#------------------------------------------------------------------------------
#$Date: 2017-05-03 04:08:13 +0200 (Wed 03 de May de 2017) $
#$Revision: 195902 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/28/7042858.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_7042858
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         'C H4 Cl2 Si'
_chemical_formula_sum            'C H4 Cl2 Si'
_chemical_formula_weight         115.03
_chemical_name_systematic        methyldichlorosilane
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_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                103.99(2)
_cell_angle_beta                 96.08(2)
_cell_angle_gamma                116.596(18)
_cell_formula_units_Z            2
_cell_length_a                   5.9079(15)
_cell_length_b                   6.3658(15)
_cell_length_c                   8.112(2)
_cell_measurement_reflns_used    3090
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.67
_cell_volume                     256.52(13)
_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      140(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  0.0699
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6123
_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         27.999
_diffrn_reflns_theta_min         2.670
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.2026
_exptl_absorpt_correction_T_min  0.0092
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       column
_exptl_crystal_F_000             116
_exptl_crystal_recrystallization_method
'in situ (liquid in capillary) on difractometer'
_exptl_crystal_size_max          45.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.435(18)
_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   1.171
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0216P)²+0.0601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1171
_reflns_number_total             1239
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00300e2.cif
_cod_data_source_block           cl2simeh_01
_cod_original_cell_volume        256.53(12)
_cod_database_code               7042858
_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   0.010
_shelx_estimated_absorpt_t_max   0.354
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
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)
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 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)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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)
