#------------------------------------------------------------------------------
#$Date: 2018-06-29 14:42:43 +0300 (Fri, 29 Jun 2018) $
#$Revision: 208728 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/96/1549637.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_1549637
loop_
_publ_author_name
'Zipse, Hendrik'
'Marin-Luna, Marta'
'Poelloth, Benjamin'
'Zott, Fabian L.'
_publ_section_title
;
 Size-Dependent Rate Acceleration in the Silylation of Secondary Alcohols:
 the Bigger the Faster
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC01889H
_journal_year                    2018
_chemical_formula_moiety         'C30 H21 Cl Si, 0.22(H2 O)'
_chemical_formula_sum            'C30 H21.45 Cl O0.22 Si'
_chemical_formula_weight         449.06
_chemical_name_common            BP151
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_block_code                C30H21ClSi_H2O_vv740_zipse
_audit_creation_method           'APEX3 v2017.3-0'
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.2923(11)
_cell_length_b                   17.2923(11)
_cell_length_c                   13.9863(10)
_cell_measurement_reflns_used    3333
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      26.3616
_cell_measurement_theta_min      3.0859
_cell_volume                     3621.9(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v2016.5-0, Bruker AXS (2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture TXS'
_diffrn_measurement_method       'mix of phi and omega scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8776
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.215
_diffrn_source                   'rotating anode (TXS)'
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0481
_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)+(0.0543P)²+8.1057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1263
_reflns_number_total             1649
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc01889h3.cif
_cod_data_source_block           vv740
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3621.9(5)
_cod_database_code               1549637
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.993
_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
O1 O 0.5062(15) 0.5071(15) 0.4526(15) 0.038(8) Uiso 0.075(6) 1 d . . .
Cl1 Cl 0.666667 0.333333 0.71610(7) 0.0407(3) Uani 1 3 d S T P
Si1 Si 0.666667 0.333333 0.56771(7) 0.0257(3) Uani 1 3 d S T P
C1 C 0.54763(15) 0.27929(15) 0.53033(16) 0.0299(5) Uani 1 1 d . . .
C2 C 0.52193(16) 0.31227(16) 0.45583(16) 0.0332(5) Uani 1 1 d . . .
H2 H 0.565802 0.363882 0.423262 0.040 Uiso 1 1 calc R U .
C3 C 0.43102(16) 0.27152(16) 0.42530(16) 0.0347(6) Uani 1 1 d . . .
C4 C 0.40505(19) 0.3030(2) 0.3461(2) 0.0497(7) Uani 1 1 d . . .
H4 H 0.448360 0.353864 0.312016 0.060 Uiso 1 1 calc R U .
C5 C 0.3172(2) 0.2606(2) 0.3176(2) 0.0601(8) Uani 1 1 d . . .
H5 H 0.300523 0.281097 0.262669 0.072 Uiso 1 1 calc R U .
C6 C 0.2523(2) 0.1876(2) 0.3690(3) 0.0592(8) Uani 1 1 d . . .
H6 H 0.191590 0.159888 0.349666 0.071 Uiso 1 1 calc R U .
C7 C 0.27500(18) 0.1559(2) 0.4460(2) 0.0524(7) Uani 1 1 d . . .
H7 H 0.230047 0.106417 0.480333 0.063 Uiso 1 1 calc R U .
C8 C 0.36646(16) 0.19643(16) 0.47626(18) 0.0383(6) Uani 1 1 d . . .
C9 C 0.39301(17) 0.16295(18) 0.55329(19) 0.0457(7) Uani 1 1 d . . .
H9 H 0.349573 0.112469 0.587731 0.055 Uiso 1 1 calc R U .
C10 C 0.48089(17) 0.20245(17) 0.57906(19) 0.0411(6) Uani 1 1 d . . .
H10 H 0.497797 0.178166 0.630512 0.049 Uiso 1 1 calc R U .
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Si1 C1 112.43(6) 2_655 .
C1 Si1 C1 112.43(6) 2_655 3_665
C1 Si1 C1 112.42(6) . 3_665
C1 Si1 Cl1 106.33(7) 2_655 .
C1 Si1 Cl1 106.33(7) . .
C1 Si1 Cl1 106.33(7) 3_665 .
C2 C1 C10 118.3(2) . .
C2 C1 Si1 120.97(18) . .
C10 C1 Si1 120.74(17) . .
C1 C2 C3 122.0(2) . .
C1 C2 H2 119.0 . .
C3 C2 H2 119.0 . .
C4 C3 C8 119.8(2) . .
C4 C3 C2 122.1(2) . .
C8 C3 C2 118.2(2) . .
C5 C4 C3 120.3(3) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.5(3) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C7 C6 C5 120.7(3) . .
C7 C6 H6 119.6 . .
C5 C6 H6 119.6 . .
C6 C7 C8 120.6(3) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C9 C8 C3 119.7(2) . .
C9 C8 C7 122.2(3) . .
C3 C8 C7 118.1(2) . .
C10 C9 C8 120.5(2) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C1 121.3(2) . .
C9 C10 H10 119.3 . .
C1 C10 H10 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 O1 1.34(4) 10_666
Cl1 Si1 2.0755(14) .
Si1 C1 1.860(2) 2_655
Si1 C1 1.860(2) .
Si1 C1 1.860(2) 3_665
C1 C2 1.364(3) .
C1 C10 1.424(3) .
C2 C3 1.429(3) .
C2 H2 0.9500 .
C3 C4 1.404(4) .
C3 C8 1.411(3) .
C4 C5 1.374(4) .
C4 H4 0.9500 .
C5 C6 1.398(5) .
C5 H5 0.9500 .
C6 C7 1.351(4) .
C6 H6 0.9500 .
C7 C8 1.437(4) .
C7 H7 0.9500 .
C8 C9 1.404(4) .
C9 C10 1.367(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
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
C1 Si1 C1 C2 -105.25(15) 2_655
C1 Si1 C1 C2 22.8(2) 3_665
Cl1 Si1 C1 C2 138.79(17) .
C1 Si1 C1 C10 74.9(3) 2_655
C1 Si1 C1 C10 -156.99(18) 3_665
Cl1 Si1 C1 C10 -41.0(2) .
C10 C1 C2 C3 -0.7(3) .
Si1 C1 C2 C3 179.50(17) .
C1 C2 C3 C4 -177.2(2) .
C1 C2 C3 C8 1.8(3) .
C8 C3 C4 C5 -0.5(4) .
C2 C3 C4 C5 178.4(3) .
C3 C4 C5 C6 2.2(5) .
C4 C5 C6 C7 -1.7(5) .
C5 C6 C7 C8 -0.3(4) .
C4 C3 C8 C9 177.6(2) .
C2 C3 C8 C9 -1.3(3) .
C4 C3 C8 C7 -1.5(4) .
C2 C3 C8 C7 179.5(2) .
C6 C7 C8 C9 -177.2(3) .
C6 C7 C8 C3 1.9(4) .
C3 C8 C9 C10 -0.1(4) .
C7 C8 C9 C10 179.0(3) .
C8 C9 C10 C1 1.3(4) .
C2 C1 C10 C9 -0.9(4) .
Si1 C1 C10 C9 179.0(2) .
