# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1620
_database_code_depnum_ccdc_archive 'CCDC 1431101'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;
_audit_creation_date             2015-10-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
(R)-6-((3R,4R,5R)-3,5-dimethoxy-2,4,6-trimethylheptan-2-yl)-5,6-dihydro-2H-pyran-2-one
_chemical_formula_moiety         'C17 H30 O4'
_chemical_formula_sum            'C17 H30 O4'
_chemical_formula_weight         298.41
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C17 H30 O4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.89706(6)
_cell_length_b                   13.34116(17)
_cell_length_c                   9.57590(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.1494(9)
_cell_angle_gamma                90
_cell_volume                     878.814(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10493
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9270
_cell_measurement_theta_min      4.5800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.3504
_exptl_crystal_size_mid          0.2982
_exptl_crystal_size_min          0.167
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14785
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.985
_diffrn_reflns_theta_min         4.630
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -129.00  -34.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  178.0000   60.0000 135

#__ type_ start__ end____ width___ exp.time_
  2 omega -117.00   -6.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -38.0000   60.0000 158

#__ type_ start__ end____ width___ exp.time_
  3 omega -116.00   -5.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000    0.0000 158

#__ type_ start__ end____ width___ exp.time_
  4 omega   57.00  128.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  178.0000   60.0000 102

#__ type_ start__ end____ width___ exp.time_
  5 omega  -46.00   73.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  -77.0000  -90.0000 171

#__ type_ start__ end____ width___ exp.time_
  6 omega   71.00  176.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000   60.0000 151

#__ type_ start__ end____ width___ exp.time_
  7 omega   71.00  176.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000   30.0000 151

#__ type_ start__ end____ width___ exp.time_
  8 omega   71.00  176.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000    0.0000 151

#__ type_ start__ end____ width___ exp.time_
  9 omega   76.00  177.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000   30.0000 145

#__ type_ start__ end____ width___ exp.time_
 10 omega   71.00  176.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000  -30.0000 151

#__ type_ start__ end____ width___ exp.time_
 11 omega   20.00  108.20   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000   60.0000 126

#__ type_ start__ end____ width___ exp.time_
 12 omega   28.00   98.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -45.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
 13 omega   74.00  176.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000   60.0000 147

#__ type_ start__ end____ width___ exp.time_
 14 omega   74.00  176.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000    0.0000 147

#__ type_ start__ end____ width___ exp.time_
 15 omega  100.00  177.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000    0.0000 110

#__ type_ start__ end____ width___ exp.time_
 16 omega   74.00  176.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000   90.0000 147

#__ type_ start__ end____ width___ exp.time_
 17 omega  100.00  177.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000  150.0000 110

#__ type_ start__ end____ width___ exp.time_
 18 omega   76.00  177.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000   60.0000 145

#__ type_ start__ end____ width___ exp.time_
 19 omega   74.00  176.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000  -30.0000 147

#__ type_ start__ end____ width___ exp.time_
 20 omega  100.00  177.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000  -90.0000 110

#__ type_ start__ end____ width___ exp.time_
 21 omega   71.00  176.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   67.0000   21.9399 151

#__ type_ start__ end____ width___ exp.time_
 22 omega   27.00   90.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -35.0000  132.0000 91

#__ type_ start__ end____ width___ exp.time_
 23 omega   76.00  177.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000    0.0000 145

#__ type_ start__ end____ width___ exp.time_
 24 omega   76.00  177.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000   90.0000 145

#__ type_ start__ end____ width___ exp.time_
 25 omega   74.00  176.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000   30.0000 147

#__ type_ start__ end____ width___ exp.time_
 26 omega -116.00   -5.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000 -150.0000 158

#__ type_ start__ end____ width___ exp.time_
 27 omega  -50.00   41.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   38.0000   60.0000 130

#__ type_ start__ end____ width___ exp.time_
 28 omega -122.00   -2.30   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000  -60.0000 171

#__ type_ start__ end____ width___ exp.time_
 29 omega  -50.00   41.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   38.0000  120.0000 130

#__ type_ start__ end____ width___ exp.time_
 30 omega -122.00   -2.30   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000   90.0000 171

#__ type_ start__ end____ width___ exp.time_
 31 omega -116.00   -5.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000  -60.0000 158

#__ type_ start__ end____ width___ exp.time_
 32 omega -116.00   -5.40   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000 -180.0000 158

#__ type_ start__ end____ width___ exp.time_
 33 omega -122.00   -2.30   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000 -180.0000 171

#__ type_ start__ end____ width___ exp.time_
 34 omega   26.00  138.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   15.0000 -120.0000 161
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1534142000
_diffrn_orient_matrix_UB_12      -0.0437050000
_diffrn_orient_matrix_UB_13      0.0923106000
_diffrn_orient_matrix_UB_21      -0.1296464000
_diffrn_orient_matrix_UB_22      -0.0268095000
_diffrn_orient_matrix_UB_23      -0.1326191000
_diffrn_orient_matrix_UB_31      0.0983434000
_diffrn_orient_matrix_UB_32      -0.1033613000
_diffrn_orient_matrix_UB_33      -0.0045751000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                2947
_reflns_number_total             3014
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 
;
 Flack x determined using 1343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3014
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0662P)²+0.0493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0927
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C7(H7), C5(H5), C4(H4), C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.2273(3) -0.52304(16) -0.3000(2) 0.0345(5) Uani 1 1 d . . . . .
H11 H -0.1835 -0.5200 -0.2004 0.041 Uiso 1 1 calc R . . . .
C12 C -0.1149(3) -0.44477(17) -0.3748(2) 0.0409(5) Uani 1 1 d . . . . .
H12A H 0.0234 -0.4546 -0.3534 0.049 Uiso 1 1 calc R . . . .
H12B H -0.1418 -0.4517 -0.4752 0.049 Uiso 1 1 calc R . . . .
C13 C -0.1711(3) -0.34263(18) -0.3302(2) 0.0426(5) Uani 1 1 d . . . . .
H13 H -0.0837 -0.2899 -0.3356 0.051 Uiso 1 1 calc R . . . .
C14 C -0.3440(3) -0.32564(19) -0.2827(2) 0.0434(5) Uani 1 1 d . . . . .
H14 H -0.3721 -0.2626 -0.2481 0.052 Uiso 1 1 calc R . . . .
C15 C -0.4913(3) -0.40490(18) -0.2842(3) 0.0435(5) Uani 1 1 d . . . . .
C8 C -0.2081(3) -0.63238(16) -0.3476(2) 0.0342(5) Uani 1 1 d . . . . .
C7 C -0.3175(3) -0.69947(16) -0.2462(2) 0.0341(5) Uani 1 1 d . . . . .
H7 H -0.4518 -0.6751 -0.2487 0.041 Uiso 1 1 calc R . . . .
C5 C -0.3265(3) -0.81293(15) -0.2852(2) 0.0341(5) Uani 1 1 d . . . . .
H5 H -0.2546 -0.8217 -0.3689 0.041 Uiso 1 1 calc R . . . .
C4 C -0.2304(3) -0.88103(16) -0.17016(19) 0.0342(5) Uani 1 1 d . . . . .
H4 H -0.2769 -0.8615 -0.0798 0.041 Uiso 1 1 calc R . . . .
C16 C 0.0677(4) -0.8439(2) -0.0325(3) 0.0542(6) Uani 1 1 d . . . . .
H16A H 0.1004 -0.7741 -0.0253 0.081 Uiso 1 1 calc GR . . . .
H16B H 0.1840 -0.8834 -0.0194 0.081 Uiso 1 1 calc GR . . . .
H16C H -0.0186 -0.8609 0.0381 0.081 Uiso 1 1 calc GR . . . .
C3 C -0.2677(3) -0.99334(18) -0.1930(2) 0.0389(5) Uani 1 1 d . . . . .
H3 H -0.4084 -1.0043 -0.1959 0.047 Uiso 1 1 calc R . . . .
C1 C -0.1740(4) -1.0536(2) -0.0706(3) 0.0557(6) Uani 1 1 d . . . . .
H1A H -0.0356 -1.0447 -0.0661 0.084 Uiso 1 1 calc GR . . . .
H1B H -0.2044 -1.1234 -0.0838 0.084 Uiso 1 1 calc GR . . . .
H1C H -0.2232 -1.0308 0.0151 0.084 Uiso 1 1 calc GR . . . .
C2 C -0.1971(4) -1.03074(19) -0.3305(3) 0.0506(6) Uani 1 1 d . . . . .
H2A H -0.2626 -0.9948 -0.4069 0.076 Uiso 1 1 calc GR . . . .
H2B H -0.2245 -1.1010 -0.3405 0.076 Uiso 1 1 calc GR . . . .
H2C H -0.0595 -1.0200 -0.3309 0.076 Uiso 1 1 calc GR . . . .
C17 C -0.3669(5) -0.6653(3) -0.0064(3) 0.0684(8) Uani 1 1 d . . . . .
H17A H -0.4329 -0.6030 -0.0256 0.103 Uiso 1 1 calc GR . . . .
H17B H -0.2997 -0.6627 0.0849 0.103 Uiso 1 1 calc GR . . . .
H17C H -0.4599 -0.7190 -0.0095 0.103 Uiso 1 1 calc GR . . . .
C6 C -0.5385(3) -0.84243(19) -0.3247(3) 0.0486(6) Uani 1 1 d . . . . .
H6A H -0.6099 -0.8425 -0.2423 0.073 Uiso 1 1 calc GR . . . .
H6B H -0.5425 -0.9081 -0.3657 0.073 Uiso 1 1 calc GR . . . .
H6C H -0.5958 -0.7951 -0.3910 0.073 Uiso 1 1 calc GR . . . .
C10 C 0.0090(3) -0.65933(17) -0.3396(2) 0.0399(5) Uani 1 1 d . . . . .
H10A H 0.0679 -0.6412 -0.2492 0.060 Uiso 1 1 calc GR . . . .
H10B H 0.0714 -0.6235 -0.4109 0.060 Uiso 1 1 calc GR . . . .
H10C H 0.0234 -0.7301 -0.3537 0.060 Uiso 1 1 calc GR . . . .
C9 C -0.2982(3) -0.64560(19) -0.4982(2) 0.0433(5) Uani 1 1 d . . . . .
H9A H -0.2749 -0.7126 -0.5295 0.065 Uiso 1 1 calc GR . . . .
H9B H -0.2402 -0.5986 -0.5587 0.065 Uiso 1 1 calc GR . . . .
H9C H -0.4357 -0.6338 -0.5005 0.065 Uiso 1 1 calc GR . . . .
O3 O -0.43559(19) -0.49870(11) -0.31222(16) 0.0412(4) Uani 1 1 d . . . . .
O1 O -0.0249(2) -0.86365(12) -0.16682(15) 0.0402(4) Uani 1 1 d . . . . .
O2 O -0.2318(2) -0.68210(12) -0.10778(14) 0.0402(4) Uani 1 1 d . . . . .
O4 O -0.6601(2) -0.38818(16) -0.2694(3) 0.0710(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 C12 1.512(3) . ?
C11 C8 1.537(3) . ?
C11 O3 1.469(2) . ?
C12 C13 1.488(3) . ?
C13 C14 1.326(3) . ?
C14 C15 1.466(3) . ?
C15 O3 1.342(3) . ?
C15 O4 1.203(3) . ?
C8 C7 1.555(3) . ?
C8 C10 1.536(3) . ?
C8 C9 1.539(3) . ?
C7 C5 1.559(3) . ?
C7 O2 1.431(2) . ?
C5 C4 1.540(3) . ?
C5 C6 1.535(3) . ?
C4 C3 1.533(3) . ?
C4 O1 1.434(2) . ?
C16 O1 1.419(3) . ?
C3 C1 1.526(3) . ?
C3 C2 1.520(3) . ?
C17 O2 1.411(3) . ?

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
_geom_angle_publ_flag
C12 C11 C8 117.16(17) . . ?
O3 C11 C12 109.99(16) . . ?
O3 C11 C8 106.93(15) . . ?
C13 C12 C11 110.05(19) . . ?
C14 C13 C12 121.0(2) . . ?
C13 C14 C15 120.9(2) . . ?
O3 C15 C14 117.79(19) . . ?
O4 C15 C14 122.7(2) . . ?
O4 C15 O3 119.3(2) . . ?
C11 C8 C7 107.74(16) . . ?
C11 C8 C9 110.44(17) . . ?
C10 C8 C11 108.19(16) . . ?
C10 C8 C7 110.45(16) . . ?
C10 C8 C9 110.25(17) . . ?
C9 C8 C7 109.74(17) . . ?
C8 C7 C5 114.96(16) . . ?
O2 C7 C8 107.36(15) . . ?
O2 C7 C5 112.68(16) . . ?
C4 C5 C7 113.19(16) . . ?
C6 C5 C7 109.19(17) . . ?
C6 C5 C4 112.22(17) . . ?
C3 C4 C5 114.53(16) . . ?
O1 C4 C5 107.11(15) . . ?
O1 C4 C3 108.45(16) . . ?
C1 C3 C4 110.36(18) . . ?
C2 C3 C4 112.55(18) . . ?
C2 C3 C1 110.3(2) . . ?
C15 O3 C11 118.86(16) . . ?
C16 O1 C4 115.44(17) . . ?
C17 O2 C7 114.46(19) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4 -2 3 0.0921 -4.0000 -2.0000 3.0000 0.9780 0.1743 -0.2004
-1 -8 2 0.1384 -1.0000 -8.0000 2.0000 0.6877 0.0789 0.7194
4 0 -3 0.0632 4.0000 -0.0000 -3.0000 -0.8906 -0.1207 0.4071
3 3 -3 0.0697 3.0000 3.0000 -3.0000 -0.8683 -0.0715 -0.0013
0 8 -2 0.1381 -0.0000 8.0000 -2.0000 -0.5343 0.0508 -0.8177
2 6 4 0.1106 2.0000 6.0000 4.0000 -0.1998 -0.9506 -0.4418
2 -8 -1 0.1628 2.0000 -8.0000 -1.0000 -0.0495 0.0878 1.0282
3 -3 3 0.2078 3.0000 -3.0000 3.0000 -0.0522 -0.7064 0.5914
-3 -1 -4 0.1225 -3.0000 -1.0000 -4.0000 0.1347 0.9462 -0.1734
2 0 -5 0.0620 2.0000 -0.0000 -5.0000 -0.7684 0.4038 0.2196
1 5 -5 0.0703 1.0000 5.0000 -5.0000 -0.8335 0.3994 -0.3956
-2 0 5 0.1183 -2.0000 0.0000 5.0000 0.7684 -0.4038 -0.2196
-1 -6 5 0.1314 -1.0000 -6.0000 5.0000 0.8772 -0.3726 0.4989
-1 4 5 0.1263 -1.0000 4.0000 5.0000 0.4401 -0.6407 -0.5347
1 -2 6 0.1694 1.0000 -2.0000 6.0000 0.4879 -0.8717 0.2776

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1659
_database_code_depnum_ccdc_archive 'CCDC 1431102'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
(R)-5-((3R,4R,5R)-3,5-dimethoxy-2,4,6-trimethylheptan-2-yl)furan-2(5H)-one
_chemical_formula_moiety         'C16 H28 O4'
_chemical_formula_sum            'C16 H28 O4'
_chemical_formula_weight         284.38
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.71157(9)
_cell_length_b                   12.95291(17)
_cell_length_c                   20.1272(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.8329(11)
_cell_angle_gamma                90
_cell_volume                     1733.42(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       monocristal
_exptl_crystal_F_000             624
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29956
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.986
_diffrn_reflns_theta_min         4.070
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5625
_reflns_number_total             6023
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    ?
_refine_diff_density_max         0.147
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 
;
 Flack x determined using 2534 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1006P)²+0.0167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1378
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H7(0.061) H11(0.073) H5(0.073) H4(0.077) H12(0.089) H10A(0.107)
 H10B(0.107) H10C(0.107) H9A(0.108) H9B(0.108) H9C(0.108) H13(0.099) H3(0.104)
 H15A(0.152) H15B(0.152) H15C(0.152) H6A(0.148) H6B(0.148) H6C(0.148)
 H16A(0.151) H16B(0.151) H16C(0.151) H1A(0.172) H1B(0.172) H1C(0.172)
 H2A(0.178) H2B(0.178) H2C(0.178) H23(0.082) H27(0.089) H26A(0.117) H26B(0.117)
 H26C(0.117) H20(0.092) H25A(0.14) H25B(0.14) H25C(0.14) H19(0.12) H21(0.096)
 H29(0.118) H28(0.109) H31A(0.142) H31B(0.142) H31C(0.142) H17A(0.182)
 H22A(0.188) H22B(0.188) H22C(0.188) H18A(0.187) H18B(0.187) H18C(0.187)
 H32A(0.218) H32B(0.218) H32C(0.218)
 Fixed X: H7(-0.6753) H11(-0.9532) H5(-0.9051) H4(-0.8138) H12(-1.1603) H10A(-
 1.2028) H10B(-1.2608) H10C(-1.2049) H9A(-0.9439) H9B(-0.9904) H9C(-0.7709)
 H13(-0.9194) H3(-0.7479) H15A(-1.0552) H15B(-1.2766) H15C(-1.1064) H6A(-
 0.5151) H6B(-0.6095) H6C(-0.5582) H16A(-0.6145) H16B(-0.702) H16C(-0.5739)
 H1A(-0.9323) H1B(-0.9997) H1C(-1.1354) H2A(-1.113) H2B(-0.9479) H2C(-0.9042)
 H23(-0.3031) H27(-0.5838) H26A(-0.8272) H26B(-0.8903) H26C(-0.8367) H20(-
 0.4305) H25A(-0.5605) H25B(-0.6342) H25C(-0.4071) H21(-0.5558) H29(-0.5572)
 H28(-0.7933) H31A(-0.7211) H31B(-0.8852) H31C(-0.6592) H17A(-0.5057) H22A(-
 0.1541) H22B(-0.2681) H22C(-0.2097) H18A(-0.6014) H18B(-0.6531) H18C(-0.7864)
 H32A(-0.2532) H32B(-0.2926) H32C(-0.1751)
 Fixed Y: H7(-0.8505) H11(-0.8317) H5(-0.8464) H4(-1.0562) H12(-0.6685) H10A(-
 0.8788) H10B(-0.7629) H10C(-0.8332) H9A(-0.6983) H9B(-0.6331) H9C(-0.6719)
 H13(-0.5533) H3(-1.0221) H15A(-1.1028) H15B(-1.1052) H15C(-1.1646) H6A(-
 0.9312) H6B(-0.8827) H6C(-0.8123) H16A(-0.9659) H16B(-1.0756) H16C(-1.017)
 H1A(-0.8758) H1B(-0.9591) H1C(-0.9354) H2A(-1.1321) H2B(-1.1438) H2C(-1.1814)
 H23(-0.4354) H27(-0.5137) H26A(-0.491) H26B(-0.3878) H26C(-0.3882) H20(-
 0.5612) H25A(-0.2542) H25B(-0.2461) H25C(-0.2682) H21(-0.3617) H29(-0.3246)
 H28(-0.38) H31A(-0.6587) H31B(-0.6578) H31C(-0.6775) H17A(-0.6066) H22A(-
 0.4239) H22B(-0.3366) H22C(-0.3206) H18A(-0.3168) H18B(-0.362) H18C(-0.3906)
 H32A(-0.6211) H32B(-0.6804) H32C(-0.5755)
 Fixed Z: H7(-0.3423) H11(-0.4672) H5(-0.2458) H4(-0.2653) H12(-0.4817) H10A(-
 0.398) H10B(-0.3891) H10C(-0.3259) H9A(-0.2828) H9B(-0.3487) H9C(-0.3251) H13(-
 0.5177) H3(-0.151) H15A(-0.3541) H15B(-0.3374) H15C(-0.2916) H6A(-0.237) H6B(-
 0.1771) H6C(-0.2358) H16A(-0.4275) H16B(-0.4156) H16C(-0.3564) H1A(-0.1392)
 H1B(-0.0903) H1C(-0.1583) H2A(-0.1727) H2B(-0.11) H2C(-0.1807) H23(-0.2074)
 H27(-0.3237) H26A(-0.2464) H26B(-0.2841) H26C(-0.2059) H20(-0.0814) H25A(-
 0.2079) H25B(-0.285) H25C(-0.2594) H21(-0.1274) H29(-0.4634) H28(-0.3927)
 H31A(-0.1594) H31B(-0.1109) H31C(-0.0824) H17A(0.0327) H22A(-0.0865) H22B(-
 0.0531) H22C(-0.1252) H18A(-0.0198) H18B(0.0481) H18C(-0.0195) H32A(-0.2524)
 H32B(-0.1876) H32C(-0.1815)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.8447(3) -0.96362(13) -0.37880(8) 0.0602(4) Uani 1 1 d . . . . .
O3 O -0.7074(3) -0.74655(16) -0.44281(9) 0.0669(4) Uani 1 1 d . . . . .
O1 O -1.0980(3) -1.01453(18) -0.27814(11) 0.0760(5) Uani 1 1 d . . . . .
C7 C -0.8118(3) -0.87424(17) -0.33826(10) 0.0510(5) Uani 1 1 d . . . . .
H7 H -0.6753 -0.8505 -0.3423 0.061 Uiso 1 1 calc R U . . .
C8 C -0.9558(4) -0.78760(18) -0.36779(11) 0.0541(5) Uani 1 1 d . . . . .
C11 C -0.9164(4) -0.7694(2) -0.44073(12) 0.0608(5) Uani 1 1 d . . . . .
H11 H -0.9532 -0.8317 -0.4672 0.073 Uiso 1 1 calc R U . . .
C5 C -0.8160(4) -0.8976(2) -0.26221(12) 0.0611(5) Uani 1 1 d . . . . .
H5 H -0.9051 -0.8464 -0.2458 0.073 Uiso 1 1 calc R U . . .
O4 O -0.5274(4) -0.6232(3) -0.48396(18) 0.1097(10) Uani 1 1 d . . . . .
C4 C -0.8961(4) -1.0037(2) -0.24684(13) 0.0644(6) Uani 1 1 d . . . . .
H4 H -0.8138 -1.0562 -0.2653 0.077 Uiso 1 1 calc R U . . .
C14 C -0.6895(5) -0.6566(3) -0.47513(17) 0.0776(8) Uani 1 1 d . . . . .
C12 C -1.0218(4) -0.6785(3) -0.47517(15) 0.0741(7) Uani 1 1 d . . . . .
H12 H -1.1603 -0.6685 -0.4817 0.089 Uiso 1 1 calc R U . . .
C10 C -1.1766(4) -0.8185(3) -0.37044(15) 0.0713(7) Uani 1 1 d . . . . .
H10A H -1.2028 -0.8788 -0.3980 0.107 Uiso 1 1 calc R U . . .
H10B H -1.2608 -0.7629 -0.3891 0.107 Uiso 1 1 calc R U . . .
H10C H -1.2049 -0.8332 -0.3259 0.107 Uiso 1 1 calc R U . . .
C9 C -0.9111(5) -0.6885(2) -0.32736(15) 0.0723(7) Uani 1 1 d . . . . .
H9A H -0.9439 -0.6983 -0.2828 0.108 Uiso 1 1 calc R U . . .
H9B H -0.9904 -0.6331 -0.3487 0.108 Uiso 1 1 calc R U . . .
H9C H -0.7709 -0.6719 -0.3251 0.108 Uiso 1 1 calc R U . . .
C13 C -0.8898(5) -0.6150(3) -0.49483(17) 0.0827(9) Uani 1 1 d . . . . .
H13 H -0.9194 -0.5533 -0.5177 0.099 Uiso 1 1 calc R U . . .
C3 C -0.8894(6) -1.0238(3) -0.17104(17) 0.0865(9) Uani 1 1 d . . . . .
H3 H -0.7479 -1.0221 -0.1510 0.104 Uiso 1 1 calc R U . . .
C15 C -1.1372(7) -1.1040(3) -0.3186(2) 0.1011(12) Uani 1 1 d . . . . .
H15A H -1.0552 -1.1028 -0.3541 0.152 Uiso 1 1 calc R U . . .
H15B H -1.2766 -1.1052 -0.3374 0.152 Uiso 1 1 calc R U . . .
H15C H -1.1064 -1.1646 -0.2916 0.152 Uiso 1 1 calc R U . . .
C6 C -0.6051(6) -0.8792(4) -0.22452(16) 0.0990(12) Uani 1 1 d . . . . .
H6A H -0.5151 -0.9312 -0.2370 0.148 Uiso 1 1 calc R U . . .
H6B H -0.6095 -0.8827 -0.1771 0.148 Uiso 1 1 calc R U . . .
H6C H -0.5582 -0.8123 -0.2358 0.148 Uiso 1 1 calc R U . . .
C16 C -0.6702(6) -1.0091(3) -0.3959(3) 0.1005(12) Uani 1 1 d . . . . .
H16A H -0.6145 -0.9659 -0.4275 0.151 Uiso 1 1 calc R U . . .
H16B H -0.7020 -1.0756 -0.4156 0.151 Uiso 1 1 calc R U . . .
H16C H -0.5739 -1.0170 -0.3564 0.151 Uiso 1 1 calc R U . . .
C1 C -0.9993(9) -0.9409(4) -0.13655(19) 0.1148(15) Uani 1 1 d . . . . .
H1A H -0.9323 -0.8758 -0.1392 0.172 Uiso 1 1 calc R U . . .
H1B H -0.9997 -0.9591 -0.0903 0.172 Uiso 1 1 calc R U . . .
H1C H -1.1354 -0.9354 -0.1583 0.172 Uiso 1 1 calc R U . . .
C2 C -0.9712(9) -1.1301(4) -0.1573(3) 0.1184(15) Uani 1 1 d . . . . .
H2A H -1.1130 -1.1321 -0.1727 0.178 Uiso 1 1 calc R U . . .
H2B H -0.9479 -1.1438 -0.1100 0.178 Uiso 1 1 calc R U . . .
H2C H -0.9042 -1.1814 -0.1807 0.178 Uiso 1 1 calc R U . . .
O5 O -0.7193(3) -0.53313(18) -0.10541(11) 0.0765(5) Uani 1 1 d . . . . .
O6 O -0.4639(3) -0.55984(17) -0.20746(12) 0.0771(5) Uani 1 1 d . . . . .
C23 C -0.4398(4) -0.4518(2) -0.19885(15) 0.0685(6) Uani 1 1 d . . . . .
H23 H -0.3031 -0.4354 -0.2074 0.082 Uiso 1 1 calc R U . . .
O8 O -0.1643(4) -0.3655(4) -0.40843(16) 0.1338(16) Uani 1 1 d . . . . .
C27 C -0.5487(4) -0.4402(3) -0.32218(15) 0.0745(7) Uani 1 1 d . . . . .
H27 H -0.5838 -0.5137 -0.3237 0.089 Uiso 1 1 calc R U . . .
C26 C -0.8053(4) -0.4178(3) -0.24690(17) 0.0780(7) Uani 1 1 d . . . . .
H26A H -0.8272 -0.4910 -0.2464 0.117 Uiso 1 1 calc R U . . .
H26B H -0.8903 -0.3878 -0.2841 0.117 Uiso 1 1 calc R U . . .
H26C H -0.8367 -0.3882 -0.2059 0.117 Uiso 1 1 calc R U . . .
C24 C -0.5850(4) -0.3961(2) -0.25381(15) 0.0700(6) Uani 1 1 d . . . . .
C20 C -0.5206(5) -0.5019(3) -0.08020(15) 0.0763(7) Uani 1 1 d . . . . .
H20 H -0.4305 -0.5612 -0.0814 0.092 Uiso 1 1 calc R U . . .
C30 C -0.3231(5) -0.3825(4) -0.39021(18) 0.0961(11) Uani 1 1 d . . . . .
C25 C -0.5428(6) -0.2804(3) -0.2513(2) 0.0937(10) Uani 1 1 d . . . . .
H25A H -0.5605 -0.2542 -0.2079 0.140 Uiso 1 1 calc R U . . .
H25B H -0.6342 -0.2461 -0.2850 0.140 Uiso 1 1 calc R U . . .
H25C H -0.4071 -0.2682 -0.2594 0.140 Uiso 1 1 calc R U . . .
C19 C -0.5184(7) -0.4681(4) -0.00638(19) 0.0999(12) Uani 1 1 d . . . . .
H19 H -0.383(9) -0.459(4) 0.017(3) 0.120 Uiso 1 1 d . U . . .
C21 C -0.4549(5) -0.4167(3) -0.12515(16) 0.0802(8) Uani 1 1 d . . . . .
H21 H -0.5558 -0.3617 -0.1274 0.096 Uiso 1 1 calc R U . . .
C29 C -0.5254(6) -0.3574(4) -0.42223(19) 0.0987(12) Uani 1 1 d . . . . .
H29 H -0.5572 -0.3246 -0.4634 0.118 Uiso 1 1 calc R U . . .
C28 C -0.6547(5) -0.3886(4) -0.38345(17) 0.0907(10) Uani 1 1 d . . . . .
H28 H -0.7933 -0.3800 -0.3927 0.109 Uiso 1 1 calc R U . . .
C31 C -0.7485(7) -0.6404(3) -0.1153(2) 0.0945(10) Uani 1 1 d . . . . .
H31A H -0.7211 -0.6587 -0.1594 0.142 Uiso 1 1 calc R U . . .
H31B H -0.8852 -0.6578 -0.1109 0.142 Uiso 1 1 calc R U . . .
H31C H -0.6592 -0.6775 -0.0824 0.142 Uiso 1 1 calc R U . . .
C17 C -0.5802(9) -0.5572(5) 0.0358(2) 0.1212(17) Uani 1 1 d . . . . .
H17A H -0.5057 -0.6066 0.0327 0.182 Uiso 1 1 calc R U . . .
C22 C -0.2528(9) -0.3701(5) -0.0946(2) 0.1250(19) Uani 1 1 d . . . . .
H22A H -0.1541 -0.4239 -0.0865 0.188 Uiso 1 1 calc R U . . .
H22B H -0.2681 -0.3366 -0.0531 0.188 Uiso 1 1 calc R U . . .
H22C H -0.2097 -0.3206 -0.1252 0.188 Uiso 1 1 calc R U . . .
O7 O -0.3383(3) -0.4295(2) -0.33095(12) 0.0874(7) Uani 1 1 d . . . . .
C18 C -0.6520(10) -0.3760(5) 0.0013(3) 0.1246(17) Uani 1 1 d . . . . .
H18A H -0.6014 -0.3168 -0.0198 0.187 Uiso 1 1 calc R U . . .
H18B H -0.6531 -0.3620 0.0481 0.187 Uiso 1 1 calc R U . . .
H18C H -0.7864 -0.3906 -0.0195 0.187 Uiso 1 1 calc R U . . .
C32 C -0.2818(9) -0.6135(5) -0.2072(4) 0.145(2) Uani 1 1 d . . . . .
H32A H -0.2532 -0.6211 -0.2524 0.218 Uiso 1 1 calc R U . . .
H32B H -0.2926 -0.6804 -0.1876 0.218 Uiso 1 1 calc R U . . .
H32C H -0.1751 -0.5755 -0.1815 0.218 Uiso 1 1 calc R U . . .
H17B H -0.733(8) -0.582(4) 0.018(2) 0.104(13) Uiso 1 1 d . . . . .
H17C H -0.565(8) -0.546(4) 0.077(3) 0.109(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C7 1.416(3) . ?
O2 C16 1.395(4) . ?
O3 C11 1.440(3) . ?
O3 C14 1.347(4) . ?
O1 C4 1.422(3) . ?
O1 C15 1.421(5) . ?
C7 C8 1.546(3) . ?
C7 C5 1.564(3) . ?
C8 C11 1.545(3) . ?
C8 C10 1.529(4) . ?
C8 C9 1.528(3) . ?
C11 C12 1.494(4) . ?
C5 C4 1.523(4) . ?
C5 C6 1.531(4) . ?
O4 C14 1.206(4) . ?
C4 C3 1.542(4) . ?
C14 C13 1.452(5) . ?
C12 C13 1.309(5) . ?
C3 C1 1.523(7) . ?
C3 C2 1.521(6) . ?
O5 C20 1.420(4) . ?
O5 C31 1.413(5) . ?
O6 C23 1.417(4) . ?
O6 C32 1.405(5) . ?
C23 C24 1.549(4) . ?
C23 C21 1.567(4) . ?
O8 C30 1.194(4) . ?
C27 C24 1.540(4) . ?
C27 C28 1.494(5) . ?
C27 O7 1.453(3) . ?
C26 C24 1.530(4) . ?
C24 C25 1.525(5) . ?
C20 C19 1.547(5) . ?
C20 C21 1.530(5) . ?
C30 C29 1.458(5) . ?
C30 O7 1.355(4) . ?
C19 C17 1.524(7) . ?
C19 C18 1.513(8) . ?
C21 C22 1.535(5) . ?
C29 C28 1.308(5) . ?

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
_geom_angle_publ_flag
C16 O2 C7 114.6(2) . . ?
C14 O3 C11 110.1(2) . . ?
C15 O1 C4 115.2(3) . . ?
O2 C7 C8 109.36(17) . . ?
O2 C7 C5 112.55(18) . . ?
C8 C7 C5 115.00(19) . . ?
C11 C8 C7 107.30(18) . . ?
C10 C8 C7 112.1(2) . . ?
C10 C8 C11 107.3(2) . . ?
C9 C8 C7 109.8(2) . . ?
C9 C8 C11 109.3(2) . . ?
C9 C8 C10 110.9(2) . . ?
O3 C11 C8 110.64(19) . . ?
O3 C11 C12 103.1(2) . . ?
C12 C11 C8 115.5(2) . . ?
C4 C5 C7 115.3(2) . . ?
C4 C5 C6 111.6(3) . . ?
C6 C5 C7 108.4(2) . . ?
O1 C4 C5 109.9(2) . . ?
O1 C4 C3 108.6(2) . . ?
C5 C4 C3 112.9(3) . . ?
O3 C14 C13 108.2(3) . . ?
O4 C14 O3 121.5(3) . . ?
O4 C14 C13 130.3(3) . . ?
C13 C12 C11 109.7(3) . . ?
C12 C13 C14 108.9(3) . . ?
C1 C3 C4 112.4(3) . . ?
C2 C3 C4 111.7(4) . . ?
C2 C3 C1 110.3(4) . . ?
C31 O5 C20 115.8(3) . . ?
C32 O6 C23 113.8(3) . . ?
O6 C23 C24 108.8(2) . . ?
O6 C23 C21 112.4(2) . . ?
C24 C23 C21 115.2(3) . . ?
C28 C27 C24 117.1(3) . . ?
O7 C27 C24 110.4(2) . . ?
O7 C27 C28 102.6(2) . . ?
C27 C24 C23 107.8(2) . . ?
C26 C24 C23 111.8(2) . . ?
C26 C24 C27 106.6(2) . . ?
C25 C24 C23 109.7(3) . . ?
C25 C24 C27 110.1(3) . . ?
C25 C24 C26 110.8(3) . . ?
O5 C20 C19 108.0(3) . . ?
O5 C20 C21 109.0(3) . . ?
C21 C20 C19 113.4(3) . . ?
O8 C30 C29 129.8(4) . . ?
O8 C30 O7 122.0(3) . . ?
O7 C30 C29 108.2(3) . . ?
C17 C19 C20 110.7(4) . . ?
C18 C19 C20 113.2(4) . . ?
C18 C19 C17 109.3(5) . . ?
C20 C21 C23 114.3(3) . . ?
C20 C21 C22 110.9(3) . . ?
C22 C21 C23 109.0(3) . . ?
C28 C29 C30 108.7(3) . . ?
C29 C28 C27 110.5(3) . . ?
C30 O7 C27 109.9(3) . . ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1666
_database_code_depnum_ccdc_archive 'CCDC 1431103'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(S)-6-((3R,4R,5R)-3,5-bis((tert-butyldimethylsilyl)oxy)-2,4,6-trimethylheptan-2-yl)-5,6-dihydro-2H-pyran-2-one
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H54 O4 Si2'
_chemical_formula_sum            'C27 H54 O4 Si2'
_chemical_formula_weight         498.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.6989(5)
_cell_length_b                   7.5129(2)
_cell_length_c                   15.8965(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.187(3)
_cell_angle_gamma                90
_cell_volume                     1592.91(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       fiber
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_F_000             552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6951
_exptl_crystal_size_mid          0.0984
_exptl_crystal_size_min          0.0580
_exptl_absorpt_coefficient_mu    1.208
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.26199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26331
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.314
_diffrn_reflns_theta_max         65.990
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             5480
_reflns_number_gt                5128
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_max     0.978
_reflns_Friedel_fraction_full    0.942

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1242P)²+0.1892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2159 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5480
_refine_ls_number_parameters     382
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1761
_refine_ls_wR_factor_gt          0.1684
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si2 Si -0.63700(7) -0.75340(13) -0.75960(6) 0.0446(3) Uani 1 1 d . . . . .
Si1 Si -0.13009(13) -0.5726(4) -0.78581(14) 0.0547(9) Uani 0.606(7) 1 d . . P A
1
O2 O -0.51507(19) -0.7902(4) -0.73799(15) 0.0446(6) Uani 1 1 d . . . . .
C15 C -0.2017(4) -0.4863(8) -0.5002(3) 0.0718(14) Uani 1 1 d . . . . .
C14 C -0.1114(5) -0.5907(11) -0.4634(4) 0.0890(18) Uani 1 1 d . . . . .
H14 H -0.0503 -0.5335 -0.4436 0.107 Uiso 1 1 calc R U . . .
C13 C -0.1168(5) -0.7651(11) -0.4586(4) 0.0882(18) Uani 1 1 d . . . . .
H13 H -0.0604 -0.8287 -0.4309 0.106 Uiso 1 1 calc R U . . .
C12 C -0.2112(5) -0.8634(8) -0.4963(3) 0.0742(14) Uani 1 1 d . . . . .
H12A H -0.2499 -0.8803 -0.4529 0.089 Uiso 1 1 calc R U . . .
H12B H -0.1957 -0.9795 -0.5166 0.089 Uiso 1 1 calc R U . . .
O1 O -0.2460(2) -0.6385(5) -0.83446(19) 0.0572(8) Uani 1 1 d . . . . .
C11 C -0.2714(3) -0.7546(7) -0.5715(2) 0.0533(9) Uani 1 1 d . . . . .
H11 H -0.2328 -0.7495 -0.6163 0.064 Uiso 1 1 calc R U . . .
C10 C -0.4418(4) -0.8308(8) -0.5465(3) 0.0648(12) Uani 1 1 d . . . . .
H10A H -0.5080 -0.8704 -0.5740 0.097 Uiso 1 1 calc R U . . .
H10B H -0.4454 -0.7138 -0.5232 0.097 Uiso 1 1 calc R U . . .
H10C H -0.4129 -0.9114 -0.5007 0.097 Uiso 1 1 calc R U . . .
C9 C -0.3653(4) -1.0155(6) -0.6454(3) 0.0595(10) Uani 1 1 d . . . . .
H9A H -0.4275 -1.0521 -0.6826 0.089 Uiso 1 1 calc R U . . .
H9B H -0.3484 -1.0949 -0.5970 0.089 Uiso 1 1 calc R U . . .
H9C H -0.3132 -1.0183 -0.6769 0.089 Uiso 1 1 calc R U . . .
C8 C -0.3759(3) -0.8258(6) -0.6132(2) 0.0488(9) Uani 1 1 d . . . . .
O3 O -0.2830(2) -0.5727(5) -0.54288(19) 0.0595(7) Uani 1 1 d . . . . .
C1 C -0.4197(5) -0.7528(11) -0.9552(3) 0.0897(18) Uani 1 1 d . . . . .
H1A H -0.3640 -0.7039 -0.9747 0.135 Uiso 1 1 calc R U . . .
H1B H -0.4632 -0.6582 -0.9459 0.135 Uiso 1 1 calc R U . . .
H1C H -0.4561 -0.8330 -0.9981 0.135 Uiso 1 1 calc R U . . .
O4 O -0.2067(4) -0.3265(7) -0.4897(3) 0.0971(14) Uani 1 1 d . . . . .
C27 C -0.6706(6) -1.0859(10) -0.8395(5) 0.0915(18) Uani 1 1 d . . . . .
H27A H -0.7007 -1.0324 -0.8941 0.137 Uiso 1 1 calc R U . . .
H27B H -0.6943 -1.2060 -0.8384 0.137 Uiso 1 1 calc R U . . .
H27C H -0.5990 -1.0863 -0.8317 0.137 Uiso 1 1 calc R U . . .
C26 C -0.8134(4) -0.9528(10) -0.7885(6) 0.101(2) Uani 1 1 d . . . . .
H26A H -0.8340 -0.8937 -0.8432 0.151 Uiso 1 1 calc R U . . .
H26B H -0.8313 -0.8813 -0.7443 0.151 Uiso 1 1 calc R U . . .
H26C H -0.8461 -1.0663 -0.7911 0.151 Uiso 1 1 calc R U . . .
C25 C -0.6676(5) -1.0825(9) -0.6819(4) 0.0839(16) Uani 1 1 d . . . . .
H25A H -0.7097 -1.1851 -0.6835 0.126 Uiso 1 1 calc R U . . .
H25B H -0.6743 -1.0066 -0.6349 0.126 Uiso 1 1 calc R U . . .
H25C H -0.5990 -1.1198 -0.6737 0.126 Uiso 1 1 calc R U . . .
C24 C -0.6990(4) -0.9801(7) -0.7674(3) 0.0615(11) Uani 1 1 d . . . . .
C6 C -0.4260(4) -0.4636(6) -0.8003(3) 0.0584(10) Uani 1 1 d . . . . .
H6A H -0.3854 -0.4095 -0.8352 0.088 Uiso 1 1 calc R U . . .
H6B H -0.4437 -0.3758 -0.7625 0.088 Uiso 1 1 calc R U . . .
H6C H -0.4858 -0.5111 -0.8370 0.088 Uiso 1 1 calc R U . . .
C2 C -0.3235(6) -1.0155(9) -0.8901(4) 0.0859(17) Uani 1 1 d . . . . .
H2A H -0.3650 -1.0857 -0.9348 0.129 Uiso 1 1 calc R U . . .
H2B H -0.3043 -1.0854 -0.8384 0.129 Uiso 1 1 calc R U . . .
H2C H -0.2646 -0.9781 -0.9084 0.129 Uiso 1 1 calc R U . . .
C7 C -0.4306(3) -0.6997(5) -0.6884(2) 0.0432(8) Uani 1 1 d . . . . .
H7 H -0.4574 -0.6006 -0.6604 0.052 Uiso 1 1 calc R U . . .
C22 C -0.6802(4) -0.6368(8) -0.8665(3) 0.0710(13) Uani 1 1 d . . . . .
H22A H -0.6564 -0.7004 -0.9102 0.106 Uiso 1 1 calc R U . . .
H22B H -0.6542 -0.5177 -0.8621 0.106 Uiso 1 1 calc R U . . .
H22C H -0.7522 -0.6329 -0.8815 0.106 Uiso 1 1 calc R U . . .
C3 C -0.3820(3) -0.8517(7) -0.8722(3) 0.0585(11) Uani 1 1 d . . . . .
H3 H -0.4403 -0.8932 -0.8517 0.070 Uiso 1 1 calc R U . . .
C4 C -0.3155(3) -0.7414(6) -0.7991(2) 0.0471(8) Uani 1 1 d . . . . .
H4 H -0.2760 -0.8260 -0.7580 0.057 Uiso 1 1 calc R U . . .
C5 C -0.3670(3) -0.6139(6) -0.7466(2) 0.0450(8) Uani 1 1 d . . . . .
H5 H -0.3118 -0.5542 -0.7064 0.054 Uiso 1 1 calc R U . . .
C23 C -0.6733(4) -0.6138(7) -0.6742(3) 0.0670(12) Uani 1 1 d . . . . .
H23A H -0.7419 -0.5769 -0.6934 0.101 Uiso 1 1 calc R U . . .
H23B H -0.6308 -0.5108 -0.6632 0.101 Uiso 1 1 calc R U . . .
H23C H -0.6658 -0.6821 -0.6221 0.101 Uiso 1 1 calc R U . . .
C16 C -0.058(2) -0.757(4) -0.721(2) 0.094(8) Uani 0.606(7) 1 d . . P A 1
H16A H -0.0646 -0.8628 -0.7553 0.141 Uiso 0.606(7) 1 calc R U P A 1
H16B H -0.0847 -0.7781 -0.6708 0.141 Uiso 0.606(7) 1 calc R U P A 1
H16C H 0.0110 -0.7239 -0.7031 0.141 Uiso 0.606(7) 1 calc R U P A 1
C21 C -0.1326(17) -0.355(4) -0.9291(10) 0.081(4) Uani 0.606(7) 1 d . . P A 1
H21A H -0.1127 -0.3392 -0.9827 0.121 Uiso 0.606(7) 1 calc R U P A 1
H21B H -0.1202 -0.2476 -0.8958 0.121 Uiso 0.606(7) 1 calc R U P A 1
H21C H -0.2028 -0.3831 -0.9406 0.121 Uiso 0.606(7) 1 calc R U P A 1
C20 C 0.0381(12) -0.458(4) -0.8472(10) 0.098(6) Uani 0.606(7) 1 d . . P A 1
H20A H 0.0631 -0.4145 -0.8951 0.147 Uiso 0.606(7) 1 calc R U P A 1
H20B H 0.0758 -0.5608 -0.8231 0.147 Uiso 0.606(7) 1 calc R U P A 1
H20C H 0.0449 -0.3667 -0.8039 0.147 Uiso 0.606(7) 1 calc R U P A 1
C18 C -0.0722(5) -0.5079(14) -0.8782(6) 0.066(2) Uani 0.606(7) 1 d . . P A 1
C17 C -0.1276(18) -0.384(3) -0.7150(13) 0.093(7) Uani 0.606(7) 1 d . . P A 1
H17A H -0.0647 -0.3226 -0.7082 0.140 Uiso 0.606(7) 1 calc R U P A 1
H17B H -0.1355 -0.4238 -0.6596 0.140 Uiso 0.606(7) 1 calc R U P A 1
H17C H -0.1813 -0.3038 -0.7395 0.140 Uiso 0.606(7) 1 calc R U P A 1
C20' C -0.107(3) -0.345(7) -0.895(2) 0.128(14) Uani 0.394(7) 1 d . . P A 2
H20D H -0.0871 -0.4039 -0.9415 0.191 Uiso 0.394(7) 1 calc R U P A 2
H20E H -0.0771 -0.2289 -0.8865 0.191 Uiso 0.394(7) 1 calc R U P A 2
H20F H -0.1790 -0.3329 -0.9081 0.191 Uiso 0.394(7) 1 calc R U P A 2
C21' C -0.109(3) -0.354(4) -0.735(3) 0.119(15) Uani 0.394(7) 1 d . . P A 2
H21D H -0.0699 -0.2488 -0.7192 0.178 Uiso 0.394(7) 1 calc R U P A 2
H21E H -0.1003 -0.4334 -0.6869 0.178 Uiso 0.394(7) 1 calc R U P A 2
H21F H -0.1789 -0.3220 -0.7534 0.178 Uiso 0.394(7) 1 calc R U P A 2
C19 C -0.0780(12) -0.665(2) -0.9412(10) 0.104(4) Uani 0.606(7) 1 d . . P A 1
H19A H -0.1463 -0.7037 -0.9595 0.156 Uiso 0.606(7) 1 calc R U P A 1
H19B H -0.0373 -0.7609 -0.9128 0.156 Uiso 0.606(7) 1 calc R U P A 1
H19C H -0.0539 -0.6275 -0.9906 0.156 Uiso 0.606(7) 1 calc R U P A 1
C16' C -0.0974(16) -0.779(4) -0.9275(15) 0.106(7) Uani 0.394(7) 1 d . . P A 2
H16D H -0.1546 -0.7676 -0.9750 0.158 Uiso 0.394(7) 1 calc R U P A 2
H16E H -0.0813 -0.9022 -0.9172 0.158 Uiso 0.394(7) 1 calc R U P A 2
H16F H -0.0413 -0.7180 -0.9412 0.158 Uiso 0.394(7) 1 calc R U P A 2
C17' C -0.074(3) -0.819(6) -0.732(4) 0.101(14) Uani 0.394(7) 1 d . . P A 2
H17D H -0.1081 -0.9321 -0.7385 0.151 Uiso 0.394(7) 1 calc R U P A 2
H17E H -0.0841 -0.7609 -0.6811 0.151 Uiso 0.394(7) 1 calc R U P A 2
H17F H -0.0040 -0.8375 -0.7278 0.151 Uiso 0.394(7) 1 calc R U P A 2
C19' C 0.043(2) -0.459(5) -0.797(3) 0.162(18) Uani 0.394(7) 1 d . . P A 2
H19D H 0.0645 -0.5809 -0.7912 0.243 Uiso 0.394(7) 1 calc R U P A 2
H19E H 0.0717 -0.3958 -0.7448 0.243 Uiso 0.394(7) 1 calc R U P A 2
H19F H 0.0642 -0.4053 -0.8446 0.243 Uiso 0.394(7) 1 calc R U P A 2
C18' C -0.0745(11) -0.451(3) -0.8140(15) 0.088(5) Uani 0.394(7) 1 d . . P A 2
Si1' Si -0.1266(2) -0.6776(6) -0.8286(3) 0.0609(14) Uani 0.394(7) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si2 O2 1.650(3) . ?
Si2 C23 1.870(5) . ?
Si2 C22 1.883(5) . ?
Si2 C24 1.895(5) . ?
Si1 O1 1.674(3) . ?
Si1 C17 1.81(2) . ?
Si1 C16 1.87(3) . ?
Si1 C18 1.885(8) . ?
O2 C7 1.417(5) . ?
C15 O4 1.216(8) . ?
C15 O3 1.333(6) . ?
C15 C14 1.469(9) . ?
C14 C13 1.316(11) . ?
C13 C12 1.491(9) . ?
C12 C11 1.525(6) . ?
O1 C4 1.437(5) . ?
O1 Si1' 1.643(4) . ?
C11 O3 1.460(6) . ?
C11 C8 1.531(6) . ?
C10 C8 1.542(6) . ?
C9 C8 1.532(7) . ?
C8 C7 1.575(5) . ?
C1 C3 1.500(8) . ?
C27 C24 1.516(8) . ?
C26 C24 1.540(7) . ?
C25 C24 1.536(8) . ?
C6 C5 1.531(6) . ?
C2 C3 1.530(8) . ?
C7 C5 1.549(5) . ?
C3 C4 1.544(6) . ?
C4 C5 1.543(6) . ?
C21 C18 1.53(2) . ?
C20 C18 1.526(19) . ?
C18 C19 1.54(2) . ?
C20' C18' 1.49(4) . ?
C21' C18' 1.61(5) . ?
C16' Si1' 1.87(2) . ?
C17' Si1' 1.87(5) . ?
C19' C18' 1.57(3) . ?
C18' Si1' 1.837(19) . ?

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
_geom_angle_publ_flag
O2 Si2 C23 111.5(2) . . ?
O2 Si2 C22 111.17(19) . . ?
C23 Si2 C22 108.2(3) . . ?
O2 Si2 C24 106.27(19) . . ?
C23 Si2 C24 111.2(3) . . ?
C22 Si2 C24 108.4(3) . . ?
O1 Si1 C17 113.7(8) . . ?
O1 Si1 C16 111.1(9) . . ?
C17 Si1 C16 107.8(13) . . ?
O1 Si1 C18 103.8(3) . . ?
C17 Si1 C18 109.3(7) . . ?
C16 Si1 C18 111.1(9) . . ?
C7 O2 Si2 134.0(2) . . ?
O4 C15 O3 119.0(6) . . ?
O4 C15 C14 122.8(6) . . ?
O3 C15 C14 118.2(6) . . ?
C13 C14 C15 120.1(6) . . ?
C14 C13 C12 121.7(6) . . ?
C13 C12 C11 108.3(5) . . ?
C4 O1 Si1' 128.4(3) . . ?
C4 O1 Si1 128.4(2) . . ?
O3 C11 C12 109.6(3) . . ?
O3 C11 C8 107.7(3) . . ?
C12 C11 C8 115.9(4) . . ?
C11 C8 C9 108.6(4) . . ?
C11 C8 C10 110.3(3) . . ?
C9 C8 C10 108.8(4) . . ?
C11 C8 C7 110.7(3) . . ?
C9 C8 C7 111.8(3) . . ?
C10 C8 C7 106.6(3) . . ?
C15 O3 C11 118.5(4) . . ?
C27 C24 C25 109.8(5) . . ?
C27 C24 C26 109.2(5) . . ?
C25 C24 C26 109.0(5) . . ?
C27 C24 Si2 109.4(4) . . ?
C25 C24 Si2 111.2(4) . . ?
C26 C24 Si2 108.2(4) . . ?
O2 C7 C5 111.5(3) . . ?
O2 C7 C8 108.7(3) . . ?
C5 C7 C8 117.9(3) . . ?
C1 C3 C2 108.9(4) . . ?
C1 C3 C4 115.0(5) . . ?
C2 C3 C4 109.1(4) . . ?
O1 C4 C5 107.7(4) . . ?
O1 C4 C3 108.9(3) . . ?
C5 C4 C3 118.4(3) . . ?
C6 C5 C4 113.9(3) . . ?
C6 C5 C7 110.1(3) . . ?
C4 C5 C7 117.0(3) . . ?
C20 C18 C21 111.2(14) . . ?
C20 C18 C19 107.4(13) . . ?
C21 C18 C19 106.8(13) . . ?
C20 C18 Si1 111.9(7) . . ?
C21 C18 Si1 109.4(10) . . ?
C19 C18 Si1 110.0(8) . . ?
C20' C18' C19' 105(2) . . ?
C20' C18' C21' 110(3) . . ?
C19' C18' C21' 111(3) . . ?
C20' C18' Si1' 111(2) . . ?
C19' C18' Si1' 110.0(17) . . ?
C21' C18' Si1' 110.0(16) . . ?
O1 Si1' C18' 101.3(6) . . ?
O1 Si1' C17' 109.8(14) . . ?
C18' Si1' C17' 111.0(16) . . ?
O1 Si1' C16' 115.2(8) . . ?
C18' Si1' C16' 109.3(12) . . ?
C17' Si1' C16' 110(2) . . ?

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.063

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1704
_database_code_depnum_ccdc_archive 'CCDC 1431104'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;
_audit_creation_date             2015-10-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
(3R,4R,5R)-2,4,6,6-tetramethyloct-7-ene-3,5-diol
_chemical_formula_moiety         'C12 H24 O2'
_chemical_formula_sum            'C12 H24 O2'
_chemical_formula_weight         200.31
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H25 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   6.3617(3)
_cell_length_b                   10.0016(3)
_cell_length_c                   20.4847(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1303.39(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.6950
_cell_measurement_theta_min      4.2740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.7354
_exptl_crystal_size_mid          0.0654
_exptl_crystal_size_min          0.0517
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11491
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.856
_diffrn_reflns_theta_min         4.317
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -122.00   20.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -19.0000  -90.0000 355

#__ type_ start__ end____ width___ exp.time_
  2 omega -129.00  -35.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  178.0000   90.0000 235

#__ type_ start__ end____ width___ exp.time_
  3 omega   57.00  129.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.7307  178.0000   60.0000 180

#__ type_ start__ end____ width___ exp.time_
  4 omega   25.00  115.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524 -111.0000  150.0000 225

#__ type_ start__ end____ width___ exp.time_
  5 omega   28.00   98.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -45.0000  120.0000 175

#__ type_ start__ end____ width___ exp.time_
  6 omega   28.00   98.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -45.0000  150.0000 175

#__ type_ start__ end____ width___ exp.time_
  7 omega  100.00  178.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000 -150.0000 195

#__ type_ start__ end____ width___ exp.time_
  8 omega   26.00   90.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000  -30.0000 160

#__ type_ start__ end____ width___ exp.time_
  9 omega   74.00  178.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000  -90.0000 260

#__ type_ start__ end____ width___ exp.time_
 10 omega -116.00   -6.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000  150.0000 275

#__ type_ start__ end____ width___ exp.time_
 11 omega -122.00   -2.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -77.0000   90.0000 300

#__ type_ start__ end____ width___ exp.time_
 12 omega   76.00  178.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000  120.0000 255

#__ type_ start__ end____ width___ exp.time_
 13 omega   20.00  108.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000  -60.0000 220

#__ type_ start__ end____ width___ exp.time_
 14 omega   69.00  177.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   30.0000 -150.0000 270

#__ type_ start__ end____ width___ exp.time_
 15 omega   69.00  177.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   30.0000   60.0000 270

#__ type_ start__ end____ width___ exp.time_
 16 omega -122.00   -2.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -77.0000  -90.0000 300

#__ type_ start__ end____ width___ exp.time_
 17 omega  -49.00   41.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307   37.0000   90.0000 225

#__ type_ start__ end____ width___ exp.time_
 18 omega   74.00  178.00   0.4000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000  -30.0000 260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0627214000
_diffrn_orient_matrix_UB_12      -0.1485291000
_diffrn_orient_matrix_UB_13      0.0031666000
_diffrn_orient_matrix_UB_21      0.0899808000
_diffrn_orient_matrix_UB_22      0.0090507000
_diffrn_orient_matrix_UB_23      -0.0697320000
_diffrn_orient_matrix_UB_31      0.2157756000
_diffrn_orient_matrix_UB_32      0.0397197000
_diffrn_orient_matrix_UB_33      0.0280991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                2271
_reflns_number_total             2530
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 
;
 Flack x determined using 860 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0732P)²+0.2898P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1639
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C2(H2A,H2B,H2C),
 C1(H1A,H1B,H1C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.2827(3) 0.1431(2) 0.06206(9) 0.0432(5) Uani 1 1 d . . . . .
H2 H 0.1975 0.1318 0.0325 0.065 Uiso 1 1 calc GR . . . .
O1 O 0.4847(3) 0.3648(2) 0.03403(10) 0.0463(5) Uani 1 1 d . . . . .
H1 H 0.4852 0.2835 0.0394 0.069 Uiso 1 1 calc GR . . . .
C4 C 0.2774(5) 0.4155(3) 0.04525(12) 0.0381(6) Uani 1 1 d . . . . .
H4 H 0.1852 0.3794 0.0112 0.046 Uiso 1 1 calc R . . . .
C5 C 0.1966(5) 0.3653(3) 0.11121(12) 0.0398(6) Uani 1 1 d . . . . .
H5 H 0.2954 0.3955 0.1448 0.048 Uiso 1 1 calc R . . . .
C7 C 0.1817(4) 0.2100(3) 0.11580(12) 0.0389(6) Uani 1 1 d . . . . .
H7 H 0.0324 0.1859 0.1148 0.047 Uiso 1 1 calc R . . . .
C8 C 0.2772(5) 0.1505(3) 0.17942(13) 0.0467(7) Uani 1 1 d . . . . .
C3 C 0.2845(6) 0.5673(3) 0.03714(15) 0.0481(7) Uani 1 1 d . . . . .
H3 H 0.1402 0.6005 0.0415 0.058 Uiso 1 1 calc R . . . .
C11 C 0.1718(6) 0.2127(4) 0.23761(15) 0.0611(9) Uani 1 1 d . . . . .
H11 H 0.0261 0.2059 0.2388 0.073 Uiso 1 1 calc R . . . .
C9 C 0.5142(6) 0.1694(4) 0.18065(16) 0.0591(9) Uani 1 1 d . . . . .
H9A H 0.5753 0.1267 0.1432 0.089 Uiso 1 1 calc GR . . . .
H9B H 0.5705 0.1302 0.2197 0.089 Uiso 1 1 calc GR . . . .
H9C H 0.5465 0.2631 0.1798 0.089 Uiso 1 1 calc GR . . . .
C6 C -0.0200(6) 0.4255(4) 0.12729(19) 0.0635(10) Uani 1 1 d . . . . .
H6A H -0.0071 0.5206 0.1322 0.095 Uiso 1 1 calc GR . . . .
H6B H -0.0716 0.3875 0.1672 0.095 Uiso 1 1 calc GR . . . .
H6C H -0.1164 0.4060 0.0925 0.095 Uiso 1 1 calc GR . . . .
C10 C 0.2253(8) 0.0004(4) 0.18091(19) 0.0738(12) Uani 1 1 d . . . . .
H10A H 0.0755 -0.0114 0.1812 0.111 Uiso 1 1 calc GR . . . .
H10B H 0.2846 -0.0390 0.2195 0.111 Uiso 1 1 calc GR . . . .
H10C H 0.2834 -0.0421 0.1430 0.111 Uiso 1 1 calc GR . . . .
C2 C 0.4154(8) 0.6357(4) 0.0891(2) 0.0716(11) Uani 1 1 d . . . . .
H2A H 0.3569 0.6172 0.1313 0.107 Uiso 1 1 calc GR . . . .
H2B H 0.4152 0.7305 0.0816 0.107 Uiso 1 1 calc GR . . . .
H2C H 0.5570 0.6028 0.0872 0.107 Uiso 1 1 calc GR . . . .
C1 C 0.3609(8) 0.6048(4) -0.03100(19) 0.0698(11) Uani 1 1 d . . . . .
H1A H 0.5082 0.5855 -0.0347 0.105 Uiso 1 1 calc GR . . . .
H1B H 0.3379 0.6985 -0.0383 0.105 Uiso 1 1 calc GR . . . .
H1C H 0.2847 0.5541 -0.0630 0.105 Uiso 1 1 calc GR . . . .
C12 C 0.2570(10) 0.2740(5) 0.28597(18) 0.0852(15) Uani 1 1 d . . . . .
H12A H 0.4022 0.2842 0.2877 0.102 Uiso 1 1 calc R . . . .
H12B H 0.1735 0.3083 0.3193 0.102 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C7 1.440(3) . ?
O1 C4 1.432(4) . ?
C4 C5 1.530(4) . ?
C4 C3 1.528(4) . ?
C5 C7 1.559(4) . ?
C5 C6 1.539(5) . ?
C7 C8 1.556(4) . ?
C8 C11 1.502(5) . ?
C8 C9 1.519(5) . ?
C8 C10 1.538(5) . ?
C3 C2 1.514(5) . ?
C3 C1 1.525(5) . ?
C11 C12 1.285(6) . ?

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
_geom_angle_publ_flag
O1 C4 C5 109.6(2) . . ?
O1 C4 C3 107.9(2) . . ?
C3 C4 C5 115.6(2) . . ?
C4 C5 C7 113.6(2) . . ?
C4 C5 C6 111.2(3) . . ?
C6 C5 C7 108.8(3) . . ?
O2 C7 C5 112.9(2) . . ?
O2 C7 C8 106.8(2) . . ?
C8 C7 C5 114.1(2) . . ?
C11 C8 C7 109.4(3) . . ?
C11 C8 C9 112.2(3) . . ?
C11 C8 C10 107.0(3) . . ?
C9 C8 C7 110.7(3) . . ?
C9 C8 C10 109.5(3) . . ?
C10 C8 C7 107.8(3) . . ?
C2 C3 C4 112.8(3) . . ?
C2 C3 C1 110.9(3) . . ?
C1 C3 C4 110.7(2) . . ?
C12 C11 C8 128.4(4) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -2 -13 0.0327 0.0004 -2.0006 -12.9954 0.2560 0.8881 -0.4445
0 2 13 0.0327 -0.0004 2.0006 12.9954 -0.2560 -0.8881 0.4445
4 1 -1 0.2656 3.9932 0.9930 -1.0010 0.0998 0.4381 0.8730
-4 -1 1 0.4474 -3.9932 -0.9930 1.0010 -0.0998 -0.4381 -0.8730
0 6 -5 0.0350 0.0264 6.0140 -4.9878 -0.9074 0.4046 0.1044
0 -6 5 0.0167 -0.0264 -6.0140 4.9878 0.9074 -0.4046 -0.1044
0 6 4 0.0383 0.0207 6.0115 4.0068 -0.8789 -0.2231 0.3558
0 6 4 0.0415 0.0207 6.0115 4.0068 -0.8789 -0.2231 0.3558
0 -6 -4 0.0210 -0.0207 -6.0115 -4.0068 0.8789 0.2231 -0.3558

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1705
_database_code_depnum_ccdc_archive 'CCDC 1431105'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;
_audit_creation_date             2015-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
(3S,4S,5S)-2,4,6,6-tetramethyloct-7-ene-3,5-diol
_chemical_formula_moiety         'C12 H24 O2'
_chemical_formula_sum            'C12 H24 O2'
_chemical_formula_weight         200.31
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H24 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   6.35866(12)
_cell_length_b                   9.99503(17)
_cell_length_c                   20.4733(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1301.18(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6950
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.0000
_cell_measurement_theta_min      4.2650
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.3547
_exptl_crystal_size_mid          0.0972
_exptl_crystal_size_min          0.0753
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.955
_diffrn_reflns_theta_min         4.319
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -122.00   20.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -19.0000 -180.0000 355

#__ type_ start__ end____ width___ exp.time_
  2 omega   57.00  129.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.7307  178.0000    0.0000 180

#__ type_ start__ end____ width___ exp.time_
  3 omega   26.00   90.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000   60.0000 160

#__ type_ start__ end____ width___ exp.time_
  4 omega   26.00   90.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000  120.0000 160

#__ type_ start__ end____ width___ exp.time_
  5 omega   28.00  140.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -61.0000  -30.0000 280

#__ type_ start__ end____ width___ exp.time_
  6 omega   25.00  115.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524 -111.0000  -30.0000 225

#__ type_ start__ end____ width___ exp.time_
  7 omega   26.00   90.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -30.0000  -30.0000 160

#__ type_ start__ end____ width___ exp.time_
  8 omega   20.00  108.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000    0.0000 220

#__ type_ start__ end____ width___ exp.time_
  9 omega -116.00   -6.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000   90.0000 275

#__ type_ start__ end____ width___ exp.time_
 10 omega -116.00   -6.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307  -57.0000  -30.0000 275

#__ type_ start__ end____ width___ exp.time_
 11 omega   26.00  178.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   15.0000  150.0000 380

#__ type_ start__ end____ width___ exp.time_
 12 omega   26.00  178.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   15.0000  -60.0000 380

#__ type_ start__ end____ width___ exp.time_
 13 omega   20.00  108.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000  150.0000 220

#__ type_ start__ end____ width___ exp.time_
 14 omega   71.00  177.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000    0.0000 265

#__ type_ start__ end____ width___ exp.time_
 15 omega  -49.00   41.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7307   37.0000    0.0000 225

#__ type_ start__ end____ width___ exp.time_
 16 omega   57.00  129.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.7307  178.0000 -180.0000 180

#__ type_ start__ end____ width___ exp.time_
 17 omega  100.00  178.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  111.0000   30.0000 195

#__ type_ start__ end____ width___ exp.time_
 18 omega   76.00  128.00   0.4000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   45.0000  -30.0000 130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0201607000
_diffrn_orient_matrix_UB_12      0.1533981000
_diffrn_orient_matrix_UB_13      -0.0038663000
_diffrn_orient_matrix_UB_21      -0.0541116000
_diffrn_orient_matrix_UB_22      0.0106300000
_diffrn_orient_matrix_UB_23      0.0731718000
_diffrn_orient_matrix_UB_31      0.2352880000
_diffrn_orient_matrix_UB_32      -0.0106223000
_diffrn_orient_matrix_UB_33      0.0171308000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2389
_reflns_number_total             2539
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 
;
 Flack x determined using 954 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0885P)²+0.0786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1282
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C),
 C3(H3A,H3B,H3C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.7173(2) 0.14298(13) 0.06206(6) 0.0435(3) Uani 1 1 d . . . . .
H2 H 0.8012 0.1346 0.0319 0.065 Uiso 1 1 calc GR . . . .
O1 O 0.5149(2) 0.36470(14) 0.03408(7) 0.0468(4) Uani 1 1 d . . . . .
C5 C 0.8040(3) 0.36555(18) 0.11125(8) 0.0398(4) Uani 1 1 d . . . . .
H5 H 0.7050 0.3959 0.1448 0.048 Uiso 1 1 calc R . . . .
C4 C 0.7233(3) 0.41537(17) 0.04517(8) 0.0386(4) Uani 1 1 d . . . . .
H4 H 0.8154 0.3791 0.0111 0.046 Uiso 1 1 calc R . . . .
C8 C 0.7229(3) 0.1504(2) 0.17938(9) 0.0467(4) Uani 1 1 d . . . . .
C7 C 0.8183(3) 0.20987(18) 0.11590(8) 0.0401(4) Uani 1 1 d . . . . .
H7 H 0.9676 0.1856 0.1149 0.048 Uiso 1 1 calc R . . . .
C2 C 0.7156(4) 0.56737(18) 0.03702(10) 0.0492(5) Uani 1 1 d . . . . .
H2A H 0.8599 0.6007 0.0415 0.059 Uiso 1 1 calc R . . . .
C11 C 0.8282(4) 0.2130(3) 0.23775(10) 0.0612(6) Uani 1 1 d . . . . .
H11 H 0.9740 0.2064 0.2389 0.073 Uiso 1 1 calc R . . . .
C10 C 0.7742(6) 0.0004(3) 0.18107(13) 0.0742(8) Uani 1 1 d . . . . .
H10A H 0.7160 -0.0423 0.1431 0.111 Uiso 1 1 calc GR . . . .
H10B H 0.7147 -0.0388 0.2197 0.111 Uiso 1 1 calc GR . . . .
H10C H 0.9240 -0.0117 0.1815 0.111 Uiso 1 1 calc GR . . . .
C9 C 0.4853(4) 0.1692(3) 0.18071(11) 0.0601(6) Uani 1 1 d . . . . .
H9A H 0.4528 0.2630 0.1792 0.090 Uiso 1 1 calc GR . . . .
H9B H 0.4294 0.1313 0.2201 0.090 Uiso 1 1 calc GR . . . .
H9C H 0.4238 0.1253 0.1436 0.090 Uiso 1 1 calc GR . . . .
C12 C 0.7435(6) 0.2741(3) 0.28610(12) 0.0842(9) Uani 1 1 d . . . . .
H12A H 0.5982 0.2841 0.2879 0.101 Uiso 1 1 calc R . . . .
H12B H 0.8273 0.3084 0.3193 0.101 Uiso 1 1 calc R . . . .
C6 C 1.0199(4) 0.4254(3) 0.12737(12) 0.0640(6) Uani 1 1 d . . . . .
H6A H 1.1173 0.4041 0.0931 0.096 Uiso 1 1 calc GR . . . .
H6B H 1.0698 0.3888 0.1679 0.096 Uiso 1 1 calc GR . . . .
H6C H 1.0077 0.5208 0.1313 0.096 Uiso 1 1 calc GR . . . .
C1 C 0.5839(5) 0.6356(2) 0.08931(14) 0.0724(7) Uani 1 1 d . . . . .
H1A H 0.4422 0.6026 0.0874 0.109 Uiso 1 1 calc GR . . . .
H1B H 0.5839 0.7305 0.0820 0.109 Uiso 1 1 calc GR . . . .
H1C H 0.6423 0.6168 0.1316 0.109 Uiso 1 1 calc GR . . . .
C3 C 0.6398(5) 0.6050(2) -0.03104(13) 0.0700(7) Uani 1 1 d . . . . .
H3A H 0.7142 0.5529 -0.0630 0.105 Uiso 1 1 calc GR . . . .
H3B H 0.6656 0.6983 -0.0386 0.105 Uiso 1 1 calc GR . . . .
H3C H 0.4918 0.5874 -0.0345 0.105 Uiso 1 1 calc GR . . . .
H1 H 0.526(6) 0.278(4) 0.0427(13) 0.074(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C7 1.440(2) . ?
O1 C4 1.437(2) . ?
C5 C4 1.530(2) . ?
C5 C7 1.562(3) . ?
C5 C6 1.533(3) . ?
C4 C2 1.529(2) . ?
C8 C7 1.552(2) . ?
C8 C11 1.506(3) . ?
C8 C10 1.535(3) . ?
C8 C9 1.523(3) . ?
C2 C1 1.521(3) . ?
C2 C3 1.522(3) . ?
C11 C12 1.282(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
_geom_angle_publ_flag
C4 C5 C7 113.43(14) . . ?
C4 C5 C6 111.32(16) . . ?
C6 C5 C7 108.89(17) . . ?
O1 C4 C5 109.53(14) . . ?
O1 C4 C2 107.68(16) . . ?
C2 C4 C5 115.49(15) . . ?
C11 C8 C7 109.39(17) . . ?
C11 C8 C10 107.0(2) . . ?
C11 C8 C9 112.07(19) . . ?
C10 C8 C7 108.04(17) . . ?
C9 C8 C7 110.81(16) . . ?
C9 C8 C10 109.3(2) . . ?
O2 C7 C5 112.95(14) . . ?
O2 C7 C8 106.80(14) . . ?
C8 C7 C5 114.18(15) . . ?
C1 C2 C4 112.73(17) . . ?
C1 C2 C3 111.1(2) . . ?
C3 C2 C4 110.82(16) . . ?
C12 C11 C8 128.6(3) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 2 13 0.0500 0.0069 1.9962 12.9988 0.2561 0.9720 0.2031
0 -2 -13 0.0472 -0.0069 -1.9962 -12.9988 -0.2561 -0.9720 -0.2031
3 -2 -8 0.1068 2.9958 -2.0004 -8.0007 -0.2155 -0.7688 0.5891
-2 2 10 0.0915 -1.9948 1.9989 10.0000 0.2278 0.8609 -0.3193
0 6 -5 0.0300 0.0000 6.0015 -5.0016 0.9400 -0.3022 -0.1494
0 -6 6 0.0427 0.0004 -6.0018 6.0015 -0.9439 0.3753 0.1667
1 -6 6 0.0435 1.0006 -6.0027 6.0010 -0.9238 0.3212 0.4020
1 6 -4 0.0576 1.0006 6.0003 -4.0022 0.9561 -0.2832 0.1031
-2 5 -6 0.0856 -2.0011 5.0036 -6.0002 0.7504 -0.2776 -0.6268
-4 -3 0 0.1832 -4.0017 -2.9964 0.0031 -0.5403 0.1849 -0.9097
-1 -5 -7 0.0600 -1.0054 -4.9971 -6.9976 -0.7598 -0.5107 -0.3034
1 -6 -6 0.0502 0.9949 -5.9992 -5.9985 -0.8770 -0.5565 0.1951
2 4 -9 0.0540 1.9976 4.0009 -9.0019 0.6888 -0.7243 0.2733

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1724
_database_code_depnum_ccdc_archive 'CCDC 1431106'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(S)-5-((3S,4S,5S)-3,5-dimethoxy-2,4,6-trimethylheptan-2-yl)furan-2(5H)-one
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H28 O4'
_chemical_formula_sum            'C16 H28 O4'
_chemical_formula_weight         284.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.71457(6)
_cell_length_b                   12.74183(11)
_cell_length_c                   19.91482(19)
_cell_angle_alpha                90
_cell_angle_beta                 98.6786(9)
_cell_angle_gamma                90
_cell_volume                     1684.32(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plateled
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4114
_exptl_crystal_size_mid          0.1206
_exptl_crystal_size_min          0.0500
_exptl_absorpt_coefficient_mu    0.635
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30641
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.133
_diffrn_reflns_theta_max         72.035
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6562
_reflns_number_gt                6377
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.981
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0658P)²+0.3002P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2945 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.05(12)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6562
_refine_ls_number_parameters     375
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1225
_refine_ls_wR_factor_gt          0.1214
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O6 O 0.6593(3) 0.25332(14) 0.12225(9) 0.0363(4) Uani 1 1 d . . . . .
O7 O 0.7877(3) 0.03505(16) 0.05621(10) 0.0418(4) Uani 1 1 d . . . . .
O5 O 0.4055(3) 0.30710(16) 0.22210(10) 0.0452(4) Uani 1 1 d . . . . .
O8 O 0.9669(3) -0.0892(2) 0.01382(15) 0.0692(7) Uani 1 1 d . . . . .
C23 C 0.6883(3) 0.16157(19) 0.16307(12) 0.0316(5) Uani 1 1 d . . . . .
H23 H 0.8243 0.1360 0.1599 0.038 Uiso 1 1 calc R U . . .
C27 C 0.5778(4) 0.0579(2) 0.05813(13) 0.0382(5) Uani 1 1 d . . . . .
H27 H 0.5399 0.1215 0.0316 0.046 Uiso 1 1 calc R U . . .
C21 C 0.6828(4) 0.1846(2) 0.23985(12) 0.0369(5) Uani 1 1 d . . . . .
H21 H 0.5907 0.1336 0.2555 0.044 Uiso 1 1 calc R U . . .
C24 C 0.5410(4) 0.0756(2) 0.13189(12) 0.0342(5) Uani 1 1 d . . . . .
C20 C 0.6071(4) 0.2943(2) 0.25532(13) 0.0387(5) Uani 1 1 d . . . . .
H20 H 0.6922 0.3467 0.2375 0.046 Uiso 1 1 calc R U . . .
C30 C 0.8052(5) -0.0561(3) 0.02283(16) 0.0490(7) Uani 1 1 d . . . . .
C28 C 0.4718(4) -0.0339(3) 0.02276(15) 0.0463(6) Uani 1 1 d . . . . .
H28 H 0.3330 -0.0438 0.0159 0.056 Uiso 1 1 calc R U . . .
C25 C 0.5831(5) -0.0260(2) 0.17209(15) 0.0450(6) Uani 1 1 d . . . . .
H25A H 0.7224 -0.0446 0.1740 0.068 Uiso 1 1 calc R U . . .
H25B H 0.5000 -0.0811 0.1502 0.068 Uiso 1 1 calc R U . . .
H25C H 0.5534 -0.0162 0.2173 0.068 Uiso 1 1 calc R U . . .
C19 C 0.6140(5) 0.3134(3) 0.33198(15) 0.0497(7) Uani 1 1 d . . . . .
H19 H 0.7556 0.3111 0.3530 0.060 Uiso 1 1 calc R U . . .
C26 C 0.3201(4) 0.1085(2) 0.12886(15) 0.0446(6) Uani 1 1 d . . . . .
H26A H 0.2940 0.1245 0.1738 0.067 Uiso 1 1 calc R U . . .
H26B H 0.2340 0.0522 0.1103 0.067 Uiso 1 1 calc R U . . .
H26C H 0.2941 0.1694 0.1005 0.067 Uiso 1 1 calc R U . . .
C22 C 0.8931(5) 0.1637(3) 0.27962(15) 0.0568(8) Uani 1 1 d . . . . .
H22A H 0.9362 0.0945 0.2693 0.085 Uiso 1 1 calc R U . . .
H22B H 0.8882 0.1689 0.3274 0.085 Uiso 1 1 calc R U . . .
H22C H 0.9864 0.2145 0.2670 0.085 Uiso 1 1 calc R U . . .
C17 C 0.5324(6) 0.4215(3) 0.3460(2) 0.0669(9) Uani 1 1 d . . . . .
H17A H 0.6045 0.4742 0.3249 0.100 Uiso 1 1 calc R U . . .
H17B H 0.5496 0.4334 0.3941 0.100 Uiso 1 1 calc R U . . .
H17C H 0.3919 0.4251 0.3278 0.100 Uiso 1 1 calc R U . . .
C29 C 0.6036(5) -0.0992(3) 0.00257(16) 0.0514(7) Uani 1 1 d . . . . .
H29 H 0.5732 -0.1619 -0.0206 0.062 Uiso 1 1 calc R U . . .
C32 C 0.8396(5) 0.2993(3) 0.1088(2) 0.0631(9) Uani 1 1 d . . . . .
H32A H 0.8964 0.2571 0.0766 0.095 Uiso 1 1 calc R U . . .
H32B H 0.9333 0.3039 0.1502 0.095 Uiso 1 1 calc R U . . .
H32C H 0.8122 0.3684 0.0905 0.095 Uiso 1 1 calc R U . . .
C31 C 0.3724(5) 0.3994(3) 0.18192(19) 0.0587(8) Uani 1 1 d . . . . .
H31A H 0.4580 0.3985 0.1474 0.088 Uiso 1 1 calc R U . . .
H31B H 0.4028 0.4600 0.2103 0.088 Uiso 1 1 calc R U . . .
H31C H 0.2341 0.4021 0.1609 0.088 Uiso 1 1 calc R U . . .
C18 C 0.5018(6) 0.2295(3) 0.36586(16) 0.0626(9) Uani 1 1 d . . . . .
H18A H 0.3658 0.2246 0.3428 0.094 Uiso 1 1 calc R U . . .
H18B H 0.5008 0.2480 0.4125 0.094 Uiso 1 1 calc R U . . .
H18C H 0.5680 0.1631 0.3635 0.094 Uiso 1 1 calc R U . . .
O1 O 0.7808(3) 0.82362(15) 0.39605(10) 0.0437(4) Uani 1 1 d . . . . .
O3 O 1.1660(3) 0.7166(2) 0.17215(11) 0.0523(5) Uani 1 1 d . . . . .
O2 O 1.0461(3) 0.84889(16) 0.29697(11) 0.0480(5) Uani 1 1 d . . . . .
O4 O 1.3397(3) 0.6514(3) 0.09426(13) 0.0789(10) Uani 1 1 d . . . . .
C7 C 1.0649(4) 0.7383(2) 0.30552(15) 0.0423(6) Uani 1 1 d . . . . .
H7 H 1.2013 0.7197 0.2979 0.051 Uiso 1 1 calc R U . . .
C11 C 0.9560(4) 0.7285(3) 0.18001(15) 0.0456(6) Uani 1 1 d . . . . .
H11 H 0.9229 0.8034 0.1786 0.055 Uiso 1 1 calc R U . . .
C8 C 0.9179(4) 0.6835(2) 0.24903(14) 0.0419(6) Uani 1 1 d . . . . .
C10 C 0.6971(4) 0.7067(2) 0.25516(15) 0.0449(6) Uani 1 1 d . . . . .
H10A H 0.6658 0.6772 0.2967 0.067 Uiso 1 1 calc R U . . .
H10B H 0.6111 0.6761 0.2173 0.067 Uiso 1 1 calc R U . . .
H10C H 0.6763 0.7812 0.2553 0.067 Uiso 1 1 calc R U . . .
C4 C 0.9785(4) 0.7901(2) 0.42423(15) 0.0438(6) Uani 1 1 d . . . . .
H4 H 1.0708 0.8496 0.4242 0.053 Uiso 1 1 calc R U . . .
C14 C 1.1799(5) 0.6689(3) 0.11203(16) 0.0561(8) Uani 1 1 d . . . . .
C5 C 1.0457(4) 0.7030(2) 0.37949(15) 0.0467(6) Uani 1 1 d . . . . .
H5 H 0.9431 0.6477 0.3760 0.056 Uiso 1 1 calc R U . . .
C15 C 0.7570(5) 0.9330(3) 0.38599(18) 0.0544(7) Uani 1 1 d . . . . .
H15A H 0.7923 0.9517 0.3426 0.082 Uiso 1 1 calc R U . . .
H15B H 0.8433 0.9697 0.4212 0.082 Uiso 1 1 calc R U . . .
H15C H 0.6194 0.9520 0.3874 0.082 Uiso 1 1 calc R U . . .
C9 C 0.9569(5) 0.5653(2) 0.25132(18) 0.0536(7) Uani 1 1 d . . . . .
H9A H 1.0918 0.5519 0.2431 0.080 Uiso 1 1 calc R U . . .
H9B H 0.8630 0.5313 0.2171 0.080 Uiso 1 1 calc R U . . .
H9C H 0.9404 0.5387 0.2952 0.080 Uiso 1 1 calc R U . . .
C3 C 0.9756(5) 0.7560(3) 0.49850(16) 0.0528(7) Uani 1 1 d . . . . .
H3 H 1.1135 0.7375 0.5184 0.063 Uiso 1 1 calc R U . . .
C13 C 0.9761(5) 0.6448(3) 0.07858(16) 0.0581(8) Uani 1 1 d . . . . .
H13 H 0.9428 0.6119 0.0367 0.070 Uiso 1 1 calc R U . . .
C12 C 0.8475(4) 0.6778(3) 0.11784(16) 0.0550(8) Uani 1 1 d . . . . .
H12 H 0.7084 0.6704 0.1080 0.066 Uiso 1 1 calc R U . . .
C1 C 0.9075(6) 0.8474(3) 0.53958(17) 0.0611(8) Uani 1 1 d . . . . .
H1A H 0.9956 0.9062 0.5374 0.092 Uiso 1 1 calc R U . . .
H1B H 0.9119 0.8262 0.5861 0.092 Uiso 1 1 calc R U . . .
H1C H 0.7723 0.8669 0.5211 0.092 Uiso 1 1 calc R U . . .
C16 C 1.2324(7) 0.9009(4) 0.3024(3) 0.0923(16) Uani 1 1 d . . . . .
H16A H 1.3027 0.8784 0.2664 0.138 Uiso 1 1 calc R U . . .
H16B H 1.3115 0.8846 0.3454 0.138 Uiso 1 1 calc R U . . .
H16C H 1.2102 0.9753 0.2992 0.138 Uiso 1 1 calc R U . . .
C6 C 1.2454(6) 0.6537(4) 0.4124(2) 0.0716(11) Uani 1 1 d . . . . .
H6A H 1.2883 0.6027 0.3821 0.107 Uiso 1 1 calc R U . . .
H6B H 1.2269 0.6201 0.4542 0.107 Uiso 1 1 calc R U . . .
H6C H 1.3460 0.7075 0.4216 0.107 Uiso 1 1 calc R U . . .
C2 C 0.8426(6) 0.6606(3) 0.50420(18) 0.0629(9) Uani 1 1 d . . . . .
H2A H 0.7103 0.6736 0.4798 0.094 Uiso 1 1 calc R U . . .
H2B H 0.8337 0.6477 0.5511 0.094 Uiso 1 1 calc R U . . .
H2C H 0.8999 0.6005 0.4852 0.094 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O6 C32 1.407(3) . ?
O6 C23 1.420(3) . ?
O7 C30 1.352(4) . ?
O7 C27 1.445(3) . ?
O5 C31 1.421(4) . ?
O5 C20 1.424(3) . ?
O8 C30 1.203(4) . ?
C23 C24 1.542(3) . ?
C23 C21 1.563(3) . ?
C27 C28 1.490(4) . ?
C27 C24 1.542(3) . ?
C21 C20 1.534(3) . ?
C21 C22 1.534(4) . ?
C24 C25 1.526(4) . ?
C24 C26 1.534(3) . ?
C20 C19 1.540(4) . ?
C30 C29 1.460(4) . ?
C28 C29 1.321(4) . ?
C19 C18 1.523(5) . ?
C19 C17 1.524(5) . ?
O1 C15 1.414(4) . ?
O1 C4 1.427(3) . ?
O3 C14 1.359(4) . ?
O3 C11 1.450(3) . ?
O2 C16 1.405(4) . ?
O2 C7 1.423(4) . ?
O4 C14 1.200(4) . ?
C7 C8 1.546(4) . ?
C7 C5 1.564(4) . ?
C11 C12 1.486(5) . ?
C11 C8 1.546(4) . ?
C8 C9 1.528(4) . ?
C8 C10 1.534(3) . ?
C4 C5 1.533(4) . ?
C4 C3 1.544(4) . ?
C14 C13 1.461(4) . ?
C5 C6 1.536(4) . ?
C3 C2 1.522(5) . ?
C3 C1 1.532(5) . ?
C13 C12 1.318(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
_geom_angle_publ_flag
C32 O6 C23 113.8(2) . . ?
C30 O7 C27 110.1(2) . . ?
C31 O5 C20 114.4(2) . . ?
O6 C23 C24 109.25(19) . . ?
O6 C23 C21 112.56(19) . . ?
C24 C23 C21 114.79(19) . . ?
O7 C27 C28 103.2(2) . . ?
O7 C27 C24 110.6(2) . . ?
C28 C27 C24 115.6(2) . . ?
C20 C21 C22 111.2(2) . . ?
C20 C21 C23 115.2(2) . . ?
C22 C21 C23 108.4(2) . . ?
C25 C24 C26 110.7(2) . . ?
C25 C24 C23 109.6(2) . . ?
C26 C24 C23 112.3(2) . . ?
C25 C24 C27 109.4(2) . . ?
C26 C24 C27 107.2(2) . . ?
C23 C24 C27 107.61(18) . . ?
O5 C20 C21 109.4(2) . . ?
O5 C20 C19 109.1(2) . . ?
C21 C20 C19 112.5(2) . . ?
O8 C30 O7 121.4(3) . . ?
O8 C30 C29 130.3(3) . . ?
O7 C30 C29 108.3(2) . . ?
C29 C28 C27 110.1(3) . . ?
C18 C19 C17 109.7(3) . . ?
C18 C19 C20 112.7(3) . . ?
C17 C19 C20 111.5(3) . . ?
C28 C29 C30 108.4(3) . . ?
C15 O1 C4 115.4(2) . . ?
C14 O3 C11 109.9(2) . . ?
C16 O2 C7 113.4(3) . . ?
O2 C7 C8 108.9(2) . . ?
O2 C7 C5 112.3(2) . . ?
C8 C7 C5 114.9(2) . . ?
O3 C11 C12 103.1(2) . . ?
O3 C11 C8 110.6(2) . . ?
C12 C11 C8 117.0(3) . . ?
C9 C8 C10 110.5(2) . . ?
C9 C8 C11 109.9(2) . . ?
C10 C8 C11 106.9(2) . . ?
C9 C8 C7 109.6(2) . . ?
C10 C8 C7 111.9(2) . . ?
C11 C8 C7 107.9(2) . . ?
O1 C4 C5 109.0(2) . . ?
O1 C4 C3 108.4(2) . . ?
C5 C4 C3 113.6(2) . . ?
O4 C14 O3 121.8(3) . . ?
O4 C14 C13 130.1(3) . . ?
O3 C14 C13 108.1(2) . . ?
C4 C5 C6 111.2(3) . . ?
C4 C5 C7 114.4(2) . . ?
C6 C5 C7 109.2(2) . . ?
C2 C3 C1 109.9(3) . . ?
C2 C3 C4 112.8(3) . . ?
C1 C3 C4 110.2(3) . . ?
C12 C13 C14 108.4(3) . . ?
C13 C12 C11 110.5(3) . . ?

_refine_diff_density_max         0.170
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.038

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1726
_database_code_depnum_ccdc_archive 'CCDC 1431107'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(R)-6-((3S,4S,5S)-3,5-bis((tert-butyldimethylsilyl)oxy)-2,4,6-trimethylheptan-2-yl)-5,6-dihydro-2H-pyran-2-one
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H54 O4 Si2'
_chemical_formula_sum            'C27 H54 O4 Si2'
_chemical_formula_weight         498.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.67692(13)
_cell_length_b                   7.47473(8)
_cell_length_c                   15.84227(18)
_cell_angle_alpha                90
_cell_angle_beta                 103.3349(10)
_cell_angle_gamma                90
_cell_volume                     1575.91(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       fiber
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_F_000             552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5922
_exptl_crystal_size_mid          0.1462
_exptl_crystal_size_min          0.1004
_exptl_absorpt_coefficient_mu    1.221
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27047
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.321
_diffrn_reflns_theta_max         65.975
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             5445
_reflns_number_gt                5305
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_max     0.982
_reflns_Friedel_fraction_full    0.947

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 The U(eq) for C19 is larger than expected and B alerts are
 reported. The carbon is part of a disordered terbutyl moiety
 but that atom itself didn't refine satisfactory when modeled
 as disordered. Thus the atom belongs to two diferents 
 parts of disorder 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1051P)²+0.1454P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2339 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(16)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5445
_refine_ls_number_parameters     372
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1308
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si2 Si 0.13901(5) -0.28394(10) -0.23932(4) 0.0307(2) Uani 1 1 d . . . . .
C19 C -0.5392(3) -0.5793(10) -0.1614(5) 0.107(2) Uani 1 1 d . . . . .
H19A H -0.5776 -0.4728 -0.1793 0.161 Uiso 1 1 calc R U . A 1
H19B H -0.5663 -0.6410 -0.1188 0.161 Uiso 1 1 calc R U . A 1
H19C H -0.5424 -0.6557 -0.2106 0.161 Uiso 1 1 calc R U . A 1
Si1 Si -0.36947(8) -0.4645(2) -0.21434(9) 0.0400(6) Uani 0.670(5) 1 d . . P B 1
C18 C -0.4271(3) -0.5278(8) -0.1212(4) 0.0482(13) Uani 0.670(5) 1 d . . P B 1
C20 C -0.3718(7) -0.6821(18) -0.0712(6) 0.062(3) Uani 0.670(5) 1 d . . P B 1
H20A H -0.3962 -0.7016 -0.0198 0.093 Uiso 0.670(5) 1 calc R U P B 1
H20B H -0.3013 -0.6556 -0.0553 0.093 Uiso 0.670(5) 1 calc R U P B 1
H20C H -0.3826 -0.7878 -0.1066 0.093 Uiso 0.670(5) 1 calc R U P B 1
C21 C -0.4207(6) -0.3712(13) -0.0588(5) 0.073(2) Uani 0.670(5) 1 d . . P B 1
H21A H -0.3515 -0.3407 -0.0358 0.109 Uiso 0.670(5) 1 calc R U P B 1
H21B H -0.4512 -0.4041 -0.0122 0.109 Uiso 0.670(5) 1 calc R U P B 1
H21C H -0.4555 -0.2701 -0.0891 0.109 Uiso 0.670(5) 1 calc R U P B 1
C16 C -0.3704(13) -0.658(3) -0.2857(10) 0.065(3) Uani 0.670(5) 1 d . . P B 1
H16A H -0.3643 -0.6172 -0.3418 0.097 Uiso 0.670(5) 1 calc R U P B 1
H16B H -0.4323 -0.7220 -0.2914 0.097 Uiso 0.670(5) 1 calc R U P B 1
H16C H -0.3150 -0.7349 -0.2613 0.097 Uiso 0.670(5) 1 calc R U P B 1
Si1' Si -0.37255(18) -0.3581(4) -0.1715(2) 0.0418(11) Uani 0.330(5) 1 d . . P B
2
C17 C -0.4395(8) -0.2817(15) -0.2808(8) 0.064(3) Uani 0.670(5) 1 d . . P B 1
H17A H -0.5099 -0.3091 -0.2948 0.077 Uiso 0.670(5) 1 calc R U P B 1
H17B H -0.4164 -0.2695 -0.3334 0.077 Uiso 0.670(5) 1 calc R U P B 1
H17C H -0.4284 -0.1716 -0.2488 0.077 Uiso 0.670(5) 1 calc R U P B 1
O2 O 0.01710(14) -0.2455(3) -0.26110(12) 0.0320(4) Uani 1 1 d . . . . .
C19' C -0.389(3) -0.688(5) -0.269(3) 0.082(10) Uani 0.330(5) 1 d . . P B 2
H19D H -0.4095 -0.6209 -0.3223 0.123 Uiso 0.330(5) 1 calc R U P B 2
H19E H -0.4198 -0.8044 -0.2772 0.123 Uiso 0.330(5) 1 calc R U P B 2
H19F H -0.3176 -0.7005 -0.2547 0.123 Uiso 0.330(5) 1 calc R U P B 2
C18' C -0.4259(9) -0.5819(19) -0.1904(11) 0.064(3) Uani 0.330(5) 1 d . . P B 2
C17' C -0.4030(12) -0.259(3) -0.0716(11) 0.073(4) Uani 0.330(5) 1 d . . P B 2
H17D H -0.4293 -0.1402 -0.0843 0.110 Uiso 0.330(5) 1 calc R U P B 2
H17E H -0.3432 -0.2538 -0.0260 0.110 Uiso 0.330(5) 1 calc R U P B 2
H17F H -0.4523 -0.3319 -0.0536 0.110 Uiso 0.330(5) 1 calc R U P B 2
O1 O -0.25313(15) -0.3981(3) -0.16530(14) 0.0421(5) Uani 1 1 d . . . . .
C11 C -0.2278(2) -0.2812(5) -0.42904(18) 0.0374(6) Uani 1 1 d . . . . .
H11 H -0.2663 -0.2867 -0.3841 0.045 Uiso 1 1 calc R U . . .
O3 O -0.21630(16) -0.4629(3) -0.45811(14) 0.0427(5) Uani 1 1 d . . . . .
C1 C -0.1783(4) -0.0219(6) -0.1097(3) 0.0660(11) Uani 1 1 d . . . . .
H1A H -0.2025 0.0444 -0.1623 0.099 Uiso 1 1 calc R U . . .
H1B H -0.1361 0.0536 -0.0675 0.099 Uiso 1 1 calc R U . . .
H1C H -0.2343 -0.0624 -0.0878 0.099 Uiso 1 1 calc R U . . .
O4 O -0.2933(3) -0.7104(4) -0.5122(2) 0.0716(8) Uani 1 1 d . . . . .
C6 C -0.0724(2) -0.5738(4) -0.1991(2) 0.0413(7) Uani 1 1 d . . . . .
H6A H -0.0555 -0.6628 -0.2370 0.062 Uiso 1 1 calc R U . . .
H6B H -0.1127 -0.6271 -0.1636 0.062 Uiso 1 1 calc R U . . .
H6C H -0.0120 -0.5262 -0.1628 0.062 Uiso 1 1 calc R U . . .
C21' C -0.383(3) -0.703(4) -0.1054(16) 0.102(11) Uani 0.330(5) 1 d . . P B 2
H21D H -0.4020 -0.8252 -0.1179 0.153 Uiso 0.330(5) 1 calc R U P B 2
H21E H -0.4114 -0.6613 -0.0586 0.153 Uiso 0.330(5) 1 calc R U P B 2
H21F H -0.3115 -0.6929 -0.0890 0.153 Uiso 0.330(5) 1 calc R U P B 2
C2 C -0.0778(3) -0.2831(7) -0.0442(2) 0.0677(11) Uani 1 1 d . . . . .
H2A H -0.1328 -0.3337 -0.0240 0.102 Uiso 1 1 calc R U . . .
H2B H -0.0412 -0.2023 -0.0013 0.102 Uiso 1 1 calc R U . . .
H2C H -0.0340 -0.3772 -0.0541 0.102 Uiso 1 1 calc R U . . .
C8 C -0.1221(2) -0.2104(4) -0.38673(17) 0.0337(6) Uani 1 1 d . . . . .
C7 C -0.06821(19) -0.3382(4) -0.31156(17) 0.0305(6) Uani 1 1 d . . . . .
H7 H -0.0415 -0.4379 -0.3395 0.037 Uiso 1 1 calc R U . . .
C10 C -0.1329(2) -0.0186(4) -0.3542(2) 0.0419(7) Uani 1 1 d . . . . .
H10A H -0.1883 -0.0140 -0.3264 0.063 Uiso 1 1 calc R U . . .
H10B H -0.1450 0.0626 -0.4024 0.063 Uiso 1 1 calc R U . . .
H10C H -0.0722 0.0150 -0.3134 0.063 Uiso 1 1 calc R U . . .
C25 C 0.3159(3) -0.0851(6) -0.2120(4) 0.0771(14) Uani 1 1 d . . . . .
H25A H 0.3381 -0.1374 -0.1554 0.116 Uiso 1 1 calc R U . . .
H25B H 0.3488 0.0279 -0.2136 0.116 Uiso 1 1 calc R U . . .
H25C H 0.3321 -0.1637 -0.2547 0.116 Uiso 1 1 calc R U . . .
C23 C 0.1747(3) -0.4251(5) -0.3250(2) 0.0488(8) Uani 1 1 d . . . . .
H23A H 0.1318 -0.5281 -0.3360 0.073 Uiso 1 1 calc R U . . .
H23B H 0.2433 -0.4629 -0.3056 0.073 Uiso 1 1 calc R U . . .
H23C H 0.1674 -0.3566 -0.3773 0.073 Uiso 1 1 calc R U . . .
C9 C -0.0566(3) -0.2046(5) -0.4537(2) 0.0468(7) Uani 1 1 d . . . . .
H9A H 0.0107 -0.1706 -0.4254 0.070 Uiso 1 1 calc R U . . .
H9B H -0.0839 -0.1190 -0.4980 0.070 Uiso 1 1 calc R U . . .
H9C H -0.0557 -0.3207 -0.4794 0.070 Uiso 1 1 calc R U . . .
C27 C 0.1743(4) 0.0505(7) -0.1585(3) 0.0695(11) Uani 1 1 d . . . . .
H27A H 0.1026 0.0635 -0.1698 0.104 Uiso 1 1 calc R U . . .
H27B H 0.2050 0.1666 -0.1551 0.104 Uiso 1 1 calc R U . . .
H27C H 0.1978 -0.0113 -0.1045 0.104 Uiso 1 1 calc R U . . .
C22 C 0.1819(2) -0.3998(6) -0.1322(2) 0.0524(9) Uani 1 1 d . . . . .
H22A H 0.1564 -0.3373 -0.0888 0.079 Uiso 1 1 calc R U . . .
H22B H 0.2540 -0.4008 -0.1160 0.079 Uiso 1 1 calc R U . . .
H22C H 0.1573 -0.5205 -0.1369 0.079 Uiso 1 1 calc R U . . .
C3 C -0.1182(2) -0.1823(5) -0.12829(19) 0.0420(7) Uani 1 1 d . . . . .
H3 H -0.0607 -0.1376 -0.1492 0.050 Uiso 1 1 calc R U . . .
C26 C 0.1702(3) 0.0463(6) -0.3172(3) 0.0632(10) Uani 1 1 d . . . . .
H26A H 0.1798 -0.0282 -0.3640 0.095 Uiso 1 1 calc R U . . .
H26B H 0.2104 0.1524 -0.3146 0.095 Uiso 1 1 calc R U . . .
H26C H 0.1006 0.0789 -0.3267 0.095 Uiso 1 1 calc R U . . .
C24 C 0.2020(2) -0.0563(5) -0.2314(2) 0.0449(7) Uani 1 1 d . . . . .
C5 C -0.1316(2) -0.4228(4) -0.25320(17) 0.0320(6) Uani 1 1 d . . . . .
H5 H -0.1868 -0.4833 -0.2935 0.038 Uiso 1 1 calc R U . . .
C4 C -0.18356(18) -0.2962(5) -0.20096(17) 0.0342(6) Uani 1 1 d . . . . .
H4 H -0.2235 -0.2124 -0.2426 0.041 Uiso 1 1 calc R U . . .
C16' C -0.4261(14) -0.209(2) -0.2657(17) 0.055(5) Uani 0.330(5) 1 d . . P B 2
H16D H -0.4075 -0.2538 -0.3166 0.082 Uiso 0.330(5) 1 calc R U P B 2
H16E H -0.4002 -0.0902 -0.2535 0.082 Uiso 0.330(5) 1 calc R U P B 2
H16F H -0.4980 -0.2072 -0.2752 0.082 Uiso 0.330(5) 1 calc R U P B 2
C15 C -0.2983(3) -0.5513(6) -0.5014(2) 0.0537(9) Uani 1 1 d . . . . .
C14 C -0.3882(3) -0.4431(7) -0.5371(3) 0.0650(11) Uani 1 1 d . . . . .
H14 H -0.4499 -0.4996 -0.5565 0.078 Uiso 1 1 calc R U . . .
C13 C -0.3828(3) -0.2694(7) -0.5418(3) 0.0663(11) Uani 1 1 d . . . . .
H13 H -0.4394 -0.2052 -0.5695 0.080 Uiso 1 1 calc R U . . .
C12 C -0.2875(3) -0.1707(5) -0.5037(2) 0.0525(9) Uani 1 1 d . . . . .
H12A H -0.3027 -0.0542 -0.4830 0.063 Uiso 1 1 calc R U . . .
H12B H -0.2489 -0.1536 -0.5473 0.063 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si2 O2 1.6480(19) . ?
Si2 C23 1.871(3) . ?
Si2 C22 1.875(3) . ?
Si2 C24 1.898(3) . ?
C19 C18 1.567(6) . ?
C19 C18' 1.715(13) . ?
Si1 O1 1.677(2) . ?
Si1 C16 1.832(19) . ?
Si1 C17 1.851(12) . ?
Si1 C18 1.886(5) . ?
C18 C20 1.501(12) . ?
C18 C21 1.521(11) . ?
Si1' O1 1.641(3) . ?
Si1' C18' 1.822(14) . ?
Si1' C16' 1.87(2) . ?
Si1' C17' 1.880(14) . ?
O2 C7 1.432(3) . ?
C19' C18' 1.65(4) . ?
C18' C21' 1.61(3) . ?
O1 C4 1.432(3) . ?
C11 O3 1.454(4) . ?
C11 C12 1.517(4) . ?
C11 C8 1.540(4) . ?
O3 C15 1.345(4) . ?
C1 C3 1.521(5) . ?
O4 C15 1.205(5) . ?
C6 C5 1.531(4) . ?
C2 C3 1.519(5) . ?
C8 C9 1.539(4) . ?
C8 C10 1.542(4) . ?
C8 C7 1.571(4) . ?
C7 C5 1.541(4) . ?
C25 C24 1.532(5) . ?
C27 C24 1.523(6) . ?
C3 C4 1.541(4) . ?
C26 C24 1.533(6) . ?
C5 C4 1.535(4) . ?
C15 C14 1.471(6) . ?
C14 C13 1.304(7) . ?
C13 C12 1.498(6) . ?

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
_geom_angle_publ_flag
O2 Si2 C23 111.55(13) . . ?
O2 Si2 C22 111.12(13) . . ?
C23 Si2 C22 108.46(18) . . ?
O2 Si2 C24 106.22(13) . . ?
C23 Si2 C24 111.28(17) . . ?
C22 Si2 C24 108.17(18) . . ?
O1 Si1 C16 112.9(6) . . ?
O1 Si1 C17 110.9(3) . . ?
C16 Si1 C17 107.5(7) . . ?
O1 Si1 C18 103.59(19) . . ?
C16 Si1 C18 109.9(4) . . ?
C17 Si1 C18 112.1(4) . . ?
C20 C18 C21 107.6(7) . . ?
C20 C18 C19 110.6(6) . . ?
C21 C18 C19 110.9(5) . . ?
C20 C18 Si1 110.8(4) . . ?
C21 C18 Si1 110.1(4) . . ?
C19 C18 Si1 106.9(4) . . ?
O1 Si1' C18' 101.4(4) . . ?
O1 Si1' C16' 111.0(7) . . ?
C18' Si1' C16' 110.3(7) . . ?
O1 Si1' C17' 115.6(5) . . ?
C18' Si1' C17' 110.0(8) . . ?
C16' Si1' C17' 108.3(10) . . ?
C7 O2 Si2 133.44(17) . . ?
C21' C18' C19' 105(2) . . ?
C21' C18' C19 87.5(13) . . ?
C19' C18' C19 131.1(15) . . ?
C21' C18' Si1' 108.8(14) . . ?
C19' C18' Si1' 112.6(13) . . ?
C19 C18' Si1' 107.3(8) . . ?
C4 O1 Si1' 128.5(2) . . ?
C4 O1 Si1 128.34(18) . . ?
O3 C11 C12 109.8(2) . . ?
O3 C11 C8 107.4(2) . . ?
C12 C11 C8 115.8(3) . . ?
C15 O3 C11 118.8(3) . . ?
C9 C8 C11 110.3(2) . . ?
C9 C8 C10 108.7(3) . . ?
C11 C8 C10 108.2(3) . . ?
C9 C8 C7 107.1(2) . . ?
C11 C8 C7 110.5(2) . . ?
C10 C8 C7 112.1(2) . . ?
O2 C7 C5 111.2(2) . . ?
O2 C7 C8 108.0(2) . . ?
C5 C7 C8 118.3(2) . . ?
C2 C3 C1 109.0(3) . . ?
C2 C3 C4 114.3(3) . . ?
C1 C3 C4 109.5(3) . . ?
C27 C24 C25 109.9(4) . . ?
C27 C24 C26 110.0(4) . . ?
C25 C24 C26 108.4(4) . . ?
C27 C24 Si2 109.4(3) . . ?
C25 C24 Si2 108.2(3) . . ?
C26 C24 Si2 111.0(2) . . ?
C6 C5 C4 113.8(2) . . ?
C6 C5 C7 109.9(2) . . ?
C4 C5 C7 117.7(2) . . ?
O1 C4 C5 108.5(3) . . ?
O1 C4 C3 108.8(2) . . ?
C5 C4 C3 118.8(2) . . ?
O4 C15 O3 119.3(4) . . ?
O4 C15 C14 123.9(4) . . ?
O3 C15 C14 116.7(4) . . ?
C13 C14 C15 121.1(4) . . ?
C14 C13 C12 121.5(4) . . ?
C13 C12 C11 107.9(3) . . ?

_refine_diff_density_max         0.505
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1727
_database_code_depnum_ccdc_archive 'CCDC 1431108'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(S)-6-((3S,4S,5S)-3,5-dimethoxy-2,4,6-trimethylheptan-2-yl)-5,6-dihydro-2H-pyran-2-one
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H30 O4'
_chemical_formula_sum            'C17 H30 O4'
_chemical_formula_weight         298.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.89663(7)
_cell_length_b                   13.34364(17)
_cell_length_c                   9.58347(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.1421(9)
_cell_angle_gamma                90
_cell_volume                     879.626(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needles
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_F_000             328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2801
_exptl_crystal_size_mid          0.2642
_exptl_crystal_size_min          0.1005
_exptl_absorpt_coefficient_mu    0.628
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.86283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Cu Kα'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15732
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.626
_diffrn_reflns_theta_max         71.921
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3347
_reflns_number_gt                3274
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0978P)²+0.0134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3347
_refine_ls_number_parameters     198
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.7318(2) 0.66179(13) 0.60803(14) 0.0396(4) Uani 1 1 d . . . . .
O1 O 0.5250(2) 0.84336(12) 0.66679(15) 0.0390(4) Uani 1 1 d . . . . .
O3 O 0.9356(2) 0.47843(12) 0.81206(17) 0.0408(4) Uani 1 1 d . . . . .
C11 C 0.7278(3) 0.50258(16) 0.79990(19) 0.0343(4) Uani 1 1 d . . . . .
H11 H 0.6838 0.4996 0.7004 0.041 Uiso 1 1 calc R U . . .
C7 C 0.8178(3) 0.67899(15) 0.7463(2) 0.0338(4) Uani 1 1 d . . . . .
H7 H 0.9521 0.6547 0.7486 0.041 Uiso 1 1 calc R U . . .
C4 C 0.7300(3) 0.86037(16) 0.67027(18) 0.0333(4) Uani 1 1 d . . . . .
H4 H 0.7765 0.8407 0.5800 0.040 Uiso 1 1 calc R U . . .
C8 C 0.7082(3) 0.61195(16) 0.8476(2) 0.0334(4) Uani 1 1 d . . . . .
C10 C 0.4910(3) 0.63898(18) 0.8396(2) 0.0390(5) Uani 1 1 d . . . . .
H10A H 0.4320 0.6206 0.7494 0.058 Uiso 1 1 calc R U . . .
H10B H 0.4767 0.7098 0.8532 0.058 Uiso 1 1 calc R U . . .
H10C H 0.4286 0.6034 0.9110 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6707(4) 0.32208(18) 0.8299(2) 0.0423(5) Uani 1 1 d . . . . .
H13 H 0.5832 0.2694 0.8353 0.051 Uiso 1 1 calc R U . . .
C3 C 0.7679(3) 0.97291(18) 0.6928(2) 0.0384(5) Uani 1 1 d . . . . .
H3 H 0.9086 0.9838 0.6956 0.046 Uiso 1 1 calc R U . . .
C15 C 0.9913(3) 0.38436(19) 0.7840(3) 0.0434(5) Uani 1 1 d . . . . .
C9 C 0.7981(4) 0.62521(19) 0.9980(2) 0.0428(5) Uani 1 1 d . . . . .
H9A H 0.7390 0.5788 1.0587 0.064 Uiso 1 1 calc R U . . .
H9B H 0.7761 0.6925 1.0288 0.064 Uiso 1 1 calc R U . . .
H9C H 0.9354 0.6126 1.0005 0.064 Uiso 1 1 calc R U . . .
C12 C 0.6148(3) 0.42462(18) 0.8748(2) 0.0410(5) Uani 1 1 d . . . . .
H12A H 0.6419 0.4315 0.9751 0.049 Uiso 1 1 calc R U . . .
H12B H 0.4766 0.4347 0.8534 0.049 Uiso 1 1 calc R U . . .
O4 O 1.1599(3) 0.36771(17) 0.7695(3) 0.0708(7) Uani 1 1 d . . . . .
C6 C 1.0386(4) 0.8221(2) 0.8247(3) 0.0481(6) Uani 1 1 d . . . . .
H6A H 1.0955 0.7750 0.8915 0.072 Uiso 1 1 calc R U . . .
H6B H 1.0429 0.8880 0.8648 0.072 Uiso 1 1 calc R U . . .
H6C H 1.1102 0.8215 0.7424 0.072 Uiso 1 1 calc R U . . .
C5 C 0.8264(3) 0.79275(16) 0.7853(2) 0.0336(4) Uani 1 1 d . . . . .
H5 H 0.7545 0.8015 0.8690 0.040 Uiso 1 1 calc R U . . .
C14 C 0.8439(3) 0.30518(19) 0.7824(2) 0.0425(5) Uani 1 1 d . . . . .
H14 H 0.8720 0.2422 0.7477 0.051 Uiso 1 1 calc R U . . .
C16 C 0.4323(4) 0.8237(2) 0.5327(3) 0.0533(6) Uani 1 1 d . . . . .
H16A H 0.3111 0.8593 0.5224 0.080 Uiso 1 1 calc R U . . .
H16B H 0.4085 0.7531 0.5228 0.080 Uiso 1 1 calc R U . . .
H16C H 0.5146 0.8455 0.4619 0.080 Uiso 1 1 calc R U . . .
C1 C 0.6741(4) 1.0335(2) 0.5708(3) 0.0544(6) Uani 1 1 d . . . . .
H1A H 0.7248 1.0116 0.4852 0.082 Uiso 1 1 calc R U . . .
H1B H 0.7028 1.1033 0.5851 0.082 Uiso 1 1 calc R U . . .
H1C H 0.5359 1.0237 0.5654 0.082 Uiso 1 1 calc R U . . .
C17 C 0.8665(5) 0.6451(3) 0.5067(3) 0.0672(8) Uani 1 1 d . . . . .
H17A H 0.9360 0.5840 0.5278 0.101 Uiso 1 1 calc R U . . .
H17B H 0.9566 0.7000 0.5074 0.101 Uiso 1 1 calc R U . . .
H17C H 0.7986 0.6400 0.4159 0.101 Uiso 1 1 calc R U . . .
C2 C 0.6971(4) 1.0105(2) 0.8306(3) 0.0495(6) Uani 1 1 d . . . . .
H2A H 0.5602 0.9980 0.8322 0.074 Uiso 1 1 calc R U . . .
H2B H 0.7212 1.0812 0.8392 0.074 Uiso 1 1 calc R U . . .
H2C H 0.7653 0.9760 0.9071 0.074 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C17 1.409(3) . ?
O2 C7 1.430(2) . ?
O1 C16 1.418(3) . ?
O1 C4 1.430(2) . ?
O3 C15 1.346(3) . ?
O3 C11 1.466(2) . ?
C11 C12 1.512(3) . ?
C11 C8 1.538(3) . ?
C7 C8 1.556(3) . ?
C7 C5 1.564(3) . ?
C4 C3 1.537(3) . ?
C4 C5 1.538(3) . ?
C8 C10 1.538(3) . ?
C8 C9 1.538(3) . ?
C13 C14 1.327(4) . ?
C13 C12 1.493(3) . ?
C3 C2 1.525(3) . ?
C3 C1 1.526(3) . ?
C15 O4 1.201(3) . ?
C15 C14 1.466(4) . ?
C6 C5 1.535(3) . ?

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
_geom_angle_publ_flag
C17 O2 C7 114.4(2) . . ?
C16 O1 C4 115.50(16) . . ?
C15 O3 C11 118.74(17) . . ?
O3 C11 C12 110.21(17) . . ?
O3 C11 C8 106.93(16) . . ?
C12 C11 C8 116.91(17) . . ?
O2 C7 C8 107.35(16) . . ?
O2 C7 C5 112.55(16) . . ?
C8 C7 C5 114.87(16) . . ?
O1 C4 C3 108.43(16) . . ?
O1 C4 C5 107.42(15) . . ?
C3 C4 C5 114.32(16) . . ?
C10 C8 C9 110.22(17) . . ?
C10 C8 C11 108.28(17) . . ?
C9 C8 C11 110.47(16) . . ?
C10 C8 C7 110.45(16) . . ?
C9 C8 C7 109.75(17) . . ?
C11 C8 C7 107.63(16) . . ?
C14 C13 C12 120.8(2) . . ?
C2 C3 C1 110.2(2) . . ?
C2 C3 C4 112.44(18) . . ?
C1 C3 C4 110.56(19) . . ?
O4 C15 O3 119.2(2) . . ?
O4 C15 C14 122.8(2) . . ?
O3 C15 C14 117.8(2) . . ?
C13 C12 C11 109.96(19) . . ?
C6 C5 C4 112.46(18) . . ?
C6 C5 C7 108.99(17) . . ?
C4 C5 C7 113.02(16) . . ?
C13 C14 C15 121.0(2) . . ?

_refine_diff_density_max         0.195
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.053

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_str1732
_database_code_depnum_ccdc_archive 'CCDC 1431109'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.
2016-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'(3S,5S,6S,7S)-5,7-bis((tert-butyldimethylsilyl)oxy)-4,4,6,8-tetramethylnon-1-en-3-yl acrylate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28.15 H54.38 O4 Si2'
_chemical_formula_weight         513.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   16.5936(3)
_cell_length_b                   16.0072(3)
_cell_length_c                   12.75162(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3387.04(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       crystal
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_F_000             1133
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.6842
_exptl_crystal_size_mid          0.1179
_exptl_crystal_size_min          0.0698
_exptl_absorpt_coefficient_mu    1.148
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.61251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16241
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.837
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.914
_reflns_number_total             5604
_reflns_number_gt                4917
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_max     0.940
_reflns_Friedel_fraction_full    0.881

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0935P)²+8.9198P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1868 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.01(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5604
_refine_ls_number_parameters     315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0885
_refine_ls_wR_factor_ref         0.2637
_refine_ls_wR_factor_gt          0.2550
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.58130(14) 0.30599(15) -0.19203(17) 0.0433(6) Uani 1 1 d . . . . .
C4 C 0.5119(5) 0.3691(5) -0.0107(6) 0.0377(17) Uani 1 1 d . . . . .
H4A H 0.5254 0.4212 -0.0471 0.045 Uiso 1 1 calc R U . . .
C19 C 0.5548(9) 0.2057(11) -0.2613(9) 0.093(3) Uani 1 1 d . . . . .
C26 C 0.3404(11) 0.4533(9) 0.4720(11) 0.107(6) Uani 1 1 d . . . . .
H26A H 0.3393 0.3947 0.4880 0.161 Uiso 1 1 calc R U . . .
H26B H 0.2872 0.4762 0.4796 0.161 Uiso 1 1 calc R U . . .
H26C H 0.3765 0.4813 0.5193 0.161 Uiso 1 1 calc R U . . .
C1 C 0.3793(9) 0.4067(14) -0.0865(14) 0.153(10) Uani 1 1 d . . . . .
H1A H 0.3974 0.4626 -0.1007 0.230 Uiso 1 1 calc R U . . .
H1B H 0.3223 0.4072 -0.0735 0.230 Uiso 1 1 calc R U . . .
H1C H 0.3905 0.3718 -0.1459 0.230 Uiso 1 1 calc R U . . .
Si2 Si 0.47215(19) 0.41768(17) 0.34197(18) 0.0539(7) Uani 1 1 d . . . . .
C2 C 0.3863(10) 0.2901(14) 0.0377(15) 0.163(11) Uani 1 1 d . . . . .
H2A H 0.3304 0.2896 0.0184 0.245 Uiso 1 1 calc R U . . .
H2B H 0.3912 0.2815 0.1120 0.245 Uiso 1 1 calc R U . . .
H2C H 0.4141 0.2463 0.0012 0.245 Uiso 1 1 calc R U . . .
O3 O 0.5287(3) 0.3032(3) -0.0844(4) 0.0395(12) Uani 1 1 d . . . . .
C3 C 0.4228(6) 0.3730(10) 0.0089(10) 0.089(5) Uani 1 1 d . . . . .
H3 H 0.4134 0.4117 0.0672 0.106 Uiso 1 1 calc R U . . .
O4 O 0.4958(3) 0.4360(3) 0.2197(4) 0.0369(12) Uani 1 1 d . . . . .
C6 C 0.5692(9) 0.2763(5) 0.1319(8) 0.078(4) Uani 1 1 d . . . . .
H6A H 0.5168 0.2672 0.1616 0.118 Uiso 1 1 calc R U . . .
H6B H 0.6091 0.2733 0.1862 0.118 Uiso 1 1 calc R U . . .
H6C H 0.5799 0.2343 0.0801 0.118 Uiso 1 1 calc R U . . .
C5 C 0.5718(5) 0.3625(4) 0.0807(6) 0.0338(16) Uani 1 1 d . . . . .
H5 H 0.6252 0.3660 0.0480 0.041 Uiso 1 1 calc R U . . .
C8 C 0.5964(5) 0.5226(5) 0.1302(5) 0.0327(16) Uani 1 1 d . . . . .
C7 C 0.5716(4) 0.4318(4) 0.1653(5) 0.0313(15) Uani 1 1 d . . . . .
H7 H 0.6114 0.4148 0.2178 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5316(6) 0.5651(5) 0.0638(7) 0.0462(19) Uani 1 1 d . . . . .
H9A H 0.5328 0.5428 -0.0060 0.069 Uiso 1 1 calc R U . . .
H9B H 0.5417 0.6241 0.0614 0.069 Uiso 1 1 calc R U . . .
H9C H 0.4796 0.5552 0.0944 0.069 Uiso 1 1 calc R U . . .
C10 C 0.6093(6) 0.5751(5) 0.2284(6) 0.047(2) Uani 1 1 d . . . . .
H10A H 0.5586 0.5831 0.2634 0.070 Uiso 1 1 calc R U . . .
H10B H 0.6313 0.6283 0.2092 0.070 Uiso 1 1 calc R U . . .
H10C H 0.6459 0.5468 0.2746 0.070 Uiso 1 1 calc R U . . .
C25 C 0.3695(7) 0.4659(7) 0.3586(9) 0.068(3) Uani 1 1 d . . . . .
C11 C 0.6753(5) 0.5172(5) 0.0674(5) 0.0379(18) Uani 1 1 d . . . . .
H11 H 0.6658 0.4860 0.0024 0.045 Uiso 1 1 calc R U . . .
C20 C 0.6029(8) 0.1984(10) -0.3625(9) 0.094(5) Uani 1 1 d . . . . .
H20A H 0.5920 0.2458 -0.4064 0.141 Uiso 1 1 calc R U . . .
H20B H 0.5877 0.1481 -0.3986 0.141 Uiso 1 1 calc R U . . .
H20C H 0.6594 0.1965 -0.3464 0.141 Uiso 1 1 calc R U . . .
C14 C 0.7191(5) 0.6205(6) -0.0540(6) 0.048(2) Uani 1 1 d . . . . .
C13 C 0.7937(6) 0.4255(8) 0.0835(10) 0.076(3) Uani 1 1 d . . . . .
H13A H 0.7859 0.4074 0.0150 0.091 Uiso 1 1 calc R U . . .
H13B H 0.8364 0.4045 0.1228 0.091 Uiso 1 1 calc R U . . .
C12 C 0.7453(5) 0.4799(6) 0.1242(7) 0.051(2) Uani 1 1 d . . . . .
H12 H 0.7547 0.4968 0.1929 0.061 Uiso 1 1 calc R U . . .
C21 C 0.4650(9) 0.2099(15) -0.2885(14) 0.157(10) Uani 1 1 d . . . . .
H21A H 0.4507 0.1627 -0.3310 0.235 Uiso 1 1 calc R U . . .
H21B H 0.4541 0.2605 -0.3264 0.235 Uiso 1 1 calc R U . . .
H21C H 0.4338 0.2092 -0.2251 0.235 Uiso 1 1 calc R U . . .
C23 C 0.4657(13) 0.3035(9) 0.3714(11) 0.125(7) Uani 1 1 d . . . . .
H23A H 0.4330 0.2766 0.3193 0.187 Uiso 1 1 calc R U . . .
H23B H 0.4421 0.2956 0.4393 0.187 Uiso 1 1 calc R U . . .
H23C H 0.5188 0.2797 0.3705 0.187 Uiso 1 1 calc R U . . .
C27 C 0.3759(9) 0.5600(8) 0.3405(14) 0.111(6) Uani 1 1 d . . . . .
H27A H 0.3974 0.5703 0.2718 0.167 Uiso 1 1 calc R U . . .
H27B H 0.4108 0.5841 0.3922 0.167 Uiso 1 1 calc R U . . .
H27C H 0.3233 0.5848 0.3459 0.167 Uiso 1 1 calc R U . . .
C22 C 0.5730(15) 0.1333(8) -0.1897(14) 0.148(9) Uani 1 1 d . . . . .
C28 C 0.3102(8) 0.4263(14) 0.2865(14) 0.141(8) Uani 1 1 d . . . . .
H28A H 0.3225 0.4417 0.2155 0.211 Uiso 1 1 calc R U . . .
H28B H 0.2569 0.4450 0.3039 0.211 Uiso 1 1 calc R U . . .
H28C H 0.3131 0.3667 0.2936 0.211 Uiso 1 1 calc R U . . .
O1H O 0.7195(7) 0.5719(6) -0.1243(6) 0.097(3) Uani 1 1 d . . . . .
C15 C 0.7407(7) 0.7106(7) -0.0672(9) 0.066(3) Uani 1 1 d . . . . .
H15 H 0.7434 0.7446 -0.0081 0.079 Uiso 1 1 calc R U . . .
C24 C 0.5463(8) 0.4606(11) 0.4335(9) 0.093(3) Uani 1 1 d . . . . .
H24A H 0.5995 0.4529 0.4055 0.140 Uiso 1 1 calc R U . . .
H24B H 0.5420 0.4322 0.4996 0.140 Uiso 1 1 calc R U . . .
H24C H 0.5362 0.5191 0.4434 0.140 Uiso 1 1 calc R U . . .
O18 O 0.6976(4) 0.6035(4) 0.0418(5) 0.0535(17) Uani 1 1 d . . . . .
H18 H 0.6963 0.6450 0.0927 0.064 Uiso 1 1 calc R U . . .
C18 C 0.5581(11) 0.4019(10) -0.2666(12) 0.117(6) Uani 1 1 d . . . . .
H18B H 0.5026 0.4012 -0.2877 0.175 Uiso 1 1 calc R U . . .
H18C H 0.5919 0.4046 -0.3276 0.175 Uiso 1 1 calc R U . . .
H18D H 0.5678 0.4499 -0.2232 0.175 Uiso 1 1 calc R U . . .
C17 C 0.6902(8) 0.3113(12) -0.1663(12) 0.106(5) Uani 1 1 d . . . . .
H17 H 0.7032 0.3645 -0.1362 0.158 Uiso 1 1 calc R U . . .
H0AB H 0.7191 0.3044 -0.2310 0.158 Uiso 1 1 calc R U . . .
H0AC H 0.7051 0.2676 -0.1185 0.158 Uiso 1 1 calc R U . . .
C16 C 0.7558(9) 0.7431(9) -0.1587(12) 0.098(5) Uani 1 1 d . . . . .
H16A H 0.7533 0.7099 -0.2185 0.117 Uiso 1 1 calc R U . . .
H16B H 0.7691 0.7993 -0.1642 0.117 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O3 1.627(6) . ?
Si1 C17 1.838(13) . ?
Si1 C18 1.847(14) . ?
Si1 C19 1.885(16) . ?
C4 O3 1.441(9) . ?
C4 C3 1.501(12) . ?
C4 C5 1.536(10) . ?
C4 H4A 0.9800 . ?
C19 C22 1.51(2) . ?
C19 C20 1.522(15) . ?
C19 C21 1.53(2) . ?
C26 C25 1.537(15) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C1 C3 1.51(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Si2 O4 1.635(5) . ?
Si2 C24 1.830(13) . ?
Si2 C23 1.868(13) . ?
Si2 C25 1.883(13) . ?
C2 C3 1.50(2) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3 0.9800 . ?
O4 C7 1.437(9) . ?
C6 C5 1.527(11) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 C7 1.548(9) . ?
C5 H5 0.9800 . ?
C8 C10 1.523(10) . ?
C8 C9 1.529(11) . ?
C8 C11 1.537(11) . ?
C8 C7 1.575(9) . ?
C7 H7 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C25 C28 1.488(19) . ?
C25 C27 1.527(16) . ?
C11 O18 1.467(10) . ?
C11 C12 1.493(13) . ?
C11 H11 0.9800 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C14 O1H 1.187(12) . ?
C14 O18 1.302(10) . ?
C14 C15 1.496(14) . ?
C13 C12 1.293(15) . ?
C13 H13A 0.9300 . ?
C13 H13B 0.9300 . ?
C12 H12 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C15 C16 1.301(17) . ?
C15 H15 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O18 H18 0.9300 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 H18D 0.9600 . ?
C17 H17 0.9600 . ?
C17 H0AB 0.9600 . ?
C17 H0AC 0.9600 . ?
C16 H16A 0.9300 . ?
C16 H16B 0.9300 . ?

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
_geom_angle_publ_flag
O3 Si1 C17 112.2(5) . . ?
O3 Si1 C18 110.2(5) . . ?
C17 Si1 C18 104.9(8) . . ?
O3 Si1 C19 104.3(4) . . ?
C17 Si1 C19 110.6(7) . . ?
C18 Si1 C19 114.8(7) . . ?
O3 C4 C3 109.3(7) . . ?
O3 C4 C5 108.6(6) . . ?
C3 C4 C5 121.0(8) . . ?
O3 C4 H4A 105.6 . . ?
C3 C4 H4A 105.6 . . ?
C5 C4 H4A 105.6 . . ?
C22 C19 C20 110.4(14) . . ?
C22 C19 C21 111.5(17) . . ?
C20 C19 C21 108.8(12) . . ?
C22 C19 Si1 108.9(10) . . ?
C20 C19 Si1 109.9(10) . . ?
C21 C19 Si1 107.2(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O4 Si2 C24 112.3(5) . . ?
O4 Si2 C23 112.4(5) . . ?
C24 Si2 C23 106.1(8) . . ?
O4 Si2 C25 104.5(4) . . ?
C24 Si2 C25 112.5(6) . . ?
C23 Si2 C25 109.1(7) . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 O3 Si1 129.4(5) . . ?
C4 C3 C2 113.6(13) . . ?
C4 C3 C1 110.6(12) . . ?
C2 C3 C1 108.6(13) . . ?
C4 C3 H3 108.0 . . ?
C2 C3 H3 108.0 . . ?
C1 C3 H3 108.0 . . ?
C7 O4 Si2 131.4(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 C5 C4 111.6(7) . . ?
C6 C5 C7 110.4(6) . . ?
C4 C5 C7 118.5(6) . . ?
C6 C5 H5 105.0 . . ?
C4 C5 H5 105.0 . . ?
C7 C5 H5 105.0 . . ?
C10 C8 C9 107.9(7) . . ?
C10 C8 C11 109.9(6) . . ?
C9 C8 C11 109.6(6) . . ?
C10 C8 C7 108.1(6) . . ?
C9 C8 C7 112.6(6) . . ?
C11 C8 C7 108.6(6) . . ?
O4 C7 C5 111.8(6) . . ?
O4 C7 C8 108.8(6) . . ?
C5 C7 C8 117.5(6) . . ?
O4 C7 H7 105.9 . . ?
C5 C7 H7 105.9 . . ?
C8 C7 H7 105.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C28 C25 C27 111.9(15) . . ?
C28 C25 C26 108.6(12) . . ?
C27 C25 C26 107.1(11) . . ?
C28 C25 Si2 110.7(9) . . ?
C27 C25 Si2 108.9(8) . . ?
C26 C25 Si2 109.7(10) . . ?
O18 C11 C12 106.8(7) . . ?
O18 C11 C8 106.1(7) . . ?
C12 C11 C8 115.6(6) . . ?
O18 C11 H11 109.4 . . ?
C12 C11 H11 109.4 . . ?
C8 C11 H11 109.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1H C14 O18 125.0(9) . . ?
O1H C14 C15 123.1(9) . . ?
O18 C14 C15 111.9(8) . . ?
C12 C13 H13A 120.0 . . ?
C12 C13 H13B 120.0 . . ?
H13A C13 H13B 120.0 . . ?
C13 C12 C11 123.9(9) . . ?
C13 C12 H12 118.1 . . ?
C11 C12 H12 118.1 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C16 C15 C14 122.1(12) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14 O18 C11 118.4(7) . . ?
C14 O18 H18 120.8 . . ?
C11 O18 H18 120.8 . . ?
Si1 C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C18 H18D 109.5 . . ?
H18B C18 H18D 109.5 . . ?
H18C C18 H18D 109.5 . . ?
Si1 C17 H17 109.5 . . ?
Si1 C17 H0AB 109.5 . . ?
H17 C17 H0AB 109.5 . . ?
Si1 C17 H0AC 109.5 . . ?
H17 C17 H0AC 109.5 . . ?
H0AB C17 H0AC 109.5 . . ?
C15 C16 H16A 120.0 . . ?
C15 C16 H16B 120.0 . . ?
H16A C16 H16B 120.0 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Si1 C19 C22 -56.6(12) . . . . ?
C17 Si1 C19 C22 64.2(13) . . . . ?
C18 Si1 C19 C22 -177.3(12) . . . . ?
O3 Si1 C19 C20 -177.7(10) . . . . ?
C17 Si1 C19 C20 -56.9(13) . . . . ?
C18 Si1 C19 C20 61.6(12) . . . . ?
O3 Si1 C19 C21 64.2(12) . . . . ?
C17 Si1 C19 C21 -174.9(12) . . . . ?
C18 Si1 C19 C21 -56.4(13) . . . . ?
C3 C4 O3 Si1 128.9(9) . . . . ?
C5 C4 O3 Si1 -97.2(7) . . . . ?
C17 Si1 O3 C4 73.8(9) . . . . ?
C18 Si1 O3 C4 -42.8(9) . . . . ?
C19 Si1 O3 C4 -166.4(8) . . . . ?
O3 C4 C3 C2 51.4(13) . . . . ?
C5 C4 C3 C2 -75.9(12) . . . . ?
O3 C4 C3 C1 -71.1(14) . . . . ?
C5 C4 C3 C1 161.7(10) . . . . ?
C24 Si2 O4 C7 42.1(9) . . . . ?
C23 Si2 O4 C7 -77.4(9) . . . . ?
C25 Si2 O4 C7 164.4(6) . . . . ?
O3 C4 C5 C6 -55.9(10) . . . . ?
C3 C4 C5 C6 71.6(12) . . . . ?
O3 C4 C5 C7 174.1(6) . . . . ?
C3 C4 C5 C7 -58.4(12) . . . . ?
Si2 O4 C7 C5 114.7(6) . . . . ?
Si2 O4 C7 C8 -113.8(6) . . . . ?
C6 C5 C7 O4 -68.5(9) . . . . ?
C4 C5 C7 O4 62.0(8) . . . . ?
C6 C5 C7 C8 164.6(8) . . . . ?
C4 C5 C7 C8 -64.9(9) . . . . ?
C10 C8 C7 O4 63.6(8) . . . . ?
C9 C8 C7 O4 -55.6(7) . . . . ?
C11 C8 C7 O4 -177.2(5) . . . . ?
C10 C8 C7 C5 -168.0(7) . . . . ?
C9 C8 C7 C5 72.8(8) . . . . ?
C11 C8 C7 C5 -48.8(8) . . . . ?
O4 Si2 C25 C28 60.7(11) . . . . ?
C24 Si2 C25 C28 -177.2(11) . . . . ?
C23 Si2 C25 C28 -59.7(12) . . . . ?
O4 Si2 C25 C27 -62.7(10) . . . . ?
C24 Si2 C25 C27 59.5(12) . . . . ?
C23 Si2 C25 C27 176.9(11) . . . . ?
O4 Si2 C25 C26 -179.6(8) . . . . ?
C24 Si2 C25 C26 -57.4(10) . . . . ?
C23 Si2 C25 C26 60.0(11) . . . . ?
C10 C8 C11 O18 -58.9(8) . . . . ?
C9 C8 C11 O18 59.5(7) . . . . ?
C7 C8 C11 O18 -177.1(5) . . . . ?
C10 C8 C11 C12 59.2(9) . . . . ?
C9 C8 C11 C12 177.7(7) . . . . ?
C7 C8 C11 C12 -58.9(8) . . . . ?
O18 C11 C12 C13 -106.6(11) . . . . ?
C8 C11 C12 C13 135.6(10) . . . . ?
O1H C14 C15 C16 5.1(19) . . . . ?
O18 C14 C15 C16 -172.7(12) . . . . ?
O1H C14 O18 C11 2.9(16) . . . . ?
C15 C14 O18 C11 -179.4(8) . . . . ?
C12 C11 O18 C14 102.9(9) . . . . ?
C8 C11 O18 C14 -133.3(8) . . . . ?

_refine_diff_density_max         0.625
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.083

_shelxl_version_number           2013-3

