#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:00:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180460 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/29/7212961.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7212961
loop_
_publ_author_name
'Drosihn, Susanne'
'Porzel, Andrea'
'Voigt, Brunhilde'
'Brandt, Wolfgang'
'Wagner, Christoph'
'Merzweiler, Kurt'
'Adam, Günter'
_publ_section_title
;
 Conformational studies of two new brassinosteroid analogues with a
 22,23-trans diol function
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              233
_journal_paper_doi               10.1039/a807440b
_journal_year                    1999
_chemical_formula_sum            'C28 H48 O4'
_chemical_formula_weight         448.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8955(17)
_cell_length_b                   11.486(2)
_cell_length_c                   28.835(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2615.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15893
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.074
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                3318
_reflns_number_total             4080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807440bsup1.cif
_cod_data_source_block           ipds434
_cod_database_code               7212961
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
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
O2 O 0.9502(2) 0.33578(15) 0.80776(5) 0.0529(4) Uani 1 1 d
H6 H 0.907(3) 0.399(2) 0.8089(9) 0.073(9) Uiso 1 1 d
O3 O 1.3525(2) -0.06467(14) 1.19978(5) 0.0563(4) Uani 1 1 d
H35 H 1.441(4) -0.101(3) 1.2016(10) 0.096(12) Uiso 1 1 d
C20 C 1.2515(2) -0.17839(17) 1.13370(6) 0.0383(4) Uani 1 1 d
H30 H 1.197(2) -0.2565(18) 1.1272(7) 0.039(5) Uiso 1 1 d
C10 C 1.0337(2) 0.10260(16) 0.92196(6) 0.0365(4) Uani 1 1 d
C4 C 0.8384(3) 0.2386(2) 0.87549(7) 0.0458(5) Uani 1 1 d
H8 H 0.801(2) 0.1763(19) 0.8569(7) 0.039(5) Uiso 1 1 d
H7 H 0.740(3) 0.293(2) 0.8766(7) 0.054(6) Uiso 1 1 d
C22 C 1.2455(2) -0.15983(17) 1.18657(6) 0.0390(4) Uani 1 1 d
H34 H 1.129(2) -0.1370(15) 1.1947(6) 0.033(4) Uiso 1 1 d
C3 C 0.9890(2) 0.29716(18) 0.85346(6) 0.0425(5) Uani 1 1 d
H5 H 1.019(2) 0.3668(18) 0.8725(7) 0.045(5) Uiso 1 1 d
C14 C 0.9812(2) 0.0004(2) 1.04920(6) 0.0426(5) Uani 1 1 d
H18 H 1.027(2) 0.0783(17) 1.0595(6) 0.036(5) Uiso 1 1 d
C9 C 1.0793(2) 0.07162(18) 0.97271(6) 0.0357(4) Uani 1 1 d
H13 H 1.105(2) 0.1423(18) 0.9871(6) 0.035(5) Uiso 1 1 d
C2 C 1.1392(3) 0.2159(2) 0.85102(7) 0.0479(5) Uani 1 1 d
H4 H 1.108(3) 0.155(2) 0.8297(8) 0.053(6) Uiso 1 1 d
H3 H 1.236(3) 0.2578(19) 0.8371(7) 0.052(6) Uiso 1 1 d
C5 C 0.8840(2) 0.19124(19) 0.92301(7) 0.0416(4) Uani 1 1 d
H9 H 0.922(2) 0.2538(17) 0.9396(7) 0.037(5) Uiso 1 1 d
C1 C 1.1828(2) 0.1631(2) 0.89806(7) 0.0447(5) Uani 1 1 d
H1 H 1.280(3) 0.108(2) 0.8927(8) 0.071(7) Uiso 1 1 d
H2 H 1.223(2) 0.2243(19) 0.9178(7) 0.042(5) Uiso 1 1 d
C17 C 1.1446(2) -0.08427(18) 1.10927(6) 0.0398(4) Uani 1 1 d
H23 H 1.194(2) -0.0079(19) 1.1162(6) 0.037(5) Uiso 1 1 d
C24 C 1.2042(3) -0.37868(17) 1.20605(7) 0.0449(5) Uani 1 1 d
H38 H 1.236(2) -0.3942(17) 1.1749(7) 0.044(5) Uiso 1 1 d
C8 C 0.9284(2) 0.0206(2) 0.99941(6) 0.0416(5) Uani 1 1 d
H12 H 0.898(2) -0.0546(18) 0.9849(7) 0.043(5) Uiso 1 1 d
C11 C 1.2357(3) -0.0064(2) 0.97820(7) 0.0482(5) Uani 1 1 d
H15 H 1.207(3) -0.079(2) 0.9630(8) 0.057(7) Uiso 1 1 d
H14 H 1.329(3) 0.037(2) 0.9628(9) 0.076(8) Uiso 1 1 d
C12 C 1.2807(3) -0.0323(2) 1.02879(7) 0.0460(5) Uani 1 1 d
H16 H 1.375(3) -0.0825(19) 1.0296(7) 0.053(6) Uiso 1 1 d
H17 H 1.298(3) 0.044(2) 1.0446(8) 0.055(6) Uiso 1 1 d
C23 C 1.2914(2) -0.26412(17) 1.21758(6) 0.0396(5) Uani 1 1 d
H36 H 1.257(2) -0.2433(17) 1.2504(7) 0.044(5) Uiso 1 1 d
C7 C 0.7740(3) 0.1020(3) 0.99694(9) 0.0670(8) Uani 1 1 d
H10 H 0.677(4) 0.062(2) 1.0107(10) 0.087(9) Uiso 1 1 d
H11 H 0.809(4) 0.174(3) 1.0140(11) 0.099(11) Uiso 1 1 d
O1 O 0.5960(2) 0.1406(3) 0.93315(8) 0.1274(11) Uani 1 1 d
C28 C 1.2704(4) -0.4778(2) 1.23638(10) 0.0664(7) Uani 1 1 d
H47 H 1.261(3) -0.458(2) 1.2674(10) 0.072(8) Uiso 1 1 d
H48 H 1.207(4) -0.555(3) 1.2263(10) 0.093(9) Uiso 1 1 d
H46 H 1.389(4) -0.484(3) 1.2307(10) 0.098(10) Uiso 1 1 d
C15 C 0.8496(3) -0.0415(3) 1.08365(9) 0.0648(7) Uani 1 1 d
H19 H 0.793(4) -0.102(3) 1.0704(10) 0.079(10) Uiso 1 1 d
H20 H 0.776(4) 0.024(3) 1.0941(9) 0.088(9) Uiso 1 1 d
C6 C 0.7364(3) 0.1427(2) 0.94908(8) 0.0638(7) Uani 1 1 d
C25 C 1.0098(3) -0.3673(2) 1.20807(9) 0.0647(7) Uani 1 1 d
H39 H 0.987(3) -0.308(3) 1.1881(9) 0.076(8) Uiso 1 1 d
C16 C 0.9558(3) -0.0844(3) 1.12464(8) 0.0644(7) Uani 1 1 d
H22 H 0.936(3) -0.043(2) 1.1511(10) 0.076(8) Uiso 1 1 d
H21 H 0.918(3) -0.162(2) 1.1336(8) 0.063(7) Uiso 1 1 d
C21 C 1.4338(3) -0.1833(2) 1.11639(8) 0.0504(5) Uani 1 1 d
H31 H 1.501(3) -0.2341(19) 1.1365(7) 0.051(6) Uiso 1 1 d
H33 H 1.439(3) -0.213(2) 1.0828(9) 0.065(6) Uiso 1 1 d
H32 H 1.487(3) -0.104(2) 1.1182(7) 0.061(6) Uiso 1 1 d
C26 C 0.9417(5) -0.3401(5) 1.25638(15) 0.1022(12) Uani 1 1 d
H44 H 0.814(6) -0.329(4) 1.2536(16) 0.168(17) Uiso 1 1 d
H43 H 0.995(6) -0.265(4) 1.2707(14) 0.152(17) Uiso 1 1 d
H45 H 0.975(6) -0.408(4) 1.2740(14) 0.142(17) Uiso 1 1 d
C27 C 0.9211(7) -0.4736(5) 1.18826(19) 0.1220(16) Uani 1 1 d
H42 H 0.944(5) -0.535(4) 1.2103(14) 0.133(15) Uiso 1 1 d
H41 H 0.818(6) -0.460(4) 1.1824(15) 0.139(16) Uiso 1 1 d
H40 H 0.982(5) -0.486(4) 1.1526(15) 0.158(17) Uiso 1 1 d
O4 O 1.47279(17) -0.27493(15) 1.21657(5) 0.0561(4) Uani 1 1 d
H37 H 1.508(3) -0.286(2) 1.2431(9) 0.057(7) Uiso 1 1 d
C13 C 1.1311(2) -0.08445(16) 1.05559(6) 0.0382(4) Uani 1 1 d
C19 C 0.9839(4) -0.0067(2) 0.89508(8) 0.0583(6) Uani 1 1 d
H28 H 0.958(3) 0.005(2) 0.8631(8) 0.064(6) Uiso 1 1 d
H29 H 0.875(4) -0.037(2) 0.9081(9) 0.084(9) Uiso 1 1 d
H27 H 1.080(4) -0.066(3) 0.8970(9) 0.092(9) Uiso 1 1 d
C18 C 1.0924(4) -0.2079(2) 1.03826(9) 0.0588(6) Uani 1 1 d
H25 H 1.061(3) -0.210(2) 1.0066(10) 0.071(7) Uiso 1 1 d
H24 H 1.194(4) -0.257(2) 1.0445(10) 0.091(9) Uiso 1 1 d
H26 H 0.996(4) -0.237(2) 1.0533(10) 0.086(9) Uiso 1 1 d
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'
