# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1557624'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_audit_creation_date             2017-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H50 Cl4 Dy2 O10'
_chemical_formula_sum            'C30 H50 Cl4 Dy2 O10'
_chemical_formula_weight         1037.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H25Cl2DyO5
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.0173(5)
_cell_length_b                   14.9995(9)
_cell_length_c                   14.8171(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.402(6)
_cell_angle_gamma                90
_cell_volume                     1922.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6251
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.6600
_cell_measurement_theta_min      5.1610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.524
_exptl_absorpt_correction_T_max  0.393
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 6 -7 0.0354
1 -6 7 0.0297
-2 -6 8 0.0301
6 -1 0 0.0669
5 3 -5 0.0798
-5 2 -1 0.0574
0 -6 -7 0.0557
0 8 6 0.0049
1 -9 -3 0.0503

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.065
loop_
_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
0.0017 5.9941 -7.0107 -0.1257 0.1853 -0.9518
0.9985 -5.9920 7.0129 0.0294 -0.0571 1.0297
-2.0025 -5.9985 8.0068 0.2682 -0.4880 0.8803
6.0015 -0.9861 0.0142 -0.4986 0.7926 0.5275
5.0025 3.0079 -4.9952 -0.4693 0.8033 -0.2129
-5.0010 1.9872 -1.0138 0.3729 -0.6411 -0.5943
0.0024 -5.9929 -6.9955 0.8296 0.4614 -0.2264
-0.0023 7.9908 5.9926 -0.9385 -0.4612 0.0213
1.0017 -8.9879 -2.9878 0.7709 0.4739 0.3694

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13827
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.982
_diffrn_reflns_theta_min         4.285
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00    8.00    --  -40.90 125.00  90.00   94
  2  ω    -69.00  32.00   1.00    8.00    --  -40.90  57.00   0.00  101
  3  ω   -113.00 -13.00   1.00    8.00    --  -40.90 -57.00-150.00  100
  4  ω    -65.00  34.00   1.00    8.00    --  -40.90  37.00 150.00   99
  5  ω     36.00 116.00   1.00   25.00    --  112.00-111.00 -90.00   80
  6  ω     84.00 178.00   1.00   25.00    --  112.00  30.00 150.00   94
  7  ω     29.00 109.00   1.00   25.00    --  112.00 -94.00 150.00   80
  8  ω     36.00 116.00   1.00   25.00    --  112.00-111.00  30.00   80
  9  ω     39.00 138.00   1.00   25.00    --  112.00 -45.00 -30.00   99
 10  ω     36.00 145.00   1.00   25.00    --  112.00 -77.00  60.00  109
 11  ω     40.00 141.00   1.00   25.00    --  112.00 -61.00-180.00  101
 12  ω    100.00 178.00   1.00   25.00    --  112.00 111.00  90.00   78
 13  ω     30.00 165.00   1.00   25.00    --  112.00 -15.00 120.00  135
 14  ω   -117.00  -8.00   1.00    8.00    --  -40.90 -77.00  30.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0960689000
_diffrn_orient_matrix_UB_12      -0.0797654000
_diffrn_orient_matrix_UB_13      -0.0502871000
_diffrn_orient_matrix_UB_21      0.1283824000
_diffrn_orient_matrix_UB_22      -0.0230780000
_diffrn_orient_matrix_UB_23      -0.0461351000
_diffrn_orient_matrix_UB_31      0.0777706000
_diffrn_orient_matrix_UB_32      -0.0604059000
_diffrn_orient_matrix_UB_33      0.0841383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3182
_reflns_number_total             3572
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         1.730
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.179
_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)+(0.0479P)²+20.3939P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1524
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C13(H13A,H13B), C4(H4A,H4B), C10(H10A,H10B), C12(H12A,H12B),
 C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C7(H7A,H7B), C14(H14A,H14B), C5(H5A,
 H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Dy1 Dy 0.00822(6) 0.11488(4) 0.23730(3) 0.03142(18) Uani 1 1 d . . . . .
Cl2 Cl -0.1417(3) -0.00824(16) 0.12619(16) 0.0414(5) Uani 1 1 d . . . . .
Cl1 Cl 0.1432(3) 0.24669(16) 0.34331(16) 0.0463(6) Uani 1 1 d . . . . .
O1 O 0.1392(7) 0.0249(4) 0.3635(4) 0.0353(14) Uani 1 1 d . . . . .
O5 O 0.2314(7) 0.0580(4) 0.1996(4) 0.0346(13) Uani 1 1 d . . . . .
O2 O -0.1376(7) 0.0890(4) 0.3417(4) 0.0357(14) Uani 1 1 d . . . . .
O3 O -0.2219(8) 0.2020(5) 0.1859(4) 0.0413(15) Uani 1 1 d . . . . .
O4 O 0.0434(8) 0.2121(4) 0.1140(4) 0.0413(15) Uani 1 1 d . . . . .
C2 C -0.0811(10) 0.0463(6) 0.4179(6) 0.0295(17) Uani 1 1 d . . . . .
C3 C -0.1580(10) 0.0315(6) 0.4853(6) 0.0325(18) Uani 1 1 d . . . . .
H3 H -0.259606 0.050555 0.475032 0.039 Uiso 1 1 calc R . . . .
C1 C 0.0827(10) 0.0116(6) 0.4319(6) 0.0321(18) Uani 1 1 d . . . . .
C15 C 0.2441(11) -0.0180(6) 0.1410(7) 0.039(2) Uani 1 1 d . . . . .
H15A H 0.166829 -0.014855 0.080418 0.047 Uiso 1 1 calc R . . . .
H15B H 0.231327 -0.073625 0.171453 0.047 Uiso 1 1 calc R . . . .
C13 C 0.4975(12) 0.0215(9) 0.2280(8) 0.057(3) Uani 1 1 d . . . . .
H13A H 0.525469 -0.027931 0.271644 0.069 Uiso 1 1 calc R . . . .
H13B H 0.590738 0.052606 0.225693 0.069 Uiso 1 1 calc R . . . .
C4 C -0.2838(13) 0.2627(7) 0.2438(8) 0.049(3) Uani 1 1 d . . . . .
H4A H -0.202061 0.299604 0.282706 0.059 Uiso 1 1 calc R . . . .
H4B H -0.331487 0.229456 0.284347 0.059 Uiso 1 1 calc R . . . .
C10 C 0.0629(12) 0.2676(7) -0.0313(7) 0.045(2) Uani 1 1 d . . . . .
H10A H 0.169415 0.283133 -0.026008 0.054 Uiso 1 1 calc R . . . .
H10B H 0.006546 0.261941 -0.097249 0.054 Uiso 1 1 calc R . . . .
C12 C 0.3849(12) 0.0849(8) 0.2562(7) 0.049(3) Uani 1 1 d . . . . .
H12A H 0.393690 0.079234 0.322742 0.059 Uiso 1 1 calc R . . . .
H12B H 0.405638 0.146244 0.243064 0.059 Uiso 1 1 calc R . . . .
C8 C 0.0428(13) 0.3076(7) 0.1167(8) 0.048(2) Uani 1 1 d . . . . .
H8A H 0.145631 0.330381 0.146492 0.057 Uiso 1 1 calc R . . . .
H8B H -0.027091 0.329048 0.151030 0.057 Uiso 1 1 calc R . . . .
C11 C 0.0535(15) 0.1827(8) 0.0218(7) 0.054(3) Uani 1 1 d . . . . .
H11A H -0.037143 0.148413 -0.010463 0.064 Uiso 1 1 calc R . . . .
H11B H 0.144768 0.146326 0.028129 0.064 Uiso 1 1 calc R . . . .
C9 C -0.0107(12) 0.3354(8) 0.0165(8) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.024421 0.395141 0.008137 0.059 Uiso 1 1 calc R . . . .
H9B H -0.122560 0.333305 -0.007048 0.059 Uiso 1 1 calc R . . . .
C7 C -0.3283(12) 0.2000(8) 0.0904(7) 0.046(2) Uani 1 1 d . . . . .
H7A H -0.362010 0.139523 0.072286 0.055 Uiso 1 1 calc R . . . .
H7B H -0.278876 0.223803 0.045286 0.055 Uiso 1 1 calc R . . . .
C14 C 0.4058(12) -0.0108(8) 0.1298(8) 0.049(3) Uani 1 1 d . . . . .
H14A H 0.409928 0.032045 0.081551 0.059 Uiso 1 1 calc R . . . .
H14B H 0.443021 -0.068054 0.114940 0.059 Uiso 1 1 calc R . . . .
C5 C -0.4005(16) 0.3187(9) 0.1766(10) 0.070(4) Uani 1 1 d . . . . .
H5A H -0.352861 0.370802 0.157735 0.085 Uiso 1 1 calc R . . . .
H5B H -0.481192 0.337843 0.203831 0.085 Uiso 1 1 calc R . . . .
C6 C -0.4633(15) 0.2577(9) 0.0953(9) 0.066(3) Uani 1 1 d . . . . .
H6A H -0.502407 0.291361 0.037539 0.080 Uiso 1 1 calc R . . . .
H6B H -0.546308 0.221463 0.105292 0.080 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
Dy1 Cl2 2.587(2) . ?
Dy1 Cl1 2.603(2) . ?
Dy1 O1 2.338(6) . ?
Dy1 O5 2.393(6) . ?
Dy1 O2 2.329(6) . ?
Dy1 O3 2.388(6) . ?
Dy1 O4 2.427(6) . ?
O1 C1 1.272(10) . ?
O5 C15 1.457(11) . ?
O5 C12 1.458(11) . ?
O2 C2 1.273(10) . ?
O3 C4 1.466(12) . ?
O3 C7 1.468(11) . ?
O4 C8 1.432(12) . ?
O4 C11 1.463(11) . ?
C2 C3 1.385(12) . ?
C2 C1 1.524(12) . ?
C3 C1 1.383(12) 3_556 ?
C15 C14 1.517(13) . ?
C13 C12 1.533(16) . ?
C13 C14 1.535(15) . ?
C4 C5 1.488(16) . ?
C10 C11 1.511(14) . ?
C10 C9 1.497(15) . ?
C8 C9 1.485(14) . ?
C7 C6 1.512(15) . ?
C5 C6 1.491(17) . ?

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
Cl2 Dy1 Cl1 175.87(8) . . ?
O1 Dy1 Cl2 98.76(17) . . ?
O1 Dy1 Cl1 84.90(17) . . ?
O1 Dy1 O5 73.3(2) . . ?
O1 Dy1 O3 140.2(2) . . ?
O1 Dy1 O4 143.6(2) . . ?
O5 Dy1 Cl2 85.39(15) . . ?
O5 Dy1 Cl1 97.53(16) . . ?
O5 Dy1 O4 75.0(2) . . ?
O2 Dy1 Cl2 90.68(17) . . ?
O2 Dy1 Cl1 88.93(17) . . ?
O2 Dy1 O1 68.0(2) . . ?
O2 Dy1 O5 140.0(2) . . ?
O2 Dy1 O3 72.6(2) . . ?
O2 Dy1 O4 144.9(2) . . ?
O3 Dy1 Cl2 86.37(18) . . ?
O3 Dy1 Cl1 89.60(18) . . ?
O3 Dy1 O5 146.4(2) . . ?
O3 Dy1 O4 73.6(2) . . ?
O4 Dy1 Cl2 96.08(17) . . ?
O4 Dy1 Cl1 81.93(17) . . ?
C1 O1 Dy1 120.2(5) . . ?
C15 O5 Dy1 129.1(5) . . ?
C15 O5 C12 109.8(7) . . ?
C12 O5 Dy1 119.4(5) . . ?
C2 O2 Dy1 120.9(5) . . ?
C4 O3 Dy1 126.4(6) . . ?
C4 O3 C7 108.9(7) . . ?
C7 O3 Dy1 124.6(6) . . ?
C8 O4 Dy1 125.3(6) . . ?
C8 O4 C11 109.2(7) . . ?
C11 O4 Dy1 125.3(6) . . ?
O2 C2 C3 124.3(8) . . ?
O2 C2 C1 115.0(7) . . ?
C3 C2 C1 120.7(7) . . ?
C1 C3 C2 119.6(8) 3_556 . ?
O1 C1 C2 115.4(8) . . ?
O1 C1 C3 124.9(8) . 3_556 ?
C3 C1 C2 119.6(8) 3_556 . ?
O5 C15 C14 104.4(7) . . ?
C12 C13 C14 103.5(8) . . ?
O3 C4 C5 105.8(9) . . ?
C9 C10 C11 103.2(8) . . ?
O5 C12 C13 105.4(8) . . ?
O4 C8 C9 104.9(9) . . ?
O4 C11 C10 105.1(8) . . ?
C8 C9 C10 102.7(9) . . ?
O3 C7 C6 104.9(9) . . ?
C15 C14 C13 101.3(8) . . ?
C4 C5 C6 103.3(10) . . ?
C5 C6 C7 105.2(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.809
_oxdiff_exptl_absorpt_empirical_full_min 0.574
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1557623'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_audit_creation_date             2017-06-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H50 Cl4 O10 Y2'
_chemical_formula_sum            'C30 H50 Cl4 O10 Y2'
_chemical_formula_weight         890.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H25Cl2Y5O5
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'
Cl Cl 0.3639 0.7018 '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'
Y Y -0.2670 2.0244 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.0004(2)
_cell_length_b                   14.8832(3)
_cell_length_c                   14.8047(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.160(2)
_cell_angle_gamma                90
_cell_volume                     1904.80(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4260
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6640
_cell_measurement_theta_min      5.9020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.069
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 2 1 0.0460
1 -6 7 0.0402
6 1 -5 0.0441
6 0 -4 0.0383
1 6 -8 0.0640
-3 5 -4 0.0489
1 -9 -2 0.0338
0 -9 4 0.0315
-1 8 5 0.0248
0 10 0 0.0141

_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.056
loop_
_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
-6.0044 2.0019 0.9905 -0.9357 -0.4636 0.2108
0.9986 -5.9941 7.0265 0.2080 0.1093 -1.0075
6.0057 0.9946 -5.0041 0.9019 0.4584 0.3219
6.0055 -0.0046 -4.0001 0.9029 0.4791 0.1733
1.0030 5.9930 -8.0260 0.1032 0.0314 1.0362
-3.0012 4.9972 -4.0213 -0.4875 -0.2863 0.7431
1.0084 -9.0048 -1.9827 -0.1557 0.8570 -0.4086
0.0029 -8.9982 4.0267 -0.1431 0.4725 -0.9017
-1.0102 8.0078 4.9901 0.2179 -0.9504 0.0860
-0.0070 10.0029 -0.0219 0.2949 -0.7788 0.6151

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6301
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.981
_diffrn_reflns_theta_min         5.196
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  88.00   1.00    1.85    --   41.65-125.00  60.00   51
  2  ω     44.00 128.00   1.00    7.41    --  112.00 -77.00  30.00   84
  3  ω     30.00 106.00   1.00    7.41    --  112.00 -94.00   0.00   76
  4  ω     24.00  53.00   1.00    1.85    --   41.65-125.00-180.00   29
  5  ω     57.00  98.00   1.00    1.85    --   41.65-125.00-180.00   41
  6  ω     86.00 162.00   1.00    7.41    --  112.00  77.00 -90.00   76
  7  ω    101.00 148.00   1.00    7.41    --  112.00 111.00  90.00   47
  8  ω     79.00 177.00   1.00    7.41    --  112.00  77.00 150.00   98
  9  ω   -115.00 -17.00   1.00    1.85    --  -41.65 -37.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1707790000
_diffrn_orient_matrix_UB_12      0.0296657000
_diffrn_orient_matrix_UB_13      0.0306342000
_diffrn_orient_matrix_UB_21      0.0418279000
_diffrn_orient_matrix_UB_22      -0.0779569000
_diffrn_orient_matrix_UB_23      -0.0568908000
_diffrn_orient_matrix_UB_31      -0.0290256000
_diffrn_orient_matrix_UB_32      0.0612789000
_diffrn_orient_matrix_UB_33      -0.0869807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3034
_reflns_number_total             3443
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.625
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+0.2319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C12(H12a,H12b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,
 H16b), C17(H17a,H17b), C19(H19a,H19b), C20(H20a,H20b), C21(H21a,H21b),
 C23(H23a,H23b), C24(H24a,H24b), C26(H26a,H26b)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Y1 Y 0.50651(3) 0.11466(2) 0.73710(2) 0.01886(9) Uani 1 1 d . . . . .
Cl2 Cl 0.64099(9) 0.24724(4) 0.84297(4) 0.02991(16) Uani 1 1 d . . . . .
Cl3 Cl 0.35859(8) -0.00987(4) 0.62674(4) 0.02707(15) Uani 1 1 d . . . . .
O3 O 0.6379(2) 0.02451(13) 0.86264(12) 0.0225(4) Uani 1 1 d . . . . .
O4 O 0.7285(2) 0.05970(13) 0.69943(12) 0.0233(4) Uani 1 1 d . . . . .
O5 O 0.2773(2) 0.20183(14) 0.68584(13) 0.0261(4) Uani 1 1 d . . . . .
O6 O 0.3628(2) 0.08931(13) 0.84202(12) 0.0230(4) Uani 1 1 d . . . . .
C7 C 0.4180(3) 0.04667(17) 0.91731(17) 0.0185(5) Uani 1 1 d . . . . .
O8 O 0.5414(3) 0.21169(13) 0.61430(12) 0.0268(4) Uani 1 1 d . . . . .
C9 C 0.5825(3) 0.01169(16) 0.93126(17) 0.0189(5) Uani 1 1 d . . . . .
C10 C 0.7441(3) -0.01705(19) 0.64102(19) 0.0268(6) Uani 1 1 d . . . . .
H10A H 0.667673 -0.014298 0.580201 0.032 Uiso 1 1 calc R . . . .
H10B H 0.731722 -0.073177 0.671431 0.032 Uiso 1 1 calc R . . . .
C11 C 0.3414(3) 0.03159(18) 0.98565(17) 0.0221(5) Uani 1 1 d . . . . .
H11 H 0.239578 0.050428 0.975678 0.026 Uiso 1 1 calc R . . . .
C12 C 0.9956(4) 0.0239(2) 0.7275(2) 0.0358(7) Uani 1 1 d . . . . .
H12A H 1.025688 -0.025924 0.770955 0.043 Uiso 1 1 calc R . . . .
H12B H 1.087600 0.056475 0.724749 0.043 Uiso 1 1 calc R . . . .
C13 C 0.5599(4) 0.2676(2) 0.4677(2) 0.0316(6) Uani 1 1 d . . . . .
H13A H 0.501775 0.260760 0.402272 0.038 Uiso 1 1 calc R . . . .
H13B H 0.665901 0.283342 0.471041 0.038 Uiso 1 1 calc R . . . .
C15 C 0.2148(4) 0.2617(2) 0.7444(2) 0.0325(6) Uani 1 1 d . . . . .
H15A H 0.295861 0.298598 0.784104 0.039 Uiso 1 1 calc R . . . .
H15B H 0.165286 0.227720 0.783814 0.039 Uiso 1 1 calc R . . . .
C16 C 0.5535(4) 0.1831(2) 0.52250(19) 0.0352(7) Uani 1 1 d . . . . .
H16A H 0.464494 0.147060 0.490603 0.042 Uiso 1 1 calc R . . . .
H16B H 0.646293 0.147532 0.529227 0.042 Uiso 1 1 calc R . . . .
C17 C 0.4865(3) 0.3384(2) 0.51609(19) 0.0287(6) Uani 1 1 d . . . . .
H17A H 0.523915 0.398135 0.507925 0.034 Uiso 1 1 calc R . . . .
H17B H 0.374603 0.337514 0.492511 0.034 Uiso 1 1 calc R . . . .
C19 C 0.5396(4) 0.30916(19) 0.6175(2) 0.0314(6) Uani 1 1 d . . . . .
H19A H 0.642031 0.332429 0.647793 0.038 Uiso 1 1 calc R . . . .
H19B H 0.468664 0.330184 0.651678 0.038 Uiso 1 1 calc R . . . .
C20 C 0.1717(3) 0.1997(2) 0.59074(19) 0.0310(6) Uani 1 1 d . . . . .
H20A H 0.141077 0.138472 0.572212 0.037 Uiso 1 1 calc R . . . .
H20B H 0.221164 0.225001 0.546062 0.037 Uiso 1 1 calc R . . . .
C21 C 0.8823(4) 0.0854(3) 0.7564(2) 0.0367(7) Uani 1 1 d . . . . .
H21A H 0.890601 0.077984 0.822747 0.044 Uiso 1 1 calc R . . . .
H21B H 0.903256 0.147674 0.745095 0.044 Uiso 1 1 calc R . . . .
C23 C 0.9056(4) -0.0089(2) 0.6305(2) 0.0341(7) Uani 1 1 d . . . . .
H23A H 0.909680 0.034227 0.582142 0.041 Uiso 1 1 calc R . . . .
H23B H 0.943957 -0.066418 0.615889 0.041 Uiso 1 1 calc R . . . .
C24 C 0.0983(5) 0.3190(3) 0.6750(3) 0.0507(9) Uani 1 1 d . . . . .
H24A H 0.147708 0.370323 0.655065 0.061 Uiso 1 1 calc R . . . .
H24B H 0.017899 0.340222 0.701891 0.061 Uiso 1 1 calc R . . . .
C26 C 0.0330(4) 0.2551(3) 0.5937(2) 0.0453(8) Uani 1 1 d . . . . .
H26A H -0.047897 0.217647 0.605456 0.054 Uiso 1 1 calc R . . . .
H26B H -0.008182 0.287583 0.535267 0.054 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
Y1 Cl2 2.5999(7) . ?
Y1 Cl3 2.5819(7) . ?
Y1 O3 2.3301(17) . ?
Y1 O4 2.3652(19) . ?
Y1 O5 2.375(2) . ?
Y1 O6 2.3124(17) . ?
Y1 O8 2.4097(18) . ?
O3 C9 1.265(3) . ?
O4 C10 1.463(3) . ?
O4 C21 1.457(4) . ?
O5 C15 1.461(3) . ?
O5 C20 1.463(3) . ?
O6 C7 1.259(3) . ?
C7 C9 1.528(4) . ?
C7 C11 1.392(4) . ?
O8 C16 1.457(3) . ?
O8 C19 1.452(3) . ?
C9 C11 1.389(4) 3_657 ?
C10 C23 1.509(4) . ?
C12 C21 1.518(5) . ?
C12 C23 1.519(4) . ?
C13 C16 1.507(4) . ?
C13 C17 1.524(4) . ?
C15 C24 1.510(4) . ?
C17 C19 1.508(4) . ?
C20 C26 1.506(5) . ?
C24 C26 1.520(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
Cl3 Y1 Cl2 176.26(2) . . ?
O3 Y1 Cl2 84.74(5) . . ?
O3 Y1 Cl3 98.59(5) . . ?
O3 Y1 O4 73.40(6) . . ?
O3 Y1 O5 140.55(6) . . ?
O3 Y1 O8 143.42(7) . . ?
O4 Y1 Cl2 97.04(5) . . ?
O4 Y1 Cl3 85.60(5) . . ?
O4 Y1 O5 146.00(6) . . ?
O4 Y1 O8 74.54(7) . . ?
O5 Y1 Cl2 89.73(5) . . ?
O5 Y1 Cl3 86.61(5) . . ?
O5 Y1 O8 73.47(7) . . ?
O6 Y1 Cl2 88.42(5) . . ?
O6 Y1 Cl3 91.24(5) . . ?
O6 Y1 O3 67.98(6) . . ?
O6 Y1 O4 140.30(7) . . ?
O6 Y1 O5 72.86(7) . . ?
O6 Y1 O8 145.00(7) . . ?
O8 Y1 Cl2 82.15(5) . . ?
O8 Y1 Cl3 96.04(5) . . ?
C9 O3 Y1 120.10(16) . . ?
C10 O4 Y1 129.48(16) . . ?
C21 O4 Y1 120.09(16) . . ?
C21 O4 C10 108.4(2) . . ?
C15 O5 Y1 125.99(16) . . ?
C15 O5 C20 109.2(2) . . ?
C20 O5 Y1 124.73(17) . . ?
C7 O6 Y1 121.34(17) . . ?
O6 C7 C9 114.9(2) . . ?
O6 C7 C11 124.8(2) . . ?
C11 C7 C9 120.3(2) . . ?
C16 O8 Y1 125.99(17) . . ?
C19 O8 Y1 124.70(15) . . ?
C19 O8 C16 109.1(2) . . ?
O3 C9 C7 115.1(2) . . ?
O3 C9 C11 125.0(2) . 3_657 ?
C11 C9 C7 119.9(2) 3_657 . ?
O4 C10 C23 104.6(2) . . ?
C9 C11 C7 119.8(2) 3_657 . ?
C21 C12 C23 103.7(2) . . ?
C16 C13 C17 103.8(2) . . ?
O5 C15 C24 104.5(2) . . ?
O8 C16 C13 106.4(2) . . ?
C19 C17 C13 102.1(2) . . ?
O8 C19 C17 105.0(2) . . ?
O5 C20 C26 106.4(2) . . ?
O4 C21 C12 106.4(2) . . ?
C10 C23 C12 101.8(2) . . ?
C15 C24 C26 103.1(3) . . ?
C20 C26 C24 103.0(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.872
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1557625'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_audit_creation_date             2017-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
2,5-Bis[(trimethylsilyl)oxy]-2,5-cyclohexadiene-1,4-dione
_chemical_formula_moiety         'C12 H20 O4 Si2'
_chemical_formula_sum            'C12 H20 O4 Si2'
_chemical_formula_weight         284.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H20O4Si2
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'

_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.38820(16)
_cell_length_b                   9.9721(3)
_cell_length_c                   11.9758(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.550(3)
_cell_angle_gamma                90
_cell_volume                     750.01(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.0870
_cell_measurement_theta_min      5.8010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             304
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -2 -5 0.2067
-3 3 5 0.2165
0 -5 4 0.0331
0 -4 -6 0.0351
0 4 6 0.0466
-4 1 0 0.2569
4 -2 -2 0.2338
0 -6 -2 0.0305
0 5 -5 0.0411
0 6 0 0.0506

_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.077
loop_
_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
3.0000 -2.0000 -5.0000 0.2223 0.0305 0.9156
-3.0000 3.0000 5.0000 -0.1257 0.0609 -0.9943
0.0000 -5.0000 4.0000 -0.8911 -0.2028 0.1877
-0.0000 -4.0000 -6.0000 0.2258 -0.7470 0.6235
0.0000 4.0000 6.0000 -0.2258 0.7470 -0.6235
-4.0000 1.0000 -0.0000 0.2228 -0.6167 -0.7467
4.0000 -2.0000 -2.0000 -0.1154 0.3982 0.9283
0.0000 -6.0000 -2.0000 -0.3755 -0.6756 0.5751
-0.0000 5.0000 -5.0000 0.9932 0.1392 -0.1362
-0.0000 6.0000 -0.0000 0.5796 0.5484 -0.4722

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2455
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         5.815
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00 -20.00   1.00    1.00    --  -41.65 -37.00 -90.00   31
  2  ω    -99.00 -56.00   1.00    1.00    --  -41.65 -37.00 -90.00   43
  3  ω    -83.00  33.00   1.00    1.00    --  -41.65  19.00 120.00  116
  4  ω     80.00 172.00   1.00    1.00    --  112.00  77.00-150.00   92
  5  ω    140.00 175.00   1.00    1.00    --  112.00 111.00-180.00   35
  6  ω     42.00 138.00   1.00    1.00    --  112.00 -45.00  60.00   96
  7  ω    135.00 178.00   1.00    1.00    --  112.00  45.00  90.00   43
  8  ω     58.00 110.00   1.00    1.00    --  112.00-111.00 -60.00   52
  9  ω     35.00 105.00   1.00    1.00    --  112.00 -94.00 -30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315574000
_diffrn_orient_matrix_UB_12      0.0966008000
_diffrn_orient_matrix_UB_13      -0.1020329000
_diffrn_orient_matrix_UB_21      0.1770368000
_diffrn_orient_matrix_UB_22      0.0914045000
_diffrn_orient_matrix_UB_23      0.0635647000
_diffrn_orient_matrix_UB_31      0.1670030000
_diffrn_orient_matrix_UB_32      -0.0786942000
_diffrn_orient_matrix_UB_33      -0.0514505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1333
_reflns_number_total             1415
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.278
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.036
_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)+(0.0447P)²+0.3273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0834
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Si1 Si 0.27361(6) 0.16111(4) 0.16862(3) 0.01748(15) Uani 1 1 d . . . . .
O1 O 0.36991(16) 0.44278(11) 0.13212(9) 0.0263(3) Uani 1 1 d . . . . .
O2 O 0.08620(16) 0.23971(10) 0.07243(9) 0.0238(3) Uani 1 1 d . . . . .
C1 C 0.2003(2) 0.47233(14) 0.07167(12) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.0380(2) 0.36377(15) 0.03654(12) 0.0178(3) Uani 1 1 d . . . . .
C3 C -0.1484(2) 0.39228(15) -0.03166(12) 0.0200(3) Uani 1 1 d . . . . .
H3 H -0.246060 0.323771 -0.053607 0.024 Uiso 1 1 calc R . . . .
C4 C 0.2927(3) 0.23617(17) 0.31148(13) 0.0256(3) Uani 1 1 d . . . . .
H4A H 0.380064 0.315085 0.316910 0.038 Uiso 1 1 calc GR . . . .
H4B H 0.355086 0.172503 0.368026 0.038 Uiso 1 1 calc GR . . . .
H4C H 0.152940 0.259835 0.323590 0.038 Uiso 1 1 calc GR . . . .
C5 C 0.5323(2) 0.15054(16) 0.12032(13) 0.0253(3) Uani 1 1 d . . . . .
H5A H 0.508828 0.124688 0.041795 0.038 Uiso 1 1 calc GR . . . .
H5B H 0.620818 0.085062 0.164972 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.601316 0.236395 0.129129 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.1526(3) -0.00827(16) 0.16800(15) 0.0297(4) Uani 1 1 d . . . . .
H6A H 0.013389 -0.001012 0.186903 0.045 Uiso 1 1 calc GR . . . .
H6B H 0.240552 -0.064032 0.222905 0.045 Uiso 1 1 calc GR . . . .
H6C H 0.141467 -0.047349 0.093885 0.045 Uiso 1 1 calc GR . . . .


_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 O2 1.6939(10) . ?
Si1 C4 1.8508(16) . ?
Si1 C5 1.8510(16) . ?
Si1 C6 1.8570(16) . ?
O1 C1 1.2239(17) . ?
O2 C2 1.3273(18) . ?
C1 C2 1.505(2) . ?
C1 C3 1.450(2) 3_565 ?
C2 C3 1.345(2) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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 Si1 C4 111.12(6) . . ?
O2 Si1 C5 111.97(6) . . ?
O2 Si1 C6 100.16(6) . . ?
C4 Si1 C5 113.60(7) . . ?
C4 Si1 C6 109.18(8) . . ?
C5 Si1 C6 109.97(8) . . ?
C2 O2 Si1 138.13(10) . . ?
O1 C1 C2 118.83(13) . . ?
O1 C1 C3 122.92(14) . 3_565 ?
C3 C1 C2 118.25(12) 3_565 . ?
O2 C2 C1 118.22(12) . . ?
O2 C2 C3 121.38(14) . . ?
C3 C2 C1 120.38(13) . . ?
C1 C3 H3 119.3 3_565 . ?
C2 C3 C1 121.37(13) . 3_565 ?
C2 C3 H3 119.3 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
Si1 O2 C2 C1 12.4(2) . . . . ?
Si1 O2 C2 C3 -169.19(12) . . . . ?
O1 C1 C2 O2 -0.2(2) . . . . ?
O1 C1 C2 C3 -178.71(14) . . . . ?
O2 C2 C3 C1 -179.46(13) . . . 3_565 ?
C1 C2 C3 C1 -1.0(2) . . . 3_565 ?
C3 C1 C2 O2 179.47(13) 3_565 . . . ?
C3 C1 C2 C3 1.0(2) 3_565 . . . ?
C4 Si1 O2 C2 53.11(17) . . . . ?
C5 Si1 O2 C2 -75.09(16) . . . . ?
C6 Si1 O2 C2 168.39(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.664
