calc R 1 . . H
H19B .1110 .1305 -.1522 .062 Uiso calc R 1 . . H
H19C .1559 .2006 -.0550 .062 Uiso calc R 1 . . H
C20 .2863(2) -.0675(8) -.3993(5) .0353(15) Uani d . 1 . . C
H20A .2887 .0420 -.4048 .042 Uiso calc R 1 . . H
C21 .2408(3) -.1169(11) -.4917(6) .047(2) Uani d . 1 . . C
H21A .2436 -.0915 -.5647 .070 Uiso calc R 1 . . H
H21B .2122 -.0673 -.4830 .070 Uiso calc R 1 . . H
H21C .2370 -.2238 -.4871 .070 Uiso calc R 1 . . H
C22 .3316(2) -.1351(10) -.4167(5) .0391(15) Uani d . 1 . . C
H22A .3283 -.2437 -.4184 .047 Uiso calc R 1 . . H
H22B .3605 -.1092 -.3518 .047 Uiso calc R 1 . . H
C23 .3403(3) -.0844(9) -.5244(6) .0433(17) Uani d . 1 . . C
H23A .3412 .0247 -.5260 .052 Uiso calc R 1 . . H
H23B .3129 -.1178 -.5901 .052 Uiso calc R 1 . . H
C24 .3878(2) -.1448(11) -.5329(5) .0437(17) Uani d . 1 . . C
H24A .4153 -.0947 -.4762 .052 Uiso calc R 1 . . H
H24B .3899 -.2509 -.5137 .052 Uiso calc R 1 . . H
C25 .3946(3) -.1277(10) -.6466(8) .063(2) Uani d D 1 . . C
H25A .3700 -.1947 -.6984 .075 Uiso calc R 1 . . H
C26 .3853(3) .0228(11) -.7004(8) .068(3) Uani d D 1 . . C
H26A .3530 .0577 -.7025 .103 Uiso calc R 1 . . H
H26B .3864 .0167 -.7769 .103 Uiso calc R 1 . . H
H26C .4102 .0918 -.6566 .103 Uiso calc R 1 . . H
C27 .4449(3) -.1883(11) -.6420(8) .060(2) Uani d D 1 . . C
H27A .4491 -.1754 -.7153 .091 Uiso calc R 1 . . H
H27B .4468 -.2934 -.6229 .091 Uiso calc R 1 . . H
H27C .4706 -.1347 -.5849 .091 Uiso calc R 1 . . H
C29 .0451(2) -.1490(9) .3604(5) .0371(15) Uani d . 1 . . C
C100 .0000 .3864(11) .0000 .065(4) Uani d SD 1 . . C
C200 .0400(14) .467(6) -.034(4) .067(14) Uani d PD .50 . . C
H20B .0257 .5152 -.1044 .101 Uiso d PR .50 . . H
H20C .0555 .5385 .0227 .101 Uiso d PR .50 . . H
H20D .0638 .3966 -.0396 .101 Uiso d PR .50 . . H
O2 -.0252(7) .2675(17) -.0709(13) .081(6) Uani d PD .50 . . O
C500 -.0429(10) .323(3) -.1845(16) .071(7) Uani d PD .50 . . C
H50A -.0593 .2456 -.2350 .106 Uiso d PR .50 . . H
H50B -.0652 .4027 -.1892 .106 Uiso d PR .50 . . H
H50C -.0157 .3573 -.2047 .106 Uiso d PR .50 . . H
C300 .0192(10) .299(3) .1115(16) .081(12) Uani d PD .50 . . C
H30A -.0063 .2499 .1303 .121 Uiso d PR .50 . . H
H30B .0429 .2283 .1062 .121 Uiso d PR .50 . . H
H30C .0346 .3701 .1686 .121 Uiso d PR .50 . . H
C400 -.0397(15) .493(5) .011(4) .055(11) Uani d PD .50 . . C
H40A -.0533 .5421 -.0595 .082 Uiso d PR .50 . . H
H40B -.0646 .4356 .0267 .082 Uiso d PR .50 . . H
H40C -.0270 .5642 .0694 .082 Uiso d PR .50 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 '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
C28 O1 C3 . . 118.8(5)
O1 C28 N1 . . 123.1(7)
O1 C28 C29 . . 113.2(6)
N1 C28 C29 . . 123.6(6)
C10 C1 C2 . . 114.4(6)
C3 C2 C1 . . 108.6(5)
O1 C3 C4 . . 110.3(6)
O1 C3 C2 . . 107.5(5)
C4 C3 C2 . . 111.7(6)
C3 C4 C5 . . 110.2(6)
C6 C5 C4 . . 120.3(6)
C6 C5 C10 . . 123.7(6)
C4 C5 C10 . . 116.0(6)
C5 C6 C7 . . 124.3(6)
C6 C7 C8 . . 113.6(5)
C14 C8 C9 . . 109.5(5)
C14 C8 C7 . . 110.8(5)
C9 C8 C7 . . 110.0(5)
C8 C9 C10 . . 112.4(5)
C8 C9 C11 . . 111.7(5)
C10 C9 C11 . . 113.3(5)
C1 C10 C5 . . 109.9(5)
C1 C10 C19 . . 109.4(6)
C5 C10 C19 . . 107.9(6)
C1 C10 C9 . . 108.5(5)
C5 C10 C9 . . 109.3(5)
C19 C10 C9 . . 111.9(5)
C12 C11 C9 . . 113.9(5)
C13 C12 C11 . . 110.3(6)
C12 C13 C17 . . 115.3(5)
C12 C13 C18 . . 111.2(6)
C17 C13 C18 . . 110.1(5)
C12 C13 C14 . . 106.3(5)
C17 C13 C14 . . 101.2(5)
C18 C13 C14 . . 112.3(5)
C15 C14 C8 . . 117.8(5)
C15 C14 C13 . . 103.3(5)
C8 C14 C13 . . 115.3(5)
C14 C15 C16 . . 103.2(5)
C15 C16 C17 . . 107.2(5)
C13 C17 C20 . . 118.6(5)
C13 C17 C16 . . 103.1(5)
C20 C17 C16 . . 111.9(5)
C21 C20 C22 . . 110.1(6)
C21 C20 C17 . . 113.4(5)
C22 C20 C17 . . 110.1(6)
C20 C22 C23 . . 114.0(6)
C22 C23 C24 . . 111.9(6)
C25 C24 C23 . . 115.5(6)
C26 C25 C24 . . 117.3(7)
C26 C25 C27 . . 111.5(7)
C24 C25 C27 . . 110.0(7)
C28 C29 Cl12 . . 107.7(6)
C28 C29 Cl13 . . 111.0(5)
Cl12 C29 Cl13 . . 109.6(4)
C28 C29 Cl11 . . 111.7(5)
Cl12 C29 Cl11 . . 107.6(4)
Cl13 C29 Cl11 . . 109.1(4)
O2 C100 O2 . 2 82.9(17)
O2 C100 C400 . 2 130.8(19)
O2 C100 C400 2 2 106(2)
O2 C100 C400 . . 106(2)
O2 C100 C400 2 . 130.8(19)
C400 C100 C400 2 . 103(4)
O2 C100 C200 . . 117(2)
O2 C100 C200 2 . 104(2)
C400 C100 C200 2 . 14(4)
C400 C100 C200 . . 112.5(14)
O2 C100 C200 . 2 104(2)
O2 C100 C200 2 2 117(2)
C400 C100 C200 2 2 112.5(14)
C400 C100 C200 . 2 14(4)
C200 C100 C200 . 2 124(4)
O2 C100 C300 . 2 25.1(9)
O2 C100 C300 2 2 98.1(15)
C400 C100 C300 2 2 107(2)
C400 C100 C300 . 2 110(2)
C200 C100 C300 . 2 94(2)
C200 C100 C300 2 2 114(2)
O2 C100 C300 . . 98.1(15)
O2 C100 C300 2 . 25.1(9)
C400 C100 C300 2 . 110(2)
C400 C100 C300 . . 107(2)
C200 C100 C300 . . 114(2)
C200 C100 C300 2 . 94(2)
C300 C100 C300 2 . 119(2)
C400 C200 C100 2 . 83(3)
C300 O2 C100 2 . 86.9(14)
C300 O2 C500 2 . 34(3)
C100 O2 C500 . . 107.5(17)
C300 C500 O2 2 . 22.4(17)
O2 C300 C500 2 2 123(5)
O2 C300 C100 2 . 68.0(12)
C500 C300 C100 2 . 133(3)
C200 C400 C100 2 . 83(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl11 C29 . 1.752(8) ?
Cl12 C29 . 1.749(8) ?
Cl13 C29 . 1.749(7) ?
O1 C28 . 1.277(9) ?
O1 C3 . 1.474(7) ?
N1 C28 . 1.291(10) ?
C28 C29 . 1.527(9) ?
C1 C10 . 1.530(10) ?
C1 C2 . 1.528(9) ?
C2 C3 . 1.502(10) ?
C3 C4 . 1.498(11) ?
C4 C5 . 1.519(9) ?
C5 C6 . 1.306(10) ?
C5 C10 . 1.544(9) ?
C6 C7 . 1.506(9) ?
C7 C8 . 1.536(8) ?
C8 C14 . 1.518(8) ?
C8 C9 . 1.529(9) ?
C9 C10 . 1.549(8) ?
C9 C11 . 1.557(8) ?
C10 C19 . 1.544(10) ?
C11 C12 . 1.548(9) ?
C12 C13 . 1.527(9) ?
C13 C17 . 1.546(8) ?
C13 C18 . 1.544(10) ?
C13 C14 . 1.552(8) ?
C14 C15 . 1.523(9) ?
C15 C16 . 1.559(8) ?
C16 C17 . 1.566(9) ?
C17 C20 . 1.551(9) ?
C20 C21 . 1.516(10) ?
C20 C22 . 1.531(9) ?
C22 C23 . 1.534(10) ?
C23 C24 . 1.521(9) ?
C24 C25 . 1.519(10) ?
C25 C26 . 1.510(9) ?
C25 C27 . 1.544(8) ?
C100 O2 . 1.439(10) ?
C100 O2 2 1.439(10) ?
C100 C400 2 1.543(10) ?
C100 C400 . 1.543(10) ?
C100 C200 . 1.544(10) ?
C100 C200 2 1.544(10) ?
C100 C300 2 1.550(10) ?
C100 C300 . 1.550(10) ?
C200 C400 2 .37(10) ?
O2 C300 2 .66(2) ?
O2 C500 . 1.446(10) ?
C500 C300 2 .98(3) ?
C300 O2 2 .66(2) ?
C300 C500 2 .98(3) ?
C400 C200 2 .37(10) ?
