#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:54:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178796 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/50/4105074.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_4105074
loop_
_publ_author_name
'Xiaofang Li'
'Masayoshi Nishiura'
'Lihong Hu'
'Kyouichi Mori'
'Zhaomin Hou'
_publ_section_title
;
 Alternating and Random Copolymerization of Isoprene and Ethylene
 Catalyzed by Cationic Half-Sandwich Scandium Alkyls
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13870
_journal_page_last               13882
_journal_paper_doi               10.1021/ja9056213
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C18 H37 O Sc Si2'
_chemical_formula_weight         370.62
_chemical_name_common            (MeC5H4)Sc(CH2SiMe3)2(thf)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.6570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6699(8)
_cell_length_b                   10.8800(9)
_cell_length_c                   21.3864(17)
_cell_measurement_temperature    173(2)
_cell_volume                     2242.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13680
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0580P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                4023
_reflns_number_total             5096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9056213_si_001_2.cif
_cod_data_source_block           2
_cod_database_code               4105074
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sc1 Sc 0.43841(3) 0.16962(3) 0.141023(14) 0.02578(10) Uani 1 1 d .
Si1 Si 0.28968(5) 0.34257(4) 0.00359(2) 0.03121(13) Uani 1 1 d .
Si2 Si 0.81429(5) 0.14427(5) 0.16226(2) 0.03247(13) Uani 1 1 d .
O1 O 0.32470(11) 0.00554(10) 0.11651(5) 0.0313(3) Uani 1 1 d .
C1 C 0.43089(18) 0.26035(16) 0.04866(8) 0.0331(4) Uani 1 1 d .
H1A H 0.5070 0.3187 0.0524 0.040 Uiso 1 1 calc R
H1B H 0.4587 0.1970 0.0203 0.040 Uiso 1 1 calc R
C2 C 0.2509(2) 0.49110(19) 0.04131(10) 0.0548(6) Uani 1 1 d .
H2A H 0.2174 0.4757 0.0816 0.082 Uiso 1 1 calc R
H2B H 0.1814 0.5345 0.0154 0.082 Uiso 1 1 calc R
H2C H 0.3338 0.5398 0.0464 0.082 Uiso 1 1 calc R
C3 C 0.1246(2) 0.2532(2) -0.00404(12) 0.0577(6) Uani 1 1 d .
H3A H 0.1364 0.1815 -0.0292 0.087 Uiso 1 1 calc R
H3B H 0.0518 0.3034 -0.0237 0.087 Uiso 1 1 calc R
H3C H 0.1006 0.2287 0.0368 0.087 Uiso 1 1 calc R
C4 C 0.3308(3) 0.3788(2) -0.07812(10) 0.0603(6) Uani 1 1 d .
H4A H 0.4126 0.4291 -0.0769 0.091 Uiso 1 1 calc R
H4B H 0.2544 0.4221 -0.0994 0.091 Uiso 1 1 calc R
H4C H 0.3468 0.3038 -0.1001 0.091 Uiso 1 1 calc R
C5 C 0.64154(17) 0.07448(17) 0.14879(8) 0.0355(4) Uani 1 1 d .
H5A H 0.6359 0.0147 0.1822 0.043 Uiso 1 1 calc R
H5B H 0.6440 0.0274 0.1104 0.043 Uiso 1 1 calc R
C6 C 0.95096(18) 0.0508(2) 0.12685(9) 0.0444(5) Uani 1 1 d .
H6A H 0.9558 -0.0292 0.1458 0.067 Uiso 1 1 calc R
H6B H 1.0391 0.0911 0.1341 0.067 Uiso 1 1 calc R
H6C H 0.9279 0.0427 0.0825 0.067 Uiso 1 1 calc R
C7 C 0.8685(2) 0.1599(2) 0.24758(9) 0.0548(6) Uani 1 1 d .
H7A H 0.8069 0.2155 0.2664 0.082 Uiso 1 1 calc R
H7B H 0.9614 0.1914 0.2528 0.082 Uiso 1 1 calc R
H7C H 0.8651 0.0809 0.2674 0.082 Uiso 1 1 calc R
C8 C 0.8187(2) 0.30109(19) 0.12733(10) 0.0474(5) Uani 1 1 d .
H8A H 0.7955 0.2961 0.0829 0.071 Uiso 1 1 calc R
H8B H 0.9100 0.3352 0.1352 0.071 Uiso 1 1 calc R
H8C H 0.7528 0.3528 0.1459 0.071 Uiso 1 1 calc R
C9 C 0.42249(19) 0.19192(18) 0.25729(8) 0.0362(4) Uani 1 1 d .
C10 C 0.48540(19) 0.29905(17) 0.23650(8) 0.0379(4) Uani 1 1 d .
H10 H 0.5761 0.3238 0.2477 0.046 Uiso 1 1 calc R
C11 C 0.3889(2) 0.36275(18) 0.19599(9) 0.0400(4) Uani 1 1 d .
H11 H 0.4040 0.4369 0.1760 0.048 Uiso 1 1 calc R
C12 C 0.26586(19) 0.29447(18) 0.19118(8) 0.0389(4) Uani 1 1 d .
H12 H 0.1846 0.3149 0.1672 0.047 Uiso 1 1 calc R
C13 C 0.28658(18) 0.18997(18) 0.22889(8) 0.0366(4) Uani 1 1 d .
H13 H 0.2210 0.1292 0.2342 0.044 Uiso 1 1 calc R
C14 C 0.4857(2) 0.0994(2) 0.30294(9) 0.0534(6) Uani 1 1 d .
H14A H 0.4784 0.1282 0.3450 0.080 Uiso 1 1 calc R
H14B H 0.5817 0.0881 0.2960 0.080 Uiso 1 1 calc R
H14C H 0.4376 0.0225 0.2971 0.080 Uiso 1 1 calc R
C15 C 0.3010(3) -0.04021(19) 0.05297(9) 0.0539(6) Uani 1 1 d .
H15A H 0.3855 -0.0350 0.0316 0.065 Uiso 1 1 calc R
H15B H 0.2296 0.0079 0.0297 0.065 Uiso 1 1 calc R
C16 C 0.2568(3) -0.1682(2) 0.05740(11) 0.0560(6) Uani 1 1 d .
H16A H 0.2943 -0.2178 0.0251 0.067 Uiso 1 1 calc R
H16B H 0.1564 -0.1745 0.0532 0.067 Uiso 1 1 calc R
C17 C 0.3135(3) -0.2083(2) 0.12087(11) 0.0788(9) Uani 1 1 d .
H17A H 0.2553 -0.2714 0.1371 0.095 Uiso 1 1 calc R
H17B H 0.4067 -0.2406 0.1195 0.095 Uiso 1 1 calc R
C18 C 0.3143(2) -0.09755(17) 0.16002(8) 0.0404(4) Uani 1 1 d .
H18A H 0.2297 -0.0920 0.1813 0.048 Uiso 1 1 calc R
H18B H 0.3930 -0.0983 0.1912 0.048 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'
O O 0.0106 0.0060 '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'
Sc Sc 0.2519 0.3716 '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
O1 Sc1 C1 100.09(6)
O1 Sc1 C5 93.64(6)
C1 Sc1 C5 103.95(7)
O1 Sc1 C12 102.36(6)
C1 Sc1 C12 99.73(6)
C5 Sc1 C12 148.53(6)
O1 Sc1 C11 135.22(6)
C1 Sc1 C11 92.97(7)
C5 Sc1 C11 124.49(7)
C12 Sc1 C11 32.93(6)
O1 Sc1 C13 86.35(5)
C1 Sc1 C13 131.21(6)
C5 Sc1 C13 124.02(6)
C12 Sc1 C13 32.83(6)
C11 Sc1 C13 54.29(6)
O1 Sc1 C10 136.75(5)
C1 Sc1 C10 118.16(7)
C5 Sc1 C10 95.80(6)
C12 Sc1 C10 54.30(6)
C11 Sc1 C10 32.84(6)
C13 Sc1 C10 53.84(6)
O1 Sc1 C9 104.55(5)
C1 Sc1 C9 147.40(6)
C5 Sc1 C9 95.51(6)
C12 Sc1 C9 54.45(6)
C11 Sc1 C9 54.45(6)
C13 Sc1 C9 32.56(6)
C10 Sc1 C9 32.56(6)
C1 Si1 C2 111.29(9)
C1 Si1 C3 112.71(9)
C2 Si1 C3 106.87(11)
C1 Si1 C4 112.82(9)
C2 Si1 C4 106.80(11)
C3 Si1 C4 105.93(12)
C5 Si2 C8 111.44(9)
C5 Si2 C7 111.78(9)
C8 Si2 C7 107.14(11)
C5 Si2 C6 111.99(9)
C8 Si2 C6 107.14(10)
C7 Si2 C6 107.06(9)
C15 O1 C18 108.59(13)
C15 O1 Sc1 123.78(11)
C18 O1 Sc1 122.89(10)
Si1 C1 Sc1 131.05(9)
Si2 C5 Sc1 127.48(10)
C13 C9 C10 106.88(17)
C13 C9 C14 126.20(18)
C10 C9 C14 126.89(18)
C13 C9 Sc1 72.59(10)
C10 C9 Sc1 72.78(10)
C14 C9 Sc1 121.66(13)
C9 C10 C11 108.78(17)
C9 C10 Sc1 74.66(10)
C11 C10 Sc1 72.87(10)
C12 C11 C10 107.57(18)
C12 C11 Sc1 73.16(10)
C10 C11 Sc1 74.29(10)
C13 C12 C11 107.94(17)
C13 C12 Sc1 74.49(10)
C11 C12 Sc1 73.91(10)
C12 C13 C9 108.83(17)
C12 C13 Sc1 72.69(10)
C9 C13 Sc1 74.85(10)
O1 C15 C16 106.96(16)
C15 C16 C17 104.49(18)
C18 C17 C16 105.36(19)
O1 C18 C17 105.28(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sc1 O1 2.1394(12)
Sc1 C1 2.2041(17)
Sc1 C5 2.2146(17)
Sc1 C12 2.4638(17)
Sc1 C11 2.4734(18)
Sc1 C13 2.4867(17)
Sc1 C10 2.4915(17)
Sc1 C9 2.5154(17)
Si1 C1 1.8386(17)
Si1 C2 1.858(2)
Si1 C3 1.865(2)
Si1 C4 1.866(2)
Si2 C5 1.8363(17)
Si2 C8 1.864(2)
Si2 C7 1.865(2)
Si2 C6 1.8752(19)
O1 C15 1.448(2)
O1 C18 1.466(2)
C9 C13 1.402(2)
C9 C10 1.404(3)
C9 C14 1.498(3)
C10 C11 1.404(3)
C11 C12 1.399(3)
C12 C13 1.399(3)
C15 C16 1.462(3)
C16 C17 1.487(3)
C17 C18 1.467(3)
