#------------------------------------------------------------------------------
#$Date: 2017-05-03 04:08:13 +0200 (Wed 03 de May de 2017) $
#$Revision: 195902 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/28/7042859.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7042859
loop_
_publ_author_name
'Wagler, Jörg'
'Gericke, Robert'
_publ_section_title
;
 Molecular structures of various alkyldichlorosilanes in the solid state
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00300E
_journal_year                    2017
_chemical_formula_moiety         'C3 H6 Cl2 Si'
_chemical_formula_sum            'C3 H6 Cl2 Si'
_chemical_formula_weight         141.07
_chemical_name_systematic        1,1-dichlorosilacyclobutane
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-23 deposited with the CCDC.
2017-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.432(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4048(4)
_cell_length_b                   11.3618(5)
_cell_length_c                   8.9222(6)
_cell_measurement_reflns_used    20330
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.91
_cell_volume                     647.33(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17335
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.908
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.2576
_exptl_absorpt_correction_T_min  0.0153
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       column
_exptl_crystal_F_000             288
_exptl_crystal_recrystallization_method
'in situ (liquid in capillary) on difractometer'
_exptl_crystal_size_max          47
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.060(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+0.2969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1474
_reflns_number_total             1560
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00300e2.cif
_cod_data_source_block           cl2sic3_03
_cod_database_code               7042859
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.011
_shelx_estimated_absorpt_t_max   0.419
_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
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'
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
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)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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_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
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)
