#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:03:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180024 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/18/7031816.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_7031816
loop_
_publ_author_name
'Morton, Jason G. M.'
'Al-Shammari, Haif'
'Sun, Yunshan'
'Zhu, Jiangtao'
'Stephan, Douglas W.'
_publ_section_title
;
 1,1-Olefin-bridged bis-(2-indenyl) metallocenes of titanium and
 zirconium.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13219
_journal_page_last               13231
_journal_paper_doi               10.1039/c4dt01583e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C44 H50 Si2'
_chemical_formula_weight         635.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.273(6)
_cell_angle_beta                 93.615(7)
_cell_angle_gamma                92.848(6)
_cell_formula_units_Z            2
_cell_length_a                   8.3973(11)
_cell_length_b                   12.1375(14)
_cell_length_c                   18.422(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1819.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42063
_diffrn_reflns_theta_full        31.12
_diffrn_reflns_theta_max         31.12
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.9738
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         11574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0504P)²+0.5099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                8550
_reflns_number_total             11574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01583e1.cif
_cod_data_source_block           jgmm023_0m
_cod_depositor_comments
'Adding full bibliography for 7031816--7031825.cif.'
_cod_original_cell_volume        1819.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031816
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.42233(4) 0.79742(3) 0.12797(2) 0.01983(8) Uani 1 1 d .
Si2 Si -0.08201(4) 0.50349(3) 0.311867(19) 0.01841(8) Uani 1 1 d .
C1 C 0.19432(14) 0.78932(10) 0.31829(7) 0.0165(2) Uani 1 1 d .
C2 C 0.18444(14) 0.69958(10) 0.25692(7) 0.0166(2) Uani 1 1 d .
C3 C 0.13975(15) 0.71437(10) 0.18123(7) 0.0175(2) Uani 1 1 d .
C4 C 0.03948(16) 0.64199(11) 0.12888(7) 0.0212(3) Uani 1 1 d .
H15A H -0.0058 0.5712 0.1341 0.025 Uiso 1 1 calc R
C5 C 0.01185(16) 0.68874(11) 0.06400(7) 0.0216(3) Uani 1 1 d .
C6 C -0.08490(18) 0.64827(13) -0.00232(8) 0.0293(3) Uani 1 1 d .
H39A H -0.1432 0.5767 -0.0117 0.035 Uiso 1 1 calc R
C7 C -0.09385(19) 0.71477(14) -0.05410(8) 0.0330(3) Uani 1 1 d .
H38A H -0.1583 0.6881 -0.0997 0.040 Uiso 1 1 calc R
C8 C -0.00989(18) 0.81998(14) -0.04038(8) 0.0306(3) Uani 1 1 d .
H32A H -0.0200 0.8650 -0.0762 0.037 Uiso 1 1 calc R
C9 C 0.08863(16) 0.86046(12) 0.02483(7) 0.0242(3) Uani 1 1 d .
H29A H 0.1465 0.9322 0.0337 0.029 Uiso 1 1 calc R
C10 C 0.10076(15) 0.79376(11) 0.07686(7) 0.0193(2) Uani 1 1 d .
C11 C 0.20175(15) 0.81079(11) 0.14922(7) 0.0175(2) Uani 1 1 d .
H8A H 0.1860 0.8859 0.1831 0.021 Uiso 1 1 calc R
C12 C 0.21373(14) 0.58351(10) 0.26433(7) 0.0175(2) Uani 1 1 d .
C13 C 0.29764(15) 0.50808(11) 0.21849(7) 0.0200(2) Uani 1 1 d .
H13A H 0.3427 0.5207 0.1748 0.024 Uiso 1 1 calc R
C14 C 0.30899(15) 0.40542(11) 0.24535(7) 0.0206(2) Uani 1 1 d .
C15 C 0.38613(17) 0.30609(12) 0.21822(8) 0.0266(3) Uani 1 1 d .
H37A H 0.4423 0.2974 0.1743 0.032 Uiso 1 1 calc R
C16 C 0.37875(18) 0.22104(12) 0.25673(9) 0.0306(3) Uani 1 1 d .
H33A H 0.4294 0.1529 0.2387 0.037 Uiso 1 1 calc R
C17 C 0.29845(17) 0.23374(12) 0.32140(9) 0.0305(3) Uani 1 1 d .
H35A H 0.2955 0.1744 0.3472 0.037 Uiso 1 1 calc R
C18 C 0.22197(16) 0.33243(12) 0.34900(8) 0.0261(3) Uani 1 1 d .
H26A H 0.1681 0.3409 0.3936 0.031 Uiso 1 1 calc R
C19 C 0.22547(15) 0.41816(11) 0.31052(7) 0.0197(2) Uani 1 1 d .
C20 C 0.14756(15) 0.52932(11) 0.32344(7) 0.0179(2) Uani 1 1 d .
H10A H 0.1821 0.5766 0.3745 0.022 Uiso 1 1 calc R
C21 C 0.11202(14) 0.89618(10) 0.32680(7) 0.0172(2) Uani 1 1 d .
C22 C -0.00223(15) 0.93208(11) 0.28011(7) 0.0208(2) Uani 1 1 d .
H14A H -0.0323 0.8871 0.2313 0.025 Uiso 1 1 calc R
C23 C -0.07122(16) 1.03415(11) 0.30590(8) 0.0245(3) Uani 1 1 d .
H27A H -0.1454 1.0602 0.2735 0.029 Uiso 1 1 calc R
C24 C -0.03370(17) 1.09881(12) 0.37813(9) 0.0273(3) Uani 1 1 d .
H28A H -0.0819 1.1685 0.3946 0.033 Uiso 1 1 calc R
C25 C 0.07381(17) 1.06222(11) 0.42641(8) 0.0252(3) Uani 1 1 d .
H23A H 0.0974 1.1052 0.4763 0.030 Uiso 1 1 calc R
C26 C 0.14654(15) 0.96153(11) 0.40065(7) 0.0195(2) Uani 1 1 d .
C27 C 0.25552(15) 0.90104(11) 0.44009(7) 0.0191(2) Uani 1 1 d .
C28 C 0.32864(17) 0.93253(12) 0.51213(7) 0.0253(3) Uani 1 1 d .
H25A H 0.3072 1.0020 0.5449 0.030 Uiso 1 1 calc R
C29 C 0.43371(17) 0.86056(13) 0.53542(8) 0.0284(3) Uani 1 1 d .
H31A H 0.4820 0.8797 0.5851 0.034 Uiso 1 1 calc R
C30 C 0.46885(16) 0.76042(13) 0.48646(8) 0.0252(3) Uani 1 1 d .
H18A H 0.5435 0.7133 0.5028 0.030 Uiso 1 1 calc R
C31 C 0.39662(15) 0.72833(11) 0.41408(7) 0.0209(3) Uani 1 1 d .
H17A H 0.4232 0.6609 0.3807 0.025 Uiso 1 1 calc R
C32 C 0.28415(14) 0.79716(11) 0.39130(7) 0.0176(2) Uani 1 1 d .
C33 C 0.54326(17) 0.80245(13) 0.21769(8) 0.0273(3) Uani 1 1 d .
H19A H 0.5039 0.7392 0.2389 0.033 Uiso 1 1 calc R
H19B H 0.6560 0.7908 0.2069 0.033 Uiso 1 1 calc R
C34 C 0.53697(19) 0.91429(15) 0.27636(8) 0.0347(4) Uani 1 1 d .
H41A H 0.6024 0.9112 0.3217 0.052 Uiso 1 1 calc R
H41B H 0.4261 0.9257 0.2884 0.052 Uiso 1 1 calc R
H41C H 0.5784 0.9773 0.2564 0.052 Uiso 1 1 calc R
C35 C 0.4485(2) 0.66166(13) 0.05771(8) 0.0319(3) Uani 1 1 d .
H34A H 0.5596 0.6404 0.0654 0.038 Uiso 1 1 calc R
H34B H 0.3765 0.6014 0.0686 0.038 Uiso 1 1 calc R
C36 C 0.4169(3) 0.66221(16) -0.02460(9) 0.0476(5) Uani 1 1 d .
H44A H 0.4335 0.5871 -0.0556 0.071 Uiso 1 1 calc R
H44B H 0.4904 0.7190 -0.0372 0.071 Uiso 1 1 calc R
H44C H 0.3063 0.6809 -0.0339 0.071 Uiso 1 1 calc R
C37 C 0.48839(17) 0.92279(12) 0.09135(8) 0.0269(3) Uani 1 1 d .
H20A H 0.4370 0.9144 0.0403 0.032 Uiso 1 1 calc R
H20B H 0.4513 0.9923 0.1235 0.032 Uiso 1 1 calc R
C38 C 0.67052(19) 0.93715(16) 0.08861(10) 0.0403(4) Uani 1 1 d .
H42A H 0.6975 1.0035 0.0688 0.060 Uiso 1 1 calc R
H42B H 0.7081 0.8692 0.0561 0.060 Uiso 1 1 calc R
H42C H 0.7222 0.9479 0.1392 0.060 Uiso 1 1 calc R
C39 C -0.17816(16) 0.64019(11) 0.31472(8) 0.0242(3) Uani 1 1 d .
H22A H -0.1343 0.6754 0.2762 0.029 Uiso 1 1 calc R
H22B H -0.2943 0.6232 0.3014 0.029 Uiso 1 1 calc R
C40 C -0.15483(19) 0.72651(13) 0.39046(9) 0.0322(3) Uani 1 1 d .
H36A H -0.2089 0.7951 0.3871 0.048 Uiso 1 1 calc R
H36B H -0.0404 0.7461 0.4036 0.048 Uiso 1 1 calc R
H36C H -0.2004 0.6935 0.4290 0.048 Uiso 1 1 calc R
C41 C -0.14379(17) 0.44926(13) 0.39405(8) 0.0277(3) Uani 1 1 d .
H30A H -0.1069 0.3719 0.3895 0.033 Uiso 1 1 calc R
H30B H -0.0897 0.4984 0.4403 0.033 Uiso 1 1 calc R
C42 C -0.32514(18) 0.44524(15) 0.40141(10) 0.0367(4) Uani 1 1 d .
H43A H -0.3489 0.4159 0.4451 0.055 Uiso 1 1 calc R
H43B H -0.3797 0.3954 0.3563 0.055 Uiso 1 1 calc R
H43C H -0.3624 0.5218 0.4075 0.055 Uiso 1 1 calc R
C43 C -0.14853(18) 0.40041(12) 0.22121(8) 0.0279(3) Uani 1 1 d .
H24A H -0.2559 0.4194 0.2044 0.033 Uiso 1 1 calc R
H24B H -0.0747 0.4120 0.1834 0.033 Uiso 1 1 calc R
C44 C -0.1569(2) 0.27439(13) 0.22208(10) 0.0353(3) Uani 1 1 d .
H40A H -0.1928 0.2289 0.1720 0.053 Uiso 1 1 calc R
H40B H -0.2325 0.2605 0.2579 0.053 Uiso 1 1 calc R
H40C H -0.0507 0.2531 0.2369 0.053 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
C33 Si1 C37 108.61(7)
C33 Si1 C35 110.48(7)
C37 Si1 C35 110.46(7)
C33 Si1 C11 108.22(6)
C37 Si1 C11 107.98(6)
C35 Si1 C11 110.99(7)
C39 Si2 C41 107.70(7)
C39 Si2 C43 109.08(6)
C41 Si2 C43 111.41(7)
C39 Si2 C20 110.29(6)
C41 Si2 C20 107.15(6)
C43 Si2 C20 111.14(6)
C2 C1 C32 127.00(11)
C2 C1 C21 127.48(11)
C32 C1 C21 105.47(10)
C1 C2 C3 121.46(11)
C1 C2 C12 121.31(11)
C3 C2 C12 117.21(10)
C4 C3 C2 125.25(11)
C4 C3 C11 109.51(11)
C2 C3 C11 125.23(11)
C3 C4 C5 109.93(11)
C6 C5 C10 120.49(13)
C6 C5 C4 131.22(13)
C10 C5 C4 108.28(11)
C7 C6 C5 118.55(14)
C6 C7 C8 120.94(13)
C7 C8 C9 121.08(13)
C8 C9 C10 118.60(14)
C9 C10 C5 120.29(12)
C9 C10 C11 131.07(12)
C5 C10 C11 108.61(11)
C10 C11 C3 102.73(10)
C10 C11 Si1 108.93(8)
C3 C11 Si1 111.52(8)
C13 C12 C2 125.85(11)
C13 C12 C20 109.59(11)
C2 C12 C20 124.52(11)
C12 C13 C14 110.42(11)
C15 C14 C19 120.69(12)
C15 C14 C13 131.30(13)
C19 C14 C13 108.00(11)
C16 C15 C14 118.58(14)
C15 C16 C17 120.95(13)
C16 C17 C18 120.88(13)
C19 C18 C17 119.16(14)
C18 C19 C14 119.72(12)
C18 C19 C20 131.40(12)
C14 C19 C20 108.84(11)
C19 C20 C12 102.58(10)
C19 C20 Si2 110.37(9)
C12 C20 Si2 113.06(8)
C22 C21 C26 118.79(12)
C22 C21 C1 131.82(11)
C26 C21 C1 108.77(11)
C23 C22 C21 119.32(12)
C24 C23 C22 121.21(13)
C25 C24 C23 120.35(13)
C24 C25 C26 118.96(13)
C25 C26 C21 121.25(12)
C25 C26 C27 130.24(12)
C21 C26 C27 108.39(11)
C28 C27 C32 121.23(12)
C28 C27 C26 130.12(12)
C32 C27 C26 108.63(11)
C27 C28 C29 118.72(13)
C28 C29 C30 120.49(13)
C31 C30 C29 121.18(13)
C30 C31 C32 118.80(12)
C31 C32 C27 119.39(11)
C31 C32 C1 131.52(12)
C27 C32 C1 108.70(11)
C34 C33 Si1 113.68(10)
C36 C35 Si1 116.97(11)
C38 C37 Si1 113.30(11)
C40 C39 Si2 114.79(10)
C42 C41 Si2 113.81(10)
C44 C43 Si2 116.69(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si1 C33 1.8715(14)
Si1 C37 1.8744(14)
Si1 C35 1.8792(15)
Si1 C11 1.9242(13)
Si2 C39 1.8724(14)
Si2 C41 1.8755(14)
Si2 C43 1.8762(15)
Si2 C20 1.9281(13)
C1 C2 1.3730(17)
C1 C32 1.4810(17)
C1 C21 1.4811(17)
C2 C3 1.4742(16)
C2 C12 1.4774(17)
C3 C4 1.3586(18)
C3 C11 1.5111(17)
C4 C5 1.4470(17)
C5 C6 1.3977(18)
C5 C10 1.4082(19)
C6 C7 1.385(2)
C7 C8 1.390(2)
C8 C9 1.390(2)
C9 C10 1.3917(17)
C10 C11 1.5007(17)
C12 C13 1.3535(18)
C12 C20 1.5153(17)
C13 C14 1.4475(18)
C14 C15 1.4017(19)
C14 C19 1.4101(18)
C15 C16 1.381(2)
C16 C17 1.387(2)
C17 C18 1.394(2)
C18 C19 1.3872(18)
C19 C20 1.5049(17)
C21 C22 1.4000(17)
C21 C26 1.4128(17)
C22 C23 1.3900(19)
C23 C24 1.389(2)
C24 C25 1.387(2)
C25 C26 1.3915(19)
C26 C27 1.4602(18)
C27 C28 1.3876(18)
C27 C32 1.4115(18)
C28 C29 1.388(2)
C29 C30 1.394(2)
C30 C31 1.3905(18)
C31 C32 1.3983(17)
C33 C34 1.534(2)
C35 C36 1.524(2)
C37 C38 1.536(2)
C39 C40 1.535(2)
C41 C42 1.537(2)
C43 C44 1.532(2)
