#------------------------------------------------------------------------------
#$Date: 2020-09-04 00:22:27 +0300 (Fri, 04 Sep 2020) $
#$Revision: 255827 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/79/4517994.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_4517994
loop_
_publ_author_name
'Lv, Weiwei'
'Liu, Shihan'
'Chen, Yanhui'
'Wen, Si'
'Lan, Yu'
'Cheng, Guolin'
_publ_section_title
;
 Palladium-Catalyzed Intermolecular Trans-Selective Carbofunctionalization
 of Internal Alkynes to Highly Functionalized Alkenes
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10516
_journal_paper_doi               10.1021/acscatal.0c02522
_journal_year                    2020
_chemical_formula_moiety         'C27 H34 Si2'
_chemical_formula_sum            'C27 H34 Si2'
_chemical_formula_weight         414.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.06
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.963(3)
_cell_length_b                   12.0779(15)
_cell_length_c                   28.792(5)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.43
_cell_volume                     5024.6(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12399
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0072P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                2090
_reflns_number_total             4721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs0c02522_si_003.cif
_cod_data_source_block           lvvv_0ma
_cod_original_cell_volume        5024.8(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4517994
loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si01 Si 0.73329(7) 0.49856(7) 0.28667(3) 0.0390(3) Uani 1 1 d . . .
Si02 Si 0.60064(8) 0.28106(8) 0.40493(4) 0.0428(3) Uani 1 1 d . . .
C003 C 0.7330(2) 0.4987(2) 0.38798(11) 0.0326(7) Uani 1 1 d . . .
C004 C 0.7178(2) 0.5533(2) 0.34572(11) 0.0328(7) Uani 1 1 d . . .
C005 C 0.7141(2) 0.5481(2) 0.43225(12) 0.0336(7) Uani 1 1 d . . .
C006 C 0.6248(3) 0.5859(3) 0.42993(13) 0.0432(9) Uani 1 1 d . . .
H006 H 0.5790 0.5826 0.4001 0.052 Uiso 1 1 calc R . .
C007 C 0.7824(2) 0.5586(3) 0.47611(12) 0.0393(8) Uani 1 1 d . . .
C008 C 0.7703(3) 0.1853(3) 0.40199(13) 0.0439(9) Uani 1 1 d . . .
H008 H 0.7393 0.1196 0.4071 0.053 Uiso 1 1 calc R . .
C009 C 0.7730(2) 0.3829(2) 0.39256(12) 0.0344(8) Uani 1 1 d . . .
C00A C 0.6929(2) 0.6744(2) 0.34298(11) 0.0357(8) Uani 1 1 d . . .
C00B C 0.7231(2) 0.2879(2) 0.39975(11) 0.0367(8) Uani 1 1 d . . .
C00C C 0.8638(3) 0.3725(3) 0.38823(13) 0.0417(8) Uani 1 1 d . . .
H00C H 0.8969 0.4370 0.3838 0.050 Uiso 1 1 calc R . .
C00D C 0.7626(3) 0.7524(2) 0.35971(12) 0.0434(9) Uani 1 1 d . . .
H00D H 0.8241 0.7283 0.3739 0.052 Uiso 1 1 calc R . .
C00E C 0.9062(3) 0.2703(3) 0.39023(14) 0.0507(10) Uani 1 1 d . . .
H00E H 0.9676 0.2648 0.3869 0.061 Uiso 1 1 calc R . .
C00F C 0.6040(3) 0.7117(3) 0.32209(13) 0.0532(10) Uani 1 1 d . . .
H00F H 0.5556 0.6599 0.3104 0.064 Uiso 1 1 calc R . .
C00G C 0.8830(3) 0.5321(3) 0.48122(14) 0.0547(10) Uani 1 1 d . . .
H00A H 0.8918 0.4516 0.4829 0.082 Uiso 1 1 calc R . .
H00B H 0.9209 0.5662 0.5107 0.082 Uiso 1 1 calc R . .
H00G H 0.9017 0.5612 0.4534 0.082 Uiso 1 1 calc R . .
C00H C 0.8592(3) 0.1771(3) 0.39709(14) 0.0493(10) Uani 1 1 d . . .
H00H H 0.8879 0.1066 0.3985 0.059 Uiso 1 1 calc R . .
C00I C 0.6678(3) 0.6339(3) 0.51274(13) 0.0513(10) Uani 1 1 d . . .
H00I H 0.6518 0.6609 0.5405 0.062 Uiso 1 1 calc R . .
C00J C 0.7573(3) 0.6009(3) 0.51563(13) 0.0486(10) Uani 1 1 d . . .
H00J H 0.8028 0.6074 0.5454 0.058 Uiso 1 1 calc R . .
C00K C 0.8496(3) 0.5439(3) 0.28199(15) 0.0575(11) Uani 1 1 d . . .
H00K H 0.8573 0.6232 0.2891 0.086 Uiso 1 1 calc R . .
H00L H 0.8553 0.5299 0.2493 0.086 Uiso 1 1 calc R . .
H00M H 0.8976 0.5024 0.3051 0.086 Uiso 1 1 calc R . .
C00L C 0.7430(4) 0.8644(3) 0.35578(15) 0.0625(13) Uani 1 1 d . . .
H00N H 0.7910 0.9166 0.3676 0.075 Uiso 1 1 calc R . .
C00M C 0.5572(3) 0.1357(3) 0.39431(17) 0.0641(12) Uani 1 1 d . . .
H00O H 0.5598 0.1118 0.3621 0.096 Uiso 1 1 calc R . .
H00P H 0.4931 0.1322 0.3967 0.096 Uiso 1 1 calc R . .
H00Q H 0.5959 0.0868 0.4185 0.096 Uiso 1 1 calc R . .
C00N C 0.6015(3) 0.6276(3) 0.46955(13) 0.0509(10) Uani 1 1 d . . .
H00R H 0.5401 0.6520 0.4672 0.061 Uiso 1 1 calc R . .
C00O C 0.5957(3) 0.3177(3) 0.46663(15) 0.0654(12) Uani 1 1 d . . .
H00S H 0.6298 0.2624 0.4893 0.098 Uiso 1 1 calc R . .
H00T H 0.5310 0.3194 0.4681 0.098 Uiso 1 1 calc R . .
H00U H 0.6237 0.3908 0.4751 0.098 Uiso 1 1 calc R . .
C00P C 0.7168(3) 0.3460(2) 0.27731(14) 0.0608(12) Uani 1 1 d . . .
H00V H 0.7639 0.3065 0.3017 0.091 Uiso 1 1 calc R . .
H00W H 0.7228 0.3264 0.2452 0.091 Uiso 1 1 calc R . .
H00X H 0.6551 0.3252 0.2801 0.091 Uiso 1 1 calc R . .
C00Q C 0.6557(4) 0.9003(3) 0.33516(16) 0.0717(16) Uani 1 1 d . . .
H00Y H 0.6431 0.9775 0.3325 0.086 Uiso 1 1 calc R . .
C00R C 0.5200(3) 0.3635(3) 0.35681(15) 0.0588(11) Uani 1 1 d . . .
H00Z H 0.5486 0.4348 0.3530 0.088 Uiso 1 1 calc R . .
H H 0.4620 0.3763 0.3658 0.088 Uiso 1 1 calc R . .
HA H 0.5071 0.3227 0.3264 0.088 Uiso 1 1 calc R . .
C00S C 0.6445(3) 0.5641(3) 0.23631(13) 0.0538(10) Uani 1 1 d . . .
H00 H 0.5825 0.5447 0.2391 0.081 Uiso 1 1 calc R . .
HB H 0.6524 0.5372 0.2055 0.081 Uiso 1 1 calc R . .
HC H 0.6521 0.6447 0.2380 0.081 Uiso 1 1 calc R . .
C00T C 0.5852(4) 0.8256(3) 0.31813(16) 0.0697(13) Uani 1 1 d . . .
H0AA H 0.5241 0.8510 0.3038 0.084 Uiso 1 1 calc R . .
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'
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
C00K Si01 C00S 107.98(19) . . ?
C00K Si01 C00P 111.73(18) . . ?
C00S Si01 C00P 105.37(17) . . ?
C00K Si01 C004 107.28(16) . . ?
C00S Si01 C004 108.70(15) . . ?
C00P Si01 C004 115.53(15) . . ?
C00O Si02 C00M 106.42(19) . . ?
C00O Si02 C00R 113.9(2) . . ?
C00M Si02 C00R 104.4(2) . . ?
C00O Si02 C00B 110.40(18) . . ?
C00M Si02 C00B 109.46(17) . . ?
C00R Si02 C00B 111.89(17) . . ?
C004 C003 C005 123.2(3) . . ?
C004 C003 C009 120.0(3) . . ?
C005 C003 C009 116.8(3) . . ?
C003 C004 C00A 120.2(3) . . ?
C003 C004 Si01 127.4(2) . . ?
C00A C004 Si01 112.2(2) . . ?
C006 C005 C007 118.4(3) . . ?
C006 C005 C003 118.6(3) . . ?
C007 C005 C003 123.0(3) . . ?
C00N C006 C005 121.8(3) . . ?
C00N C006 H006 119.1 . . ?
C005 C006 H006 119.1 . . ?
C00J C007 C005 118.8(3) . . ?
C00J C007 C00G 118.4(3) . . ?
C005 C007 C00G 122.8(3) . . ?
C00H C008 C00B 122.7(3) . . ?
C00H C008 H008 118.6 . . ?
C00B C008 H008 118.6 . . ?
C00C C009 C00B 120.1(3) . . ?
C00C C009 C003 116.5(3) . . ?
C00B C009 C003 123.4(3) . . ?
C00F C00A C00D 118.5(3) . . ?
C00F C00A C004 122.3(3) . . ?
C00D C00A C004 119.1(3) . . ?
C009 C00B C008 116.1(3) . . ?
C009 C00B Si02 127.6(2) . . ?
C008 C00B Si02 116.2(3) . . ?
C00E C00C C009 121.4(3) . . ?
C00E C00C H00C 119.3 . . ?
C009 C00C H00C 119.3 . . ?
C00L C00D C00A 120.6(4) . . ?
C00L C00D H00D 119.7 . . ?
C00A C00D H00D 119.7 . . ?
C00H C00E C00C 119.5(4) . . ?
C00H C00E H00E 120.2 . . ?
C00C C00E H00E 120.2 . . ?
C00A C00F C00T 120.3(4) . . ?
C00A C00F H00F 119.9 . . ?
C00T C00F H00F 119.9 . . ?
C007 C00G H00A 109.5 . . ?
C007 C00G H00B 109.5 . . ?
H00A C00G H00B 109.5 . . ?
C007 C00G H00G 109.5 . . ?
H00A C00G H00G 109.5 . . ?
H00B C00G H00G 109.5 . . ?
C00E C00H C008 120.1(3) . . ?
C00E C00H H00H 119.9 . . ?
C008 C00H H00H 119.9 . . ?
C00N C00I C00J 119.9(4) . . ?
C00N C00I H00I 120.0 . . ?
C00J C00I H00I 120.0 . . ?
C00I C00J C007 121.6(4) . . ?
C00I C00J H00J 119.2 . . ?
C007 C00J H00J 119.2 . . ?
Si01 C00K H00K 109.5 . . ?
Si01 C00K H00L 109.5 . . ?
H00K C00K H00L 109.5 . . ?
Si01 C00K H00M 109.5 . . ?
H00K C00K H00M 109.5 . . ?
H00L C00K H00M 109.5 . . ?
C00Q C00L C00D 120.5(4) . . ?
C00Q C00L H00N 119.7 . . ?
C00D C00L H00N 119.7 . . ?
Si02 C00M H00O 109.5 . . ?
Si02 C00M H00P 109.5 . . ?
H00O C00M H00P 109.5 . . ?
Si02 C00M H00Q 109.5 . . ?
H00O C00M H00Q 109.5 . . ?
H00P C00M H00Q 109.5 . . ?
C006 C00N C00I 119.5(4) . . ?
C006 C00N H00R 120.3 . . ?
C00I C00N H00R 120.3 . . ?
Si02 C00O H00S 109.5 . . ?
Si02 C00O H00T 109.5 . . ?
H00S C00O H00T 109.5 . . ?
Si02 C00O H00U 109.5 . . ?
H00S C00O H00U 109.5 . . ?
H00T C00O H00U 109.5 . . ?
Si01 C00P H00V 109.5 . . ?
Si01 C00P H00W 109.5 . . ?
H00V C00P H00W 109.5 . . ?
Si01 C00P H00X 109.5 . . ?
H00V C00P H00X 109.5 . . ?
H00W C00P H00X 109.5 . . ?
C00L C00Q C00T 120.4(4) . . ?
C00L C00Q H00Y 119.8 . . ?
C00T C00Q H00Y 119.8 . . ?
Si02 C00R H00Z 109.5 . . ?
Si02 C00R H 109.5 . . ?
H00Z C00R H 109.5 . . ?
Si02 C00R HA 109.5 . . ?
H00Z C00R HA 109.5 . . ?
H C00R HA 109.5 . . ?
Si01 C00S H00 109.5 . . ?
Si01 C00S HB 109.5 . . ?
H00 C00S HB 109.5 . . ?
Si01 C00S HC 109.5 . . ?
H00 C00S HC 109.5 . . ?
HB C00S HC 109.5 . . ?
C00Q C00T C00F 119.6(4) . . ?
C00Q C00T H0AA 120.2 . . ?
C00F C00T H0AA 120.2 . . ?
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
Si01 C00K 1.863(4) . ?
Si01 C00S 1.869(4) . ?
Si01 C00P 1.869(3) . ?
Si01 C004 1.894(3) . ?
Si02 C00O 1.851(4) . ?
Si02 C00M 1.870(3) . ?
Si02 C00R 1.871(4) . ?
Si02 C00B 1.879(4) . ?
C003 C004 1.350(4) . ?
C003 C005 1.499(4) . ?
C003 C009 1.513(4) . ?
C004 C00A 1.506(4) . ?
C005 C006 1.397(5) . ?
C005 C007 1.409(5) . ?
C006 C00N 1.373(5) . ?
C006 H006 0.9500 . ?
C007 C00J 1.385(4) . ?
C007 C00G 1.509(5) . ?
C008 C00H 1.377(5) . ?
C008 C00B 1.419(4) . ?
C008 H008 0.9500 . ?
C009 C00C 1.402(5) . ?
C009 C00B 1.413(4) . ?
C00A C00F 1.386(5) . ?
C00A C00D 1.395(5) . ?
C00C C00E 1.381(4) . ?
C00C H00C 0.9500 . ?
C00D C00L 1.382(4) . ?
C00D H00D 0.9500 . ?
C00E C00H 1.369(5) . ?
C00E H00E 0.9500 . ?
C00F C00T 1.403(5) . ?
C00F H00F 0.9500 . ?
C00G H00A 0.9800 . ?
C00G H00B 0.9800 . ?
C00G H00G 0.9800 . ?
C00H H00H 0.9500 . ?
C00I C00N 1.377(5) . ?
C00I C00J 1.379(5) . ?
C00I H00I 0.9500 . ?
C00J H00J 0.9500 . ?
C00K H00K 0.9800 . ?
C00K H00L 0.9800 . ?
C00K H00M 0.9800 . ?
C00L C00Q 1.358(7) . ?
C00L H00N 0.9500 . ?
C00M H00O 0.9800 . ?
C00M H00P 0.9800 . ?
C00M H00Q 0.9800 . ?
C00N H00R 0.9500 . ?
C00O H00S 0.9800 . ?
C00O H00T 0.9800 . ?
C00O H00U 0.9800 . ?
C00P H00V 0.9800 . ?
C00P H00W 0.9800 . ?
C00P H00X 0.9800 . ?
C00Q C00T 1.378(6) . ?
C00Q H00Y 0.9500 . ?
C00R H00Z 0.9800 . ?
C00R H 0.9800 . ?
C00R HA 0.9800 . ?
C00S H00 0.9800 . ?
C00S HB 0.9800 . ?
C00S HC 0.9800 . ?
C00T H0AA 0.9500 . ?
