# 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_cl2sic4_01
_database_code_depnum_ccdc_archive 'CCDC 1529073'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        1,1-dichlorosilacyclopentane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Cl2 Si'
_chemical_formula_sum            'C4 H8 Cl2 Si'
_chemical_formula_weight         155.09

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_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, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   10.5190(5)
_cell_length_b                   7.2737(6)
_cell_length_c                   10.4185(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.558(4)
_cell_angle_gamma                90
_cell_volume                     719.14(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    16811
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      28.30

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          23.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    0.955
_shelx_estimated_absorpt_T_min   0.017
_shelx_estimated_absorpt_T_max   0.448
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0314
_exptl_absorpt_correction_T_max  0.2984
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12814
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.800
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1736
_reflns_number_gt                1682
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 120 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 212 K) followed by
 slow cooling to 170 K (at a rate of 40 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained an essentially single-crystalline
 column.
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0450P)²+0.2587P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.030(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1736
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0966
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_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
Cl1 Cl 0.92917(5) 0.68093(7) 0.07542(5) 0.04118(17) Uani 1 1 d . . . . .
Si1 Si 1.0000 0.85076(8) 0.2500 0.02501(17) Uani 1 2 d S T P . .
C1 C 0.86436(17) 1.0176(3) 0.2453(2) 0.0353(4) Uani 1 1 d . . . . .
H1A H 0.7701 0.9860 0.1699 0.042 Uiso 1 1 calc R U . . .
H1B H 0.8596 1.0235 0.3380 0.042 Uiso 1 1 calc R U . . .
C2 C 0.91931(19) 1.2003(3) 0.2118(2) 0.0394(4) Uani 1 1 d . . . . .
H2A H 0.8878 1.2124 0.1079 0.047 Uiso 1 1 calc R U . . .
H2B H 0.8815 1.3056 0.2447 0.047 Uiso 1 1 calc R U . . .
Cl2 Cl 0.67254(5) 0.62973(7) 0.31545(5) 0.04333(17) Uani 1 1 d . . . . .
Si2 Si 0.5000 0.45935(9) 0.2500 0.02720(18) Uani 1 2 d S T P . .
C3 C 0.49317(19) 0.2931(2) 0.11192(19) 0.0339(4) Uani 1 1 d . . . . .
H3A H 0.4172 0.3246 0.0175 0.041 Uiso 1 1 calc R U . . .
H3B H 0.5842 0.2880 0.1052 0.041 Uiso 1 1 calc R U . . .
C4 C 0.46196(19) 0.1096(3) 0.16821(19) 0.0356(4) Uani 1 1 d . . . . .
H4A H 0.3592 0.0959 0.1366 0.043 Uiso 1 1 calc R U . . .
H4B H 0.4953 0.0050 0.1300 0.043 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0486(3) 0.0401(3) 0.0327(3) -0.00828(17) 0.0155(2) -0.00069(18)
Si1 0.0237(3) 0.0262(3) 0.0281(3) 0.000 0.0140(2) 0.000
C1 0.0293(7) 0.0343(9) 0.0476(10) -0.0022(7) 0.0216(7) 0.0024(6)
C2 0.0390(9) 0.0311(9) 0.0510(11) 0.0034(8) 0.0222(9) 0.0058(7)
Cl2 0.0322(2) 0.0417(3) 0.0484(3) 0.0020(2) 0.0101(2) -0.00989(17)
Si2 0.0258(3) 0.0279(3) 0.0290(3) 0.000 0.0129(2) 0.000
C3 0.0398(8) 0.0357(9) 0.0325(8) -0.0016(7) 0.0216(7) -0.0013(7)
C4 0.0395(8) 0.0319(9) 0.0407(10) -0.0044(7) 0.0224(8) -0.0031(7)

_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
Cl1 Si1 2.0542(6) . ?
Si1 C1 1.8576(16) . ?
C1 C2 1.548(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.533(4) 2_755 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
Cl2 Si2 2.0560(6) . ?
Si2 C3 1.8570(17) . ?
C3 C4 1.549(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C4 1.539(4) 2_655 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?

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
C1 Si1 C1 98.40(11) 2_755 . ?
C1 Si1 Cl1 113.42(6) . 2_755 ?
C1 Si1 Cl1 113.42(6) 2_755 . ?
C1 Si1 Cl1 112.86(6) . . ?
Cl1 Si1 Cl1 106.07(4) 2_755 . ?
C2 C1 Si1 102.11(10) . . ?
C2 C1 H1A 111.3 . . ?
Si1 C1 H1A 111.3 . . ?
C2 C1 H1B 111.3 . . ?
Si1 C1 H1B 111.3 . . ?
H1A C1 H1B 109.2 . . ?
C2 C2 C1 108.71(12) 2_755 . ?
C2 C2 H2A 109.9 2_755 . ?
C1 C2 H2A 109.9 . . ?
C2 C2 H2B 109.9 2_755 . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C3 Si2 C3 98.72(11) . 2_655 ?
C3 Si2 Cl2 112.53(5) . . ?
C3 Si2 Cl2 113.71(6) 2_655 . ?
C3 Si2 Cl2 113.71(6) . 2_655 ?
Cl2 Si2 Cl2 105.86(4) . 2_655 ?
C4 C3 Si2 102.22(11) . . ?
C4 C3 H3A 111.3 . . ?
Si2 C3 H3A 111.3 . . ?
C4 C3 H3B 111.3 . . ?
Si2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C4 C4 C3 108.99(12) 2_655 . ?
C4 C4 H4A 109.9 2_655 . ?
C3 C4 H4A 109.9 . . ?
C4 C4 H4B 109.9 2_655 . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?

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
C1 Si1 C1 C2 12.88(9) 2_755 . . . ?
Cl1 Si1 C1 C2 132.34(11) 2_755 . . . ?
Cl1 Si1 C1 C2 -107.00(12) . . . . ?
Si1 C1 C2 C2 -36.2(2) . . . 2_755 ?
C3 Si2 C3 C4 12.57(8) 2_655 . . . ?
Cl2 Si2 C3 C4 132.83(10) . . . . ?
Cl2 Si2 C3 C4 -106.82(11) 2_655 . . . ?
Si2 C3 C4 C4 -35.26(18) . . . 2_655 ?

_refine_diff_density_max         0.562
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.078

_shelx_res_file                  
;

    cl2sic4_01.res created by SHELXL-2014/7


TITL cl2sic4_01
CELL  0.71073   10.5190   7.2737  10.4185   90.000  115.558   90.000
ZERR     4.00    0.0005   0.0006   0.0005    0.000    0.004    0.000
LATT 1
SYMM -X, Y, -Z+ 0.50000
SFAC C  H  Si Cl
UNIT 16  32  4  8
OMIT 0 56
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
CONF
SIZE 23 1 1
TEMP -93
WGHT    0.045000    0.258700
EXTI    0.029986
FVAR       0.94762
MOLE 1
CL1   4    0.929167    0.680934    0.075422    11.00000    0.04856    0.04013 =
         0.03274   -0.00828    0.01555   -0.00069
SI1   3    1.000000    0.850760    0.250000    10.50000    0.02372    0.02620 =
         0.02808    0.00000    0.01399    0.00000
C1    1    0.864362    1.017628    0.245280    11.00000    0.02929    0.03434 =
         0.04761   -0.00221    0.02161    0.00240
AFIX  23
H1A   2    0.770144    0.986039    0.169914    11.00000   -1.20000
H1B   2    0.859598    1.023478    0.338041    11.00000   -1.20000
AFIX   0
C2    1    0.919307    1.200326    0.211830    11.00000    0.03896    0.03107 =
         0.05103    0.00339    0.02223    0.00585
AFIX  23
H2A   2    0.887754    1.212447    0.107909    11.00000   -1.20000
H2B   2    0.881458    1.305602    0.244728    11.00000   -1.20000
AFIX   0
CL2   4    0.672544    0.629734    0.315453    11.00000    0.03221    0.04174 =
         0.04837    0.00204    0.01014   -0.00989
SI2   3    0.500000    0.459346    0.250000    10.50000    0.02583    0.02785 =
         0.02902    0.00000    0.01289    0.00000
C3    1    0.493172    0.293062    0.111923    11.00000    0.03979    0.03568 =
         0.03252   -0.00159    0.02159   -0.00132
AFIX  23
H3A   2    0.417225    0.324586    0.017525    11.00000   -1.20000
H3B   2    0.584167    0.287951    0.105221    11.00000   -1.20000
AFIX   0
C4    1    0.461959    0.109574    0.168207    11.00000    0.03949    0.03193 =
         0.04073   -0.00436    0.02236   -0.00309
AFIX  23
H4A   2    0.359172    0.095873    0.136571    11.00000   -1.20000
H4B   2    0.495271    0.005008    0.129998    11.00000   -1.20000
AFIX   0
HKLF 4

REM  cl2sic4_01
REM R1 =  0.0368 for    1682 Fo > 4sig(Fo)  and  0.0376 for all    1736 data
REM     66 parameters refined using      0 restraints

END

WGHT      0.0450      0.2567

REM Highest difference peak  0.562,  deepest hole -0.398,  1-sigma level  0.078
Q1    1   0.9274  0.7957  0.0703  11.00000  0.05    0.56
Q2    1   0.6789  0.5200  0.3113  11.00000  0.05    0.45
Q3    1   0.5000  0.1089  0.2500  10.50000  0.05    0.40
Q4    1   0.5000  0.3438  0.2500  10.50000  0.05    0.39
Q5    1   0.4816  0.4047  0.1479  11.00000  0.05    0.37
Q6    1   1.0000  0.7312  0.2500  10.50000  0.05    0.37
Q7    1   1.0000  0.9694  0.2500  10.50000  0.05    0.37
Q8    1   0.6780  0.6233  0.3966  11.00000  0.05    0.34
Q9    1   0.6794  0.7473  0.3179  11.00000  0.05    0.34
Q10   1   0.9250  0.5576  0.0774  11.00000  0.05    0.33
Q11   1   0.4769  0.2043  0.1340  11.00000  0.05    0.30
Q12   1   0.5000  0.5758  0.2500  10.50000  0.05    0.28
Q13   1   0.9396  0.6639  0.1609  11.00000  0.05    0.28
Q14   1   0.9574  0.7601  0.1738  11.00000  0.05    0.26
Q15   1   0.9376  0.6847 -0.0224  11.00000  0.05    0.22
Q16   1   1.0000  0.6142  0.2500  10.50000  0.05    0.21
Q17   1   0.9216  0.9109  0.0704  11.00000  0.05    0.19
Q18   1   1.0605  0.6293  0.2289  11.00000  0.05    0.19
Q19   1   1.0000  1.2003  0.2500  10.50000  0.05    0.19
Q20   1   0.8885  1.1122  0.2411  11.00000  0.05    0.19
;
_shelx_res_checksum              72263

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cl2sic5_01
_database_code_depnum_ccdc_archive 'CCDC 1529074'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        1,1-dichlorosilacyclohexane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H10 Cl2 Si'
_chemical_formula_sum            'C5 H10 Cl2 Si'
_chemical_formula_weight         169.12

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.1265(6)
_cell_length_b                   8.4569(6)
_cell_length_c                   10.6073(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.733(6)
_cell_angle_gamma                90
_cell_volume                     818.62(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    12556
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      28.45

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          46.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    0.845
_shelx_estimated_absorpt_T_min   0.012
_shelx_estimated_absorpt_T_max   0.485
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0206
_exptl_absorpt_correction_T_max  0.2794
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10915
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.926
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1977
_reflns_number_gt                1843
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 120 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 205 K) followed by
 slow cooling to 160 K (at a rate of 40 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained an essentially single-crystalline
 column.
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+0.3264P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1977
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0702
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.96709(4) 0.16584(5) 0.36197(4) 0.04335(13) Uani 1 1 d . . . . .
Cl2 Cl 0.68591(5) -0.06433(5) 0.42848(5) 0.05174(15) Uani 1 1 d . . . . .
Si1 Si 0.76980(4) 0.15859(4) 0.45422(4) 0.03033(12) Uani 1 1 d . . . . .
C1 C 0.80117(19) 0.20715(18) 0.62176(14) 0.0399(3) Uani 1 1 d . . . . .
H1A H 0.7116 0.1846 0.6703 0.048 Uiso 1 1 calc R U . . .
H1B H 0.8818 0.1414 0.6565 0.048 Uiso 1 1 calc R U . . .
C2 C 0.84104(19) 0.3835(2) 0.63378(15) 0.0424(4) Uani 1 1 d . . . . .
H2A H 0.8526 0.4103 0.7242 0.051 Uiso 1 1 calc R U . . .
H2B H 0.9364 0.4019 0.5929 0.051 Uiso 1 1 calc R U . . .
C3 C 0.72629(18) 0.49331(18) 0.57419(15) 0.0389(3) Uani 1 1 d . . . . .
H3A H 0.7537 0.6040 0.5935 0.047 Uiso 1 1 calc R U . . .
H3B H 0.6306 0.4725 0.6139 0.047 Uiso 1 1 calc R U . . .
C4 C 0.70798(17) 0.47613(18) 0.43100(14) 0.0363(3) Uani 1 1 d . . . . .
H4A H 0.8041 0.4942 0.3913 0.044 Uiso 1 1 calc R U . . .
H4B H 0.6402 0.5593 0.4000 0.044 Uiso 1 1 calc R U . . .
C5 C 0.64885(16) 0.31348(17) 0.38834(14) 0.0336(3) Uani 1 1 d . . . . .
H5A H 0.6471 0.3072 0.2951 0.040 Uiso 1 1 calc R U . . .
H5B H 0.5477 0.2986 0.4188 0.040 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0355(2) 0.0500(2) 0.0447(2) -0.00343(16) 0.00864(15) 0.00801(15)
Cl2 0.0615(3) 0.0312(2) 0.0628(3) -0.00541(17) 0.0096(2) -0.00499(17)
Si1 0.0338(2) 0.0276(2) 0.0296(2) -0.00009(14) 0.00276(15) 0.00490(14)
C1 0.0540(9) 0.0371(8) 0.0287(7) 0.0028(6) 0.0005(6) 0.0138(7)
C2 0.0500(9) 0.0422(8) 0.0347(8) -0.0058(6) -0.0085(6) 0.0072(7)
C3 0.0456(8) 0.0306(7) 0.0406(8) -0.0045(6) -0.0019(6) 0.0056(6)
C4 0.0381(7) 0.0315(7) 0.0392(7) 0.0064(6) -0.0038(6) 0.0009(6)
C5 0.0315(7) 0.0344(7) 0.0348(7) 0.0017(5) -0.0026(5) 0.0022(5)

_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
Cl1 Si1 2.0612(6) . ?
Cl2 Si1 2.0516(6) . ?
Si1 C1 1.8427(16) . ?
Si1 C5 1.8446(15) . ?
C1 C2 1.540(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.531(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.533(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.543(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

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
C1 Si1 C5 106.97(7) . . ?
C1 Si1 Cl2 112.72(6) . . ?
C5 Si1 Cl2 112.43(5) . . ?
C1 Si1 Cl1 108.99(6) . . ?
C5 Si1 Cl1 108.73(5) . . ?
Cl2 Si1 Cl1 106.91(2) . . ?
C2 C1 Si1 109.23(10) . . ?
C2 C1 H1A 109.8 . . ?
Si1 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
Si1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C3 C2 C1 113.20(13) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.8 . . ?
C2 C3 C4 114.65(13) . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 114.10(12) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 Si1 108.45(10) . . ?
C4 C5 H5A 110.0 . . ?
Si1 C5 H5A 110.0 . . ?
C4 C5 H5B 110.0 . . ?
Si1 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?

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
C5 Si1 C1 C2 -47.27(13) . . . . ?
Cl2 Si1 C1 C2 -171.35(9) . . . . ?
Cl1 Si1 C1 C2 70.12(11) . . . . ?
Si1 C1 C2 C3 55.64(16) . . . . ?
C1 C2 C3 C4 -64.41(19) . . . . ?
C2 C3 C4 C5 64.64(18) . . . . ?
C3 C4 C5 Si1 -55.18(15) . . . . ?
C1 Si1 C5 C4 46.61(12) . . . . ?
Cl2 Si1 C5 C4 170.87(8) . . . . ?
Cl1 Si1 C5 C4 -70.95(10) . . . . ?

_refine_diff_density_max         0.355
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.049

_shelx_res_file                  
;

    cl2sic5_01.res created by SHELXL-2014/7


TITL cl2sic5_01
CELL  0.71073    9.1265   8.4569  10.6073   90.000   90.733   90.000
ZERR     4.00    0.0006   0.0006   0.0008    0.000    0.006    0.000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC C  H  Si Cl
UNIT 20  40  4  8
OMIT 0 56
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
CONF
SIZE 46 1 1
TEMP -103
WGHT    0.024600    0.326400
EXTI    0.024136
FVAR       0.88239
MOLE 1
CL1   4    0.967088    0.165837    0.361968    11.00000    0.03552    0.05004 =
         0.04470   -0.00343    0.00864    0.00801
CL2   4    0.685911   -0.064327    0.428481    11.00000    0.06152    0.03117 =
         0.06277   -0.00541    0.00958   -0.00499
SI1   3    0.769798    0.158589    0.454223    11.00000    0.03377    0.02763 =
         0.02965   -0.00009    0.00276    0.00490
C1    1    0.801168    0.207146    0.621759    11.00000    0.05402    0.03709 =
         0.02867    0.00283    0.00053    0.01380
AFIX  23
H1A   2    0.711606    0.184599    0.670277    11.00000   -1.20000
H1B   2    0.881844    0.141391    0.656485    11.00000   -1.20000
AFIX   0
C2    1    0.841037    0.383455    0.633780    11.00000    0.04996    0.04220 =
         0.03467   -0.00575   -0.00853    0.00717
AFIX  23
H2A   2    0.852566    0.410319    0.724205    11.00000   -1.20000
H2B   2    0.936448    0.401896    0.592915    11.00000   -1.20000
AFIX   0
C3    1    0.726292    0.493312    0.574185    11.00000    0.04564    0.03059 =
         0.04055   -0.00452   -0.00186    0.00560
AFIX  23
H3A   2    0.753680    0.604040    0.593520    11.00000   -1.20000
H3B   2    0.630616    0.472498    0.613877    11.00000   -1.20000
AFIX   0
C4    1    0.707983    0.476130    0.431003    11.00000    0.03806    0.03154 =
         0.03918    0.00645   -0.00379    0.00090
AFIX  23
H4A   2    0.804122    0.494176    0.391284    11.00000   -1.20000
H4B   2    0.640178    0.559283    0.400045    11.00000   -1.20000
AFIX   0
C5    1    0.648852    0.313475    0.388344    11.00000    0.03149    0.03443 =
         0.03484    0.00174   -0.00258    0.00220
AFIX  23
H5A   2    0.647074    0.307160    0.295141    11.00000   -1.20000
H5B   2    0.547687    0.298558    0.418763    11.00000   -1.20000
AFIX   0
HKLF 4

REM  cl2sic5_01
REM R1 =  0.0287 for    1843 Fo > 4sig(Fo)  and  0.0314 for all    1977 data
REM     74 parameters refined using      0 restraints

END

WGHT      0.0246      0.3264

REM Highest difference peak  0.355,  deepest hole -0.318,  1-sigma level  0.049
Q1    1   0.6628 -0.0560  0.4951  11.00000  0.05    0.35
Q2    1   0.6287 -0.0449  0.3843  11.00000  0.05    0.26
Q3    1   0.7774  0.1713  0.5496  11.00000  0.05    0.24
Q4    1   0.8136  0.2999  0.6346  11.00000  0.05    0.24
Q5    1   0.7046  0.0423  0.4377  11.00000  0.05    0.22
Q6    1   0.7055  0.2459  0.4171  11.00000  0.05    0.21
Q7    1   1.0001  0.1880  0.4174  11.00000  0.05    0.21
Q8    1   0.7228  0.4769  0.5006  11.00000  0.05    0.20
Q9    1   0.8984  0.2019  0.4208  11.00000  0.05    0.18
Q10   1   0.8623  0.1518  0.4047  11.00000  0.05    0.16
Q11   1   0.7815  0.4384  0.6009  11.00000  0.05    0.16
Q12   1   0.6816  0.3929  0.3996  11.00000  0.05    0.14
Q13   1   0.8353 -0.0985  0.3869  11.00000  0.05    0.14
Q14   1   0.7904  0.4171  0.7594  11.00000  0.05    0.14
Q15   1   0.9692  0.2302  0.3281  11.00000  0.05    0.12
Q16   1   0.7654  0.4990  0.3811  11.00000  0.05    0.12
Q17   1   0.6345  0.1780  0.6584  11.00000  0.05    0.12
Q18   1   0.7020  0.5635  0.6033  11.00000  0.05    0.12
Q19   1   0.5377  0.2290  0.4468  11.00000  0.05    0.12
Q20   1   0.9196  0.0571  0.3938  11.00000  0.05    0.12
;
_shelx_res_checksum              41181

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cl2sime2_02
_database_code_depnum_ccdc_archive 'CCDC 1529075'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        dimethyldichlorosilane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 Cl2 Si'
_chemical_formula_sum            'C2 H6 Cl2 Si'
_chemical_formula_weight         129.06

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

_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, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.7688(12)
_cell_length_b                   9.1937(14)
_cell_length_c                   7.9480(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     640.75(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    5022
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      28.25

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          30.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    1.057
_shelx_estimated_absorpt_T_min   0.013
_shelx_estimated_absorpt_T_max   0.418
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0113
_exptl_absorpt_correction_T_max  0.1823
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3441
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.210
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             446
_reflns_number_gt                422
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 150 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 192 K) followed by
 slow cooling to 160 K (at a rate of 30 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained an essentially single-crystalline
 column.
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0112P)²+0.5421P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         446
_refine_ls_number_parameters     25
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_restrained_S_all      1.251
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.18678(8) 0.04109(8) 0.2500 0.0585(3) Uani 1 2 d S T P . .
Si1 Si 0.0000 0.17634(9) 0.2500 0.0335(3) Uani 1 4 d S T P . .
C1 C 0.0000 0.2818(3) 0.0538(4) 0.0504(6) Uani 1 2 d S T P . .
H1A H 0.082(2) 0.336(3) 0.052(4) 0.091(8) Uiso 1 1 d . . . . .
H1B H 0.0000 0.223(4) -0.033(5) 0.093(13) Uiso 1 2 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0532(4) 0.0686(5) 0.0538(4) 0.000 0.000 0.0244(3)
Si1 0.0355(5) 0.0330(5) 0.0318(4) 0.000 0.000 0.000
C1 0.0615(17) 0.0473(14) 0.0424(12) 0.0089(12) 0.000 0.000

_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
Cl1 Si1 2.0563(8) . ?
Si1 C1 1.836(3) . ?
C1 H1A 0.88(2) . ?
C1 H1B 0.88(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
C1 Si1 C1 116.2(2) 10_556 . ?
C1 Si1 Cl1 108.62(6) . 11 ?
C1 Si1 Cl1 108.62(6) 10_556 . ?
C1 Si1 Cl1 108.62(6) . . ?
Cl1 Si1 Cl1 105.59(6) 11 . ?
Si1 C1 H1A 108.5(18) . . ?
Si1 C1 H1B 110(2) . . ?
H1A C1 H1B 110(2) . . ?

_refine_diff_density_max         0.203
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.045

_shelx_res_file                  
;

    cl2sime2_02.res created by SHELXL-2014/7


TITL cl2sime2_02
CELL  0.71073    8.7688   9.1937   7.9480   90.000   90.000   90.000
ZERR     4.00    0.0012   0.0014   0.0009    0.000    0.000    0.000
LATT 7
SYMM -X, -Y, Z+ 0.50000
SYMM X, -Y, -Z
SYMM -X, Y, -Z+ 0.50000
SFAC C  H  Si Cl
UNIT 8  24  4  8
OMIT 0 56
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
CONF
SIZE 30 1 1
TEMP -103
WGHT    0.011200    0.542100
EXTI    0.036185
FVAR       0.95431
MOLE 1
CL1   4    0.186777    0.041091    0.250000    10.50000    0.05318    0.06858 =
         0.05384    0.00000    0.00000    0.02437
SI1   3    0.000000    0.176335    0.250000    10.25000    0.03552    0.03304 =
         0.03184    0.00000    0.00000    0.00000
C1    1    0.000000    0.281817    0.053785    10.50000    0.06151    0.04729 =
         0.04235    0.00888    0.00000    0.00000
H1A   2    0.082313    0.336280    0.051648    11.00000    0.09143
H1B   2    0.000000    0.223400   -0.033176    10.50000    0.09251

HKLF 4

REM  cl2sime2_02
REM R1 =  0.0281 for     422 Fo > 4sig(Fo)  and  0.0297 for all     446 data
REM     25 parameters refined using      0 restraints

END

WGHT      0.0113      0.5381

REM Highest difference peak  0.203,  deepest hole -0.205,  1-sigma level  0.045
Q1    1   0.0000  0.2187  0.1309  10.50000  0.05    0.20
Q2    1   0.0898  0.1033  0.1882  11.00000  0.05    0.17
Q3    1   0.2047  0.1271  0.2500  10.50000  0.05    0.15
Q4    1   0.1187  0.0101  0.1963  11.00000  0.05    0.13
Q5    1   0.0426  0.4135  0.1167  11.00000  0.05    0.11
Q6    1   0.2120  0.0786  0.1095  11.00000  0.05    0.10
Q7    1   0.2273  0.1156  0.1398  11.00000  0.05    0.09
Q8    1   0.1741  0.0000  0.0000  10.50000  0.05    0.09
Q9    1   0.1240  0.4573  0.0468  11.00000  0.05    0.09
Q10   1   0.1385  0.3297  0.0118  11.00000  0.05    0.08
Q11   1   0.0000  0.3186  0.1412  10.50000  0.05    0.08
Q12   1   0.1378  0.3844  0.1327  11.00000  0.05    0.08
Q13   1   0.0362  0.1298 -0.0514  11.00000  0.05    0.08
Q14   1   0.3014 -0.1221  0.2500  10.50000  0.05    0.07
Q15   1   0.0548  0.2798  0.0216  11.00000  0.05    0.06
Q16   1   0.2238  0.0200  0.2500  10.50000  0.05    0.06
Q17   1   0.0812  0.0281  0.0511  11.00000  0.05    0.06
Q18   1   0.1893  0.1016  0.0081  11.00000  0.05    0.06
Q19   1   0.1975  0.3772 -0.0452  11.00000  0.05    0.06
Q20   1   0.0000 -0.0188  0.1444  10.50000  0.05    0.05
;
_shelx_res_checksum              44439

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cl2simeh_01
_database_code_depnum_ccdc_archive 'CCDC 1529076'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        methyldichlorosilane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H4 Cl2 Si'
_chemical_formula_sum            'C H4 Cl2 Si'
_chemical_formula_weight         115.03

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   5.9079(15)
_cell_length_b                   6.3658(15)
_cell_length_c                   8.112(2)
_cell_angle_alpha                103.99(2)
_cell_angle_beta                 96.08(2)
_cell_angle_gamma                116.596(18)
_cell_volume                     256.53(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    3090
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      28.36

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          45.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    1.310
_shelx_estimated_absorpt_T_min   0.010
_shelx_estimated_absorpt_T_max   0.354
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0092
_exptl_absorpt_correction_T_max  0.2026
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6123
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.670
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1239
_reflns_number_gt                1171
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 115 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 173 K) followed by
 slow cooling to 140 K (at a rate of 40 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained a single-crystalline column.
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²+0.0601P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.435(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1239
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0628
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.001
_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
Cl1 Cl 0.96486(8) 0.84480(8) 0.16215(6) 0.04240(15) Uani 1 1 d . . . . .
Cl2 Cl 0.46946(8) 0.67963(8) 0.34287(6) 0.04490(16) Uani 1 1 d . . . . .
Si1 Si 0.78179(7) 0.62852(7) 0.30722(5) 0.02559(14) Uani 1 1 d . . . . .
H1 H 0.944(4) 0.720(4) 0.464(3) 0.046(5) Uiso 1 1 d . . . . .
C1 C 0.6746(4) 0.3026(3) 0.1909(2) 0.0383(3) Uani 1 1 d . . . . .
H1A H 0.563(5) 0.250(5) 0.079(4) 0.069(7) Uiso 1 1 d . . . . .
H1B H 0.583(5) 0.204(4) 0.259(3) 0.055(6) Uiso 1 1 d . . . . .
H1C H 0.816(5) 0.287(4) 0.170(3) 0.061(7) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0448(3) 0.0437(3) 0.0516(3) 0.02779(19) 0.02368(19) 0.02361(19)
Cl2 0.0424(3) 0.0547(3) 0.0595(3) 0.0265(2) 0.0256(2) 0.0351(2)
Si1 0.0263(2) 0.0262(2) 0.0261(2) 0.00815(15) 0.00606(15) 0.01463(16)
C1 0.0414(8) 0.0293(8) 0.0429(9) 0.0080(6) 0.0097(7) 0.0182(7)

_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
Cl1 Si1 2.0421(7) . ?
Cl2 Si1 2.0493(7) . ?
Si1 C1 1.8293(17) . ?
Si1 H1 1.33(2) . ?
C1 H1A 0.94(3) . ?
C1 H1B 0.96(2) . ?
C1 H1C 0.91(2) . ?

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
C1 Si1 Cl1 110.10(6) . . ?
C1 Si1 Cl2 111.06(6) . . ?
Cl1 Si1 Cl2 106.31(3) . . ?
C1 Si1 H1 114.5(8) . . ?
Cl1 Si1 H1 107.5(9) . . ?
Cl2 Si1 H1 107.0(9) . . ?
Si1 C1 H1A 110.5(15) . . ?
Si1 C1 H1B 108.8(13) . . ?
H1A C1 H1B 109.5(19) . . ?
Si1 C1 H1C 109.2(15) . . ?
H1A C1 H1C 106(2) . . ?
H1B C1 H1C 113.2(18) . . ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.056

_shelx_res_file                  
;

    cl2simeh_01.res created by SHELXL-2014/7


TITL cl2simeh_01
CELL  0.71073    5.9079   6.3658   8.1122  103.985   96.084  116.596
ZERR     2.00    0.0015   0.0015   0.0024    0.021    0.022    0.018
LATT 1
SFAC C  H  Si Cl
UNIT 2  8  2  4
OMIT 0 56
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 1 1 45
CONF
TEMP -133
WGHT    0.021600    0.060100
EXTI    0.434688
FVAR       2.26407
MOLE 1
CL1   4    0.964858    0.844804    0.162148    11.00000    0.04477    0.04371 =
         0.05160    0.02779    0.02368    0.02361
CL2   4    0.469458    0.679626    0.342874    11.00000    0.04241    0.05470 =
         0.05953    0.02647    0.02560    0.03506
SI1   3    0.781789    0.628517    0.307221    11.00000    0.02630    0.02622 =
         0.02607    0.00815    0.00606    0.01463
H1    2    0.944269    0.720077    0.463956    11.00000    0.04583
C1    1    0.674613    0.302598    0.190947    11.00000    0.04141    0.02929 =
         0.04293    0.00796    0.00975    0.01820
H1A   2    0.563118    0.249583    0.079484    11.00000    0.06903
H1B   2    0.583155    0.203672    0.258674    11.00000    0.05541
H1C   2    0.815855    0.287151    0.169681    11.00000    0.06067
HKLF 4

REM  cl2simeh_01
REM R1 =  0.0243 for    1171 Fo > 4sig(Fo)  and  0.0260 for all    1239 data
REM     54 parameters refined using      0 restraints

END

WGHT      0.0218      0.0601

REM Highest difference peak  0.377,  deepest hole -0.268,  1-sigma level  0.056
Q1    1   0.7226  0.4536  0.2496  11.00000  0.05    0.38
Q2    1   0.9115  0.7101  0.0985  11.00000  0.05    0.27
Q3    1   0.3982  0.5465  0.3153  11.00000  0.05    0.22
Q4    1   0.6205  0.9157  0.4766  11.00000  0.05    0.21
Q5    1   0.5891  0.6584  0.2913  11.00000  0.05    0.20
Q6    1   0.8357  0.6727  0.1717  11.00000  0.05    0.18
Q7    1   0.9418  0.8299  0.2538  11.00000  0.05    0.18
Q8    1   0.6338  0.6393  0.3504  11.00000  0.05    0.17
Q9    1   1.3374  0.9453  0.5375  11.00000  0.05    0.16
Q10   1   0.6019  0.9076  0.3629  11.00000  0.05    0.15
Q11   1   0.6877  0.3402  0.0518  11.00000  0.05    0.15
Q12   1   0.9715  0.8851  0.5376  11.00000  0.05    0.15
Q13   1   1.1044  0.8458  0.5712  11.00000  0.05    0.15
Q14   1   0.4364  0.8685  0.3542  11.00000  0.05    0.14
Q15   1   0.5301  0.0681  0.3570  11.00000  0.05    0.13
Q16   1   1.1174  0.9068  0.6788  11.00000  0.05    0.13
Q17   1   0.7699  0.3484 -0.0214  11.00000  0.05    0.12
Q18   1   0.8298  0.5427  0.0541  11.00000  0.05    0.12
Q19   1   0.9749  0.3836  0.2400  11.00000  0.05    0.12
Q20   1   0.5288  0.1958  0.4396  11.00000  0.05    0.12
;
_shelx_res_checksum              12837

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cl2sic3_03
_database_code_depnum_ccdc_archive 'CCDC 1529072'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        1,1-dichlorosilacyclobutane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H6 Cl2 Si'
_chemical_formula_sum            'C3 H6 Cl2 Si'
_chemical_formula_weight         141.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.4048(4)
_cell_length_b                   11.3618(5)
_cell_length_c                   8.9222(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.432(5)
_cell_angle_gamma                90
_cell_volume                     647.33(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    20330
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      28.41

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          47
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    1.053
_shelx_estimated_absorpt_T_min   0.011
_shelx_estimated_absorpt_T_max   0.419
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0153
_exptl_absorpt_correction_T_max  0.2576
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17335
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.908
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1560
_reflns_number_gt                1474
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 140 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 208 K) followed by
 slow cooling to 170 K (at a rate of 40 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained an essentially single-crystalline
 column.
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+0.2969P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.060(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1560
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0871
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_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
Cl1 Cl 1.36170(8) 0.11471(5) 0.40015(6) 0.05157(18) Uani 1 1 d . . . . .
Cl2 Cl 0.90427(9) 0.07597(5) 0.21452(7) 0.0585(2) Uani 1 1 d . . . . .
Si1 Si 1.06308(7) 0.17974(4) 0.37483(5) 0.03306(16) Uani 1 1 d . . . . .
C1 C 1.0235(3) 0.33954(16) 0.3481(2) 0.0447(4) Uani 1 1 d . . . . .
H1A H 1.1496 0.3878 0.3748 0.054 Uiso 1 1 calc R U . . .
H1B H 0.9563 0.3617 0.2484 0.054 Uiso 1 1 calc R U . . .
C2 C 0.8695(4) 0.33024(19) 0.4749(3) 0.0552(5) Uani 1 1 d . . . . .
H2A H 0.8946 0.3938 0.5500 0.066 Uiso 1 1 calc R U . . .
H2B H 0.7219 0.3336 0.4330 0.066 Uiso 1 1 calc R U . . .
C3 C 0.9234(3) 0.20739(17) 0.5451(2) 0.0448(4) Uani 1 1 d . . . . .
H3A H 0.8005 0.1559 0.5550 0.054 Uiso 1 1 calc R U . . .
H3B H 1.0151 0.2102 0.6395 0.054 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0433(3) 0.0580(3) 0.0527(3) 0.0037(2) -0.0004(2) 0.0133(2)
Cl2 0.0595(3) 0.0553(3) 0.0585(3) -0.0178(2) -0.0095(2) -0.0102(2)
Si1 0.0382(3) 0.0286(3) 0.0322(3) 0.00125(16) 0.00171(18) 0.00076(16)
C1 0.0584(11) 0.0333(9) 0.0427(9) 0.0048(7) 0.0062(8) 0.0040(8)
C2 0.0716(15) 0.0423(10) 0.0537(12) 0.0021(9) 0.0171(11) 0.0167(10)
C3 0.0520(11) 0.0430(9) 0.0403(9) 0.0045(8) 0.0102(8) 0.0018(8)

_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
Cl1 Si1 2.0465(7) . ?
Cl2 Si1 2.0604(7) . ?
Si1 C1 1.8462(19) . ?
Si1 C3 1.848(2) . ?
C1 C2 1.561(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.558(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

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
C1 Si1 C3 82.47(9) . . ?
C1 Si1 Cl1 119.14(8) . . ?
C3 Si1 Cl1 118.57(7) . . ?
C1 Si1 Cl2 114.68(7) . . ?
C3 Si1 Cl2 115.05(7) . . ?
Cl1 Si1 Cl2 106.08(3) . . ?
C2 C1 Si1 85.85(12) . . ?
C2 C1 H1A 114.3 . . ?
Si1 C1 H1A 114.3 . . ?
C2 C1 H1B 114.3 . . ?
Si1 C1 H1B 114.3 . . ?
H1A C1 H1B 111.5 . . ?
C3 C2 C1 102.66(15) . . ?
C3 C2 Si1 52.30(9) . . ?
C1 C2 Si1 52.21(9) . . ?
C3 C2 H2A 111.2 . . ?
C1 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
C1 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
C2 C3 Si1 85.89(12) . . ?
C2 C3 H3A 114.3 . . ?
Si1 C3 H3A 114.3 . . ?
C2 C3 H3B 114.3 . . ?
Si1 C3 H3B 114.3 . . ?
H3A C3 H3B 111.5 . . ?

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
C3 Si1 C1 C2 -12.14(14) . . . . ?
Cl1 Si1 C1 C2 -130.73(12) . . . . ?
Cl2 Si1 C1 C2 102.02(13) . . . . ?
Si1 C1 C2 C3 14.68(17) . . . . ?
C1 C2 C3 Si1 -14.67(17) . . . . ?
C1 Si1 C3 C2 12.17(14) . . . . ?
Cl1 Si1 C3 C2 131.33(12) . . . . ?
Cl2 Si1 C3 C2 -101.60(13) . . . . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.065

_shelx_res_file                  
;

    cl2sic3_03.res created by SHELXL-2014/7


TITL cl2sic3_03
CELL  0.71073    6.4048  11.3618   8.9222   90.000   94.432   90.000
ZERR     4.00    0.0004   0.0005   0.0006    0.000    0.005    0.000
LATT 1
SYMM -X+ 0.50000, Y+ 0.50000, -Z+ 0.50000
SFAC C  H  Si Cl
UNIT 12  24  4  8
OMIT 0 56
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 1.0 1.0 1.0
CONF
TEMP -88
WGHT    0.038300    0.296900
EXTI    0.059858
FVAR       1.22307
MOLE 1
CL1   4    1.361698    0.114707    0.400148    11.00000    0.04333    0.05801 =
         0.05272    0.00372   -0.00044    0.01329
CL2   4    0.904267    0.075969    0.214524    11.00000    0.05955    0.05532 =
         0.05848   -0.01783   -0.00954   -0.01021
SI1   3    1.063076    0.179736    0.374829    11.00000    0.03820    0.02862 =
         0.03222    0.00125    0.00171    0.00076
C1    1    1.023544    0.339542    0.348051    11.00000    0.05841    0.03329 =
         0.04274    0.00479    0.00620    0.00402
AFIX  23
H1A   2    1.149647    0.387793    0.374824    11.00000   -1.20000
H1B   2    0.956259    0.361707    0.248422    11.00000   -1.20000
AFIX   0
C2    1    0.869451    0.330239    0.474865    11.00000    0.07156    0.04233 =
         0.05375    0.00207    0.01709    0.01670
AFIX  23
H2A   2    0.894605    0.393816    0.549971    11.00000   -1.20000
H2B   2    0.721871    0.333619    0.432957    11.00000   -1.20000
AFIX   0
C3    1    0.923380    0.207388    0.545069    11.00000    0.05203    0.04305 =
         0.04026    0.00450    0.01023    0.00183
AFIX  23
H3A   2    0.800481    0.155932    0.555030    11.00000   -1.20000
H3B   2    1.015094    0.210189    0.639547    11.00000   -1.20000
AFIX   0
HKLF 4

REM  cl2sic3_03
REM R1 =  0.0327 for    1474 Fo > 4sig(Fo)  and  0.0346 for all    1560 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0383      0.2969

REM Highest difference peak  0.406,  deepest hole -0.419,  1-sigma level  0.065
Q1    1   0.9258  0.1195  0.1938  11.00000  0.05    0.41
Q2    1   0.9990  0.0656  0.2039  11.00000  0.05    0.40
Q3    1   0.9062  0.0626  0.2823  11.00000  0.05    0.36
Q4    1   0.9625  0.1781  0.4688  11.00000  0.05    0.33
Q5    1   0.8850  0.0628  0.1806  11.00000  0.05    0.29
Q6    1   0.8400  0.0735  0.2134  11.00000  0.05    0.28
Q7    1   1.2504  0.1030  0.4424  11.00000  0.05    0.26
Q8    1   1.3615  0.1791  0.4194  11.00000  0.05    0.22
Q9    1   0.9373  0.3367  0.3993  11.00000  0.05    0.20
Q10   1   0.8310  0.1945  0.6370  11.00000  0.05    0.19
Q11   1   0.7675  0.3831  0.5196  11.00000  0.05    0.16
Q12   1   1.0408  0.3987  0.2674  11.00000  0.05    0.15
Q13   1   0.7287  0.0309  0.3017  11.00000  0.05    0.14
Q14   1   1.0561  0.2643  0.3182  11.00000  0.05    0.14
Q15   1   1.4291  0.1212  0.2756  11.00000  0.05    0.14
Q16   1   1.0072  0.2171  0.5803  11.00000  0.05    0.14
Q17   1   1.1098  0.2045  0.6038  11.00000  0.05    0.14
Q18   1   0.8985  0.2618  0.4923  11.00000  0.05    0.13
Q19   1   1.3120  0.0682  0.5636  11.00000  0.05    0.13
Q20   1   1.0389  0.1544  0.1367  11.00000  0.05    0.13
;
_shelx_res_checksum              22006

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_cl3sime_01
_database_code_depnum_ccdc_archive 'CCDC 1529077'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        methyltrichlorosilane
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H3 Cl3 Si'
_chemical_formula_sum            'C H3 Cl3 Si'
_chemical_formula_weight         149.47

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'
Si Si 0.0817 0.0704 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -2yc'

_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, z+1/2'

_cell_length_a                   9.8770(8)
_cell_length_b                   6.3981(3)
_cell_length_c                   9.8704(7)
_cell_angle_alpha                90
_cell_angle_beta                 103.471(6)
_cell_angle_gamma                90
_cell_volume                     606.59(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    165(2)
_cell_measurement_reflns_used    20124
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      28.50

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_F_000             296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          40.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_exptl_absorpt_coefficient_mu    1.555
_shelx_estimated_absorpt_T_min   0.010
_shelx_estimated_absorpt_T_max   0.305
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.0143
_exptl_absorpt_correction_T_max  0.2497
_exptl_absorpt_process_details   XShape
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      165(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11014
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.184
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2936
_reflns_number_gt                2669
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_max     0.999
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 This compound is a liquid at room temperature. For crystallization
 it was transferred into a glass capillary (1 mm diameter) and
 sealed. On the diffractometer the sample was cooled to 140 K (it 
 formed a polycrystalline solid, which produced a powder diffraction
 pattern. Slow melting with retention of some of the crystalline
 material in the central and coldest part of the capillary (by
 heating the N2-flow up to 195 K) followed by
 slow cooling to 140 K (at a rate of 10 K per hour) caused the
 formation of larger crystalline domains in the parts of the
 capillary adjacent to the central polycrystalline spot. One of these
 parts of the capillary contained a larger seemingly
 single-crystalline population, which was used for data collection.
 (In spite of of various attempts at recrystallization, 
 the material always formed poly-crystalline columns.) 
 In addition to the absorption correction with a long
 needle model, to account for the absorption by this compound and
 the surrounding glass capillary container, scaling and outlier
 rejection was applied.

 The structure was refined as a 2-component inversion twin. The atomic
 coordinates themselves adhere to space group type P21/c. Refinement
 in P21/c, however, causes disorder of the methyl group with one
 chlorine atom with site occupancies of 0.5. Therefore, the structure
 was solved in space group Pc, which allowed for disorder-free
 refinement. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0717P)²+0.5312P] 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   0.5(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2936
_refine_ls_number_parameters     94
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1331
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Cl1 Cl 0.3939(2) 0.3162(3) 1.0722(2) 0.0516(4) Uani 1 1 d . . . . .
Cl2 Cl 0.1728(2) 0.6157(3) 0.8583(2) 0.0541(4) Uani 1 1 d . . . . .
Cl3 Cl 0.07138(18) 0.1652(3) 0.95646(19) 0.0519(5) Uani 1 1 d . . . . .
Si1 Si 0.23244(17) 0.3152(2) 0.90173(16) 0.0338(4) Uani 1 1 d . . . . .
C1 C 0.2806(8) 0.1851(11) 0.7536(7) 0.0430(16) Uani 1 1 d . . . . .
H1A H 0.2010 0.1870 0.6729 0.065 Uiso 1 1 calc R U . . .
H1B H 0.3072 0.0400 0.7785 0.065 Uiso 1 1 calc R U . . .
H1C H 0.3592 0.2588 0.7304 0.065 Uiso 1 1 calc R U . . .
Cl4 Cl 0.89042(19) 0.3236(3) 0.5583(2) 0.0512(5) Uani 1 1 d . . . . .
Cl5 Cl 0.56339(18) 0.1899(3) 0.45242(18) 0.0510(4) Uani 1 1 d . . . . .
Cl6 Cl 0.6860(2) 0.3259(3) 0.77738(19) 0.0521(5) Uani 1 1 d . . . . .
Si2 Si 0.73230(17) 0.1694(2) 0.61500(16) 0.0331(4) Uani 1 1 d . . . . .
C2 C 0.7807(7) -0.1050(9) 0.6611(7) 0.0398(13) Uani 1 1 d . . . . .
H2A H 0.7044 -0.1747 0.6913 0.060 Uiso 1 1 calc R U . . .
H2B H 0.8648 -0.1083 0.7369 0.060 Uiso 1 1 calc R U . . .
H2C H 0.7987 -0.1775 0.5796 0.060 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0458(9) 0.0570(10) 0.0465(8) -0.0031(7) -0.0009(7) -0.0004(7)
Cl2 0.0668(11) 0.0327(7) 0.0647(10) 0.0055(7) 0.0190(9) 0.0079(8)
Cl3 0.0441(10) 0.0538(10) 0.0599(11) 0.0098(7) 0.0164(9) -0.0087(7)
Si1 0.0358(9) 0.0289(8) 0.0368(8) 0.0008(5) 0.0089(7) 0.0002(6)
C1 0.046(4) 0.048(4) 0.037(3) -0.001(2) 0.011(3) 0.009(3)
Cl4 0.0428(9) 0.0517(10) 0.0604(11) 0.0113(7) 0.0149(8) -0.0067(7)
Cl5 0.0436(10) 0.0579(10) 0.0448(9) -0.0002(7) -0.0031(8) 0.0003(7)
Cl6 0.0650(13) 0.0502(9) 0.0423(9) -0.0083(6) 0.0147(8) 0.0080(7)
Si2 0.0353(9) 0.0314(8) 0.0325(7) 0.0001(5) 0.0075(6) -0.0001(6)
C2 0.048(4) 0.030(3) 0.041(3) 0.001(2) 0.009(3) -0.001(3)

_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
Cl1 Si1 2.031(3) . ?
Cl2 Si1 2.027(2) . ?
Cl3 Si1 2.036(2) . ?
Si1 C1 1.839(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Cl4 Si2 2.033(2) . ?
Cl5 Si2 2.032(2) . ?
Cl6 Si2 2.030(2) . ?
Si2 C2 1.848(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
C1 Si1 Cl2 112.2(2) . . ?
C1 Si1 Cl1 111.2(3) . . ?
Cl2 Si1 Cl1 107.80(11) . . ?
C1 Si1 Cl3 111.1(3) . . ?
Cl2 Si1 Cl3 107.26(11) . . ?
Cl1 Si1 Cl3 107.04(11) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 Si2 Cl6 111.5(2) . . ?
C2 Si2 Cl5 111.9(2) . . ?
Cl6 Si2 Cl5 107.29(11) . . ?
C2 Si2 Cl4 110.9(2) . . ?
Cl6 Si2 Cl4 107.86(11) . . ?
Cl5 Si2 Cl4 107.05(11) . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_refine_diff_density_max         0.472
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.082

_shelx_res_file                  
;

    cl3sime_01.res created by SHELXL-2014/7


TITL cl3sime_01
CELL  0.71073    9.8770   6.3981   9.8704   90.000  103.471   90.000
ZERR     4.00    0.0008   0.0003   0.0007    0.000    0.006    0.000
LATT -1
SYMM X, -Y, Z+ 0.50000
SFAC C  H  Si Cl
UNIT 4  12  4  12
OMIT 0 56
omit -11 0 -4
omit -3 7 3
omit 10 4 -1

L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 40 1 1
twin -1 0 0 0 -1 0 0 0 -1
CONF
TEMP -108
WGHT    0.071700    0.531200
BASF   0.51713
FVAR       0.69292
MOLE 1
CL1   4    0.393937    0.316188    1.072222    11.00000    0.04575    0.05699 =
         0.04647   -0.00310   -0.00090   -0.00043
CL2   4    0.172778    0.615687    0.858338    11.00000    0.06680    0.03272 =
         0.06473    0.00547    0.01903    0.00789
CL3   4    0.071385    0.165196    0.956458    11.00000    0.04415    0.05380 =
         0.05989    0.00981    0.01636   -0.00867
SI1   3    0.232436    0.315238    0.901734    11.00000    0.03583    0.02889 =
         0.03684    0.00083    0.00895    0.00018
C1    1    0.280563    0.185072    0.753615    11.00000    0.04556    0.04761 =
         0.03650   -0.00103    0.01078    0.00870
AFIX 137
H1A   2    0.200990    0.187041    0.672937    11.00000   -1.50000
H1B   2    0.307160    0.040039    0.778513    11.00000   -1.50000
H1C   2    0.359190    0.258759    0.730449    11.00000   -1.50000
AFIX   0
CL4   4    0.890418    0.323561    0.558264    11.00000    0.04280    0.05171 =
         0.06044    0.01130    0.01492   -0.00670
CL5   4    0.563387    0.189908    0.452420    11.00000    0.04358    0.05790 =
         0.04480   -0.00025   -0.00313    0.00026
CL6   4    0.686040    0.325883    0.777376    11.00000    0.06502    0.05019 =
         0.04228   -0.00833    0.01471    0.00803
SI2   3    0.732301    0.169379    0.615004    11.00000    0.03525    0.03144 =
         0.03253    0.00011    0.00754   -0.00011
C2    1    0.780731   -0.105017    0.661134    11.00000    0.04751    0.02986 =
         0.04129    0.00113    0.00890   -0.00050
AFIX 137
H2A   2    0.704377   -0.174659    0.691283    11.00000   -1.50000
H2B   2    0.864800   -0.108345    0.736947    11.00000   -1.50000
H2C   2    0.798693   -0.177525    0.579628    11.00000   -1.50000
AFIX   0
HKLF 4

REM  cl3sime_01
REM R1 =  0.0452 for    2669 Fo > 4sig(Fo)  and  0.0503 for all    2936 data
REM     94 parameters refined using      2 restraints

END

WGHT      0.0724      0.5245

REM Highest difference peak  0.472,  deepest hole -0.396,  1-sigma level  0.082
Q1    1   0.3134  0.3058  0.9909  11.00000  0.05    0.47
Q2    1   0.6769  0.1450  0.5157  11.00000  0.05    0.47
Q3    1   0.0501  0.1941  0.8428  11.00000  0.05    0.31
Q4    1   0.5055  0.1944  0.3781  11.00000  0.05    0.30
Q5    1   0.8175  0.2993  0.4964  11.00000  0.05    0.30
Q6    1   0.6373  0.1981  0.8549  11.00000  0.05    0.30
Q7    1   0.2849  0.2997  1.0948  11.00000  0.05    0.30
Q8    1   0.1395  0.1729  1.0239  11.00000  0.05    0.29
Q9    1   0.4432  0.3673  1.0216  11.00000  0.05    0.29
Q10   1   0.2177  0.2015  0.7961  11.00000  0.05    0.29
Q11   1   0.4611  0.3238  1.1438  11.00000  0.05    0.28
Q12   1   0.4603  0.1959  0.5062  11.00000  0.05    0.28
Q13   1   0.5560  0.3936  0.4463  11.00000  0.05    0.28
Q14   1   0.5623  0.4172  0.7400  11.00000  0.05    0.27
Q15   1   0.7942  0.3274  0.5894  11.00000  0.05    0.27
Q16   1   0.7515  0.2671  0.7205  11.00000  0.05    0.26
Q17   1   0.6736  0.1990  0.4278  11.00000  0.05    0.26
Q18   1   0.2663  0.6237  0.9430  11.00000  0.05    0.26
Q19   1   0.0844  0.3268  0.9771  11.00000  0.05    0.25
Q20   1   0.0801  0.5024  0.9627  11.00000  0.05    0.25
;
_shelx_res_checksum              40943

_exptl_crystal_recrystallization_method 
'in situ (liquid in capillary) on difractometer'
_chemical_properties_physical    ', Moisture-sensitive'
