 
data_(OSSOtBu)TiCl2
# start Validation Reply Form
_vrf_RINTA01_OSSOtBuTiCl2
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Due to the poor crystal quality a small very weakly diffracting 
crystal was selected. The high Rint depends on the fact that a large proportion 
of essentially "unobserved" reflections are being used in the refinement.
; 
_audit_creation_method            SHELXL-2014/6
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C36 H48 Cl2 O2 S2 Ti' 
_chemical_formula_weight          695.66

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ti'  'Ti'   0.2776   0.4457
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    14.2494(6)
_cell_length_b                    15.1062(7)
_cell_length_c                    17.1323(7)
_cell_angle_alpha                 90
_cell_angle_beta                  101.223(3)
_cell_angle_gamma                 90
_cell_volume                      3617.3(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     1347
_cell_measurement_theta_min       2.17
_cell_measurement_theta_max       15.47
 
_exptl_crystal_description        'irregular'
_exptl_crystal_colour             'yellow'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.277          
_exptl_crystal_F_000              1472
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.10
_exptl_absorpt_coefficient_mu     0.530
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5873
_exptl_absorpt_correction_T_max   0.7457
_exptl_absorpt_process_details    SADABS
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             50482
_diffrn_reflns_av_unetI/netI      0.1403
_diffrn_reflns_av_R_equivalents   0.2416
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.457
_diffrn_reflns_theta_max          24.498
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.918
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.918
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.918
_reflns_number_total              6012
_reflns_number_gt                 2777
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)] 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_number_reflns          6012
_refine_ls_number_parameters      401
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1723
_refine_ls_R_factor_gt            0.0581
_refine_ls_wR_factor_ref          0.1099
_refine_ls_wR_factor_gt           0.0830
_refine_ls_goodness_of_fit_ref    1.109
_refine_ls_restrained_S_all       1.109
_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
Ti Ti 0.64595(6) 0.77961(5) 0.71584(6) 0.0432(3) Uani 1 1 d . . . . .
S1 S 0.61639(9) 0.61543(8) 0.75001(8) 0.0418(4) Uani 1 1 d . . . . .
S2 S 0.66371(9) 0.69829(8) 0.58554(8) 0.0463(4) Uani 1 1 d . . . . .
Cl2 Cl 0.68037(10) 0.90571(8) 0.65491(9) 0.0682(5) Uani 1 1 d . . . . .
Cl1 Cl 0.62196(10) 0.82416(10) 0.83745(9) 0.0719(5) Uani 1 1 d . . . . .
O2 O 0.7723(2) 0.74436(19) 0.75233(18) 0.0403(9) Uani 1 1 d . . . . .
O1 O 0.5177(2) 0.77528(19) 0.67270(18) 0.0422(9) Uani 1 1 d . . . . .
C23 C 0.8226(3) 0.6675(3) 0.7535(3) 0.0373(13) Uani 1 1 d . . . . .
C24 C 0.8286(3) 0.6309(3) 0.6799(3) 0.0361(13) Uani 1 1 d . . . . .
C1 C 0.4327(4) 0.7321(3) 0.6558(3) 0.0379(13) Uani 1 1 d . . . . .
C2 C 0.4194(3) 0.6557(3) 0.6998(3) 0.0356(13) Uani 1 1 d . . . . .
C6 C 0.3566(4) 0.7628(3) 0.5964(3) 0.0369(13) Uani 1 1 d . . . . .
C3 C 0.3327(4) 0.6119(3) 0.6848(3) 0.0423(14) Uani 1 1 d . . . . .
H3 H 0.3261 0.5603 0.7129 0.051 Uiso 1 1 calc R U . . .
C16 C 0.6055(3) 0.5519(3) 0.6617(3) 0.0396(13) Uani 1 1 d . . . . .
C28 C 0.8631(3) 0.6230(3) 0.8239(3) 0.0415(14) Uani 1 1 d . . . . .
C15 C 0.4950(3) 0.6237(3) 0.7673(3) 0.0430(14) Uani 1 1 d . . . . .
H15A H 0.4761 0.5657 0.7830 0.052 Uiso 1 1 calc R U . . .
H15B H 0.4957 0.6631 0.8121 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6285(3) 0.5869(3) 0.5927(3) 0.0391(13) Uani 1 1 d . . . . .
C22 C 0.7937(3) 0.6837(3) 0.6065(3) 0.0427(14) Uani 1 1 d . . . . .
H22B H 0.8125 0.6543 0.5616 0.051 Uiso 1 1 calc R U . . .
H22A H 0.8240 0.7414 0.6123 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2549(4) 0.6422(3) 0.6294(3) 0.0401(13) Uani 1 1 d . . . . .
C26 C 0.8866(3) 0.4928(3) 0.7427(3) 0.0421(14) Uani 1 1 d . . . . .
C7 C 0.1591(4) 0.5936(3) 0.6191(3) 0.0473(14) Uani 1 1 d . . . . .
C27 C 0.8905(3) 0.5359(3) 0.8151(3) 0.0455(14) Uani 1 1 d . . . . .
H27 H 0.9133 0.5039 0.8612 0.055 Uiso 1 1 calc R U . . .
C5 C 0.2704(3) 0.7169(3) 0.5858(3) 0.0429(14) Uani 1 1 d . . . . .
H5 H 0.2199 0.7374 0.5472 0.051 Uiso 1 1 calc R U . . .
C25 C 0.8586(3) 0.5437(3) 0.6757(3) 0.0433(14) Uani 1 1 d . . . . .
H25 H 0.8597 0.5191 0.6261 0.052 Uiso 1 1 calc R U . . .
C11 C 0.3668(4) 0.8465(3) 0.5470(3) 0.0451(14) Uani 1 1 d . . . . .
C17 C 0.5810(3) 0.4634(3) 0.6641(3) 0.0528(15) Uani 1 1 d . . . . .
H17 H 0.5637 0.4401 0.7094 0.063 Uiso 1 1 calc R U . . .
C33 C 0.8743(4) 0.6612(3) 0.9086(3) 0.0480(15) Uani 1 1 d . . . . .
C20 C 0.6277(3) 0.5317(4) 0.5277(3) 0.0518(15) Uani 1 1 d . . . . .
H20 H 0.6415 0.5552 0.4810 0.062 Uiso 1 1 calc R U . . .
C29 C 0.9046(4) 0.3935(3) 0.7411(3) 0.0467(14) Uani 1 1 d . . . . .
C13 C 0.3901(4) 0.9267(3) 0.6014(3) 0.0623(17) Uani 1 1 d . . . . .
H13C H 0.3908 0.9790 0.5697 0.094 Uiso 1 1 calc R U . . .
H13A H 0.4518 0.9188 0.6351 0.094 Uiso 1 1 calc R U . . .
H13B H 0.3425 0.9328 0.6337 0.094 Uiso 1 1 calc R U . . .
C19 C 0.6070(4) 0.4432(4) 0.5311(4) 0.0636(18) Uani 1 1 d . . . . .
H19 H 0.6096 0.4064 0.4880 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4467(4) 0.8349(3) 0.4988(3) 0.0658(17) Uani 1 1 d . . . . .
H14B H 0.4490 0.8862 0.4661 0.099 Uiso 1 1 calc R U . . .
H14C H 0.4338 0.7834 0.4656 0.099 Uiso 1 1 calc R U . . .
H14A H 0.5071 0.8279 0.5346 0.099 Uiso 1 1 calc R U . . .
C35 C 0.8793(4) 0.7616(3) 0.9099(3) 0.0622(17) Uani 1 1 d . . . . .
H35A H 0.9260 0.7810 0.8801 0.093 Uiso 1 1 calc R U . . .
H35B H 0.8972 0.7817 0.9639 0.093 Uiso 1 1 calc R U . . .
H35C H 0.8178 0.7854 0.8865 0.093 Uiso 1 1 calc R U . . .
C18 C 0.5823(4) 0.4099(4) 0.5990(4) 0.0652(18) Uani 1 1 d . . . . .
H18 H 0.5664 0.3503 0.6012 0.078 Uiso 1 1 calc R U . . .
C8 C 0.0768(3) 0.6467(3) 0.5702(3) 0.0654(17) Uani 1 1 d . . . . .
H8C H 0.0180 0.6146 0.5673 0.098 Uiso 1 1 calc R U . . .
H8B H 0.0886 0.6557 0.5175 0.098 Uiso 1 1 calc R U . . .
H8A H 0.0721 0.7029 0.5952 0.098 Uiso 1 1 calc R U . . .
C12 C 0.2739(4) 0.8676(3) 0.4878(3) 0.0715(19) Uani 1 1 d . . . . .
H12B H 0.2235 0.8788 0.5164 0.107 Uiso 1 1 calc R U . . .
H12A H 0.2568 0.8182 0.4527 0.107 Uiso 1 1 calc R U . . .
H12C H 0.2834 0.9190 0.4573 0.107 Uiso 1 1 calc R U . . .
C10 C 0.1337(4) 0.5757(4) 0.7007(3) 0.083(2) Uani 1 1 d . . . . .
H10C H 0.0716 0.5488 0.6936 0.124 Uiso 1 1 calc R U . . .
H10A H 0.1333 0.6306 0.7290 0.124 Uiso 1 1 calc R U . . .
H10B H 0.1804 0.5367 0.7307 0.124 Uiso 1 1 calc R U . . .
C32 C 1.0064(4) 0.3702(3) 0.7853(3) 0.079(2) Uani 1 1 d . . . . .
H32A H 1.0523 0.3937 0.7566 0.119 Uiso 1 1 calc R U . . .
H32B H 1.0132 0.3071 0.7891 0.119 Uiso 1 1 calc R U . . .
H32C H 1.0171 0.3954 0.8377 0.119 Uiso 1 1 calc R U . . .
C30 C 0.8937(4) 0.3583(3) 0.6562(3) 0.082(2) Uani 1 1 d . . . . .
H30A H 0.9406 0.3855 0.6307 0.122 Uiso 1 1 calc R U . . .
H30B H 0.8308 0.3719 0.6270 0.122 Uiso 1 1 calc R U . . .
H30C H 0.9028 0.2953 0.6576 0.122 Uiso 1 1 calc R U . . .
C31 C 0.8302(4) 0.3466(3) 0.7800(4) 0.086(2) Uani 1 1 d . . . . .
H31A H 0.8361 0.2837 0.7745 0.129 Uiso 1 1 calc R U . . .
H31C H 0.7672 0.3650 0.7545 0.129 Uiso 1 1 calc R U . . .
H31B H 0.8407 0.3617 0.8355 0.129 Uiso 1 1 calc R U . . .
C34 C 0.7916(5) 0.6308(4) 0.9463(4) 0.119(3) Uani 1 1 d . . . . .
H34B H 0.7328 0.6549 0.9171 0.178 Uiso 1 1 calc R U . . .
H34A H 0.8015 0.6510 1.0005 0.178 Uiso 1 1 calc R U . . .
H34C H 0.7882 0.5673 0.9453 0.178 Uiso 1 1 calc R U . . .
C9 C 0.1662(4) 0.5053(3) 0.5768(4) 0.091(2) Uani 1 1 d . . . . .
H9C H 0.2163 0.4702 0.6075 0.136 Uiso 1 1 calc R U . . .
H9A H 0.1803 0.5161 0.5251 0.136 Uiso 1 1 calc R U . . .
H9B H 0.1065 0.4742 0.5713 0.136 Uiso 1 1 calc R U . . .
C36 C 0.9700(5) 0.6295(4) 0.9588(3) 0.117(3) Uani 1 1 d . . . . .
H36C H 0.9655 0.5677 0.9707 0.176 Uiso 1 1 calc R U . . .
H36A H 0.9838 0.6626 1.0075 0.176 Uiso 1 1 calc R U . . .
H36B H 1.0202 0.6383 0.9295 0.176 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
Ti O1 1.835(3) . ?
Ti O2 1.864(3) . ?
Ti Cl2 2.2711(16) . ?
Ti Cl1 2.2777(17) . ?
Ti S1 2.6015(15) . ?
Ti S2 2.6032(16) . ?
S1 C16 1.772(5) . ?
S1 C15 1.815(4) . ?
S2 C21 1.767(5) . ?
S2 C22 1.830(4) . ?
O2 C23 1.363(5) . ?
O1 C1 1.356(5) . ?
C23 C24 1.394(6) . ?
C23 C28 1.403(6) . ?
C24 C25 1.392(6) . ?
C24 C22 1.490(6) . ?
C1 C2 1.412(6) . ?
C1 C6 1.413(6) . ?
C2 C3 1.381(6) . ?
C2 C15 1.499(6) . ?
C6 C5 1.392(6) . ?
C6 C11 1.544(6) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C16 C17 1.384(6) . ?
C16 C21 1.392(6) . ?
C28 C27 1.388(6) . ?
C28 C33 1.541(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C21 C20 1.390(6) . ?
C22 H22B 0.9700 . ?
C22 H22A 0.9700 . ?
C4 C5 1.395(6) . ?
C4 C7 1.529(6) . ?
C26 C25 1.375(6) . ?
C26 C27 1.392(6) . ?
C26 C29 1.524(6) . ?
C7 C8 1.529(6) . ?
C7 C9 1.530(6) . ?
C7 C10 1.536(6) . ?
C27 H27 0.9300 . ?
C5 H5 0.9300 . ?
C25 H25 0.9300 . ?
C11 C13 1.526(6) . ?
C11 C12 1.536(6) . ?
C11 C14 1.542(6) . ?
C17 C18 1.380(6) . ?
C17 H17 0.9300 . ?
C33 C35 1.518(6) . ?
C33 C34 1.521(7) . ?
C33 C36 1.540(7) . ?
C20 C19 1.373(6) . ?
C20 H20 0.9300 . ?
C29 C30 1.528(6) . ?
C29 C31 1.532(6) . ?
C29 C32 1.540(7) . ?
C13 H13C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C19 C18 1.376(7) . ?
C19 H19 0.9300 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 H14A 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C18 H18 0.9300 . ?
C8 H8C 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12C 0.9600 . ?
C10 H10C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31C 0.9600 . ?
C31 H31B 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34C 0.9600 . ?
C9 H9C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C36 H36C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 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
O1 Ti O2 161.09(14) . . ?
O1 Ti Cl2 97.59(10) . . ?
O2 Ti Cl2 96.48(10) . . ?
O1 Ti Cl1 93.67(11) . . ?
O2 Ti Cl1 94.86(11) . . ?
Cl2 Ti Cl1 104.89(6) . . ?
O1 Ti S1 82.20(10) . . ?
O2 Ti S1 80.81(10) . . ?
Cl2 Ti S1 164.15(6) . . ?
Cl1 Ti S1 90.92(6) . . ?
O1 Ti S2 83.87(10) . . ?
O2 Ti S2 84.50(10) . . ?
Cl2 Ti S2 86.32(6) . . ?
Cl1 Ti S2 168.76(6) . . ?
S1 Ti S2 77.88(5) . . ?
C16 S1 C15 104.4(2) . . ?
C16 S1 Ti 108.39(18) . . ?
C15 S1 Ti 99.91(15) . . ?
C21 S2 C22 99.3(2) . . ?
C21 S2 Ti 108.27(19) . . ?
C22 S2 Ti 98.75(16) . . ?
C23 O2 Ti 136.0(3) . . ?
C1 O1 Ti 151.8(3) . . ?
O2 C23 C24 116.7(5) . . ?
O2 C23 C28 123.2(5) . . ?
C24 C23 C28 120.0(5) . . ?
C25 C24 C23 119.7(5) . . ?
C25 C24 C22 121.2(5) . . ?
C23 C24 C22 118.8(5) . . ?
O1 C1 C2 119.1(4) . . ?
O1 C1 C6 121.6(4) . . ?
C2 C1 C6 119.2(5) . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 C15 118.2(4) . . ?
C1 C2 C15 121.6(4) . . ?
C5 C6 C1 117.7(4) . . ?
C5 C6 C11 120.7(4) . . ?
C1 C6 C11 121.5(4) . . ?
C2 C3 C4 122.4(5) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C17 C16 C21 119.6(5) . . ?
C17 C16 S1 118.6(4) . . ?
C21 C16 S1 121.5(4) . . ?
C27 C28 C23 115.9(5) . . ?
C27 C28 C33 118.5(5) . . ?
C23 C28 C33 125.5(5) . . ?
C2 C15 S1 117.5(3) . . ?
C2 C15 H15A 107.9 . . ?
S1 C15 H15A 107.9 . . ?
C2 C15 H15B 107.9 . . ?
S1 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
C20 C21 C16 119.1(5) . . ?
C20 C21 S2 118.3(4) . . ?
C16 C21 S2 122.6(4) . . ?
C24 C22 S2 112.9(3) . . ?
C24 C22 H22B 109.0 . . ?
S2 C22 H22B 109.0 . . ?
C24 C22 H22A 109.0 . . ?
S2 C22 H22A 109.0 . . ?
H22B C22 H22A 107.8 . . ?
C3 C4 C5 116.4(5) . . ?
C3 C4 C7 119.8(5) . . ?
C5 C4 C7 123.8(5) . . ?
C25 C26 C27 115.9(5) . . ?
C25 C26 C29 123.9(5) . . ?
C27 C26 C29 120.0(5) . . ?
C8 C7 C4 112.6(4) . . ?
C8 C7 C9 108.2(4) . . ?
C4 C7 C9 109.5(4) . . ?
C8 C7 C10 107.4(4) . . ?
C4 C7 C10 110.0(4) . . ?
C9 C7 C10 109.1(5) . . ?
C28 C27 C26 125.2(5) . . ?
C28 C27 H27 117.4 . . ?
C26 C27 H27 117.4 . . ?
C6 C5 C4 124.1(5) . . ?
C6 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C26 C25 C24 121.9(5) . . ?
C26 C25 H25 119.1 . . ?
C24 C25 H25 119.1 . . ?
C13 C11 C12 107.2(4) . . ?
C13 C11 C14 108.8(4) . . ?
C12 C11 C14 107.5(4) . . ?
C13 C11 C6 110.4(4) . . ?
C12 C11 C6 111.8(4) . . ?
C14 C11 C6 111.0(4) . . ?
C18 C17 C16 120.0(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C35 C33 C34 109.4(5) . . ?
C35 C33 C36 105.6(4) . . ?
C34 C33 C36 110.1(5) . . ?
C35 C33 C28 112.5(4) . . ?
C34 C33 C28 109.9(4) . . ?
C36 C33 C28 109.2(4) . . ?
C19 C20 C21 121.2(5) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C26 C29 C30 111.9(4) . . ?
C26 C29 C31 108.3(4) . . ?
C30 C29 C31 107.6(5) . . ?
C26 C29 C32 111.2(4) . . ?
C30 C29 C32 107.5(4) . . ?
C31 C29 C32 110.2(5) . . ?
C11 C13 H13C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C20 C19 C18 119.0(6) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C19 C18 C17 121.0(6) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C7 C8 H8C 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
C7 C10 H10C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
H10C C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10C C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31C C31 H31B 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34A 109.5 . . ?
H34B C34 H34A 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
C7 C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9C C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
H36C C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36C C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
 
_refine_diff_density_max    0.316
_refine_diff_density_min   -0.400
_refine_diff_density_rms    0.073

_shelxl_version_number 2014/6



