#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:03:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180024 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/18/7031818.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_7031818
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            'C38 H26 Cl2 Zr'
_chemical_formula_weight         644.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2021(9)
_cell_length_b                   9.6547(8)
_cell_length_c                   30.541(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3008.2(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            19014
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.527
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0623
_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)+(0.0388P)²+18.5417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                2572
_reflns_number_total             3661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01583e1.cif
_cod_data_source_block           jgmm015_0m_Compound_9b
_cod_depositor_comments
'Adding full bibliography for 7031816--7031825.cif.'
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7031818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Zr1 Zr 0.67303(6) 0.2500 0.37844(2) 0.02125(18) Uani 1 2 d S
Cl1 Cl 0.73323(12) 0.05359(18) 0.33425(4) 0.0417(4) Uani 1 1 d .
C1 C 0.4970(6) 0.2500 0.5094(2) 0.0207(14) Uani 1 2 d S
C2 C 0.5492(6) 0.2500 0.4697(2) 0.0217(14) Uani 1 2 d S
C3 C 0.6936(6) 0.2500 0.4584(2) 0.0221(14) Uani 1 2 d S
C4 C 0.7617(4) 0.1298(6) 0.44382(14) 0.0234(10) Uani 1 1 d .
H4A H 0.7417 0.0324 0.4527 0.028 Uiso 1 1 calc R
C5 C 0.8810(4) 0.1763(6) 0.42343(15) 0.0299(12) Uani 1 1 d .
C6 C 0.9866(5) 0.1024(8) 0.40399(17) 0.0413(15) Uani 1 1 d .
H6A H 0.9868 0.0040 0.4034 0.050 Uiso 1 1 calc R
C7 C 1.0873(5) 0.1758(7) 0.38619(18) 0.0463(17) Uani 1 1 d .
H7A H 1.1591 0.1276 0.3735 0.056 Uiso 1 1 calc R
C8 C 0.4811(6) 0.2500 0.4265(2) 0.0212(14) Uani 1 2 d S
C9 C 0.4687(4) 0.1294(6) 0.39977(14) 0.0224(10) Uani 1 1 d .
H9A H 0.4624 0.0319 0.4106 0.027 Uiso 1 1 calc R
C10 C 0.4350(4) 0.1765(5) 0.35602(15) 0.0232(10) Uani 1 1 d .
C11 C 0.4069(4) 0.1030(6) 0.31719(16) 0.0297(12) Uani 1 1 d .
H11A H 0.4081 0.0046 0.3168 0.036 Uiso 1 1 calc R
C12 C 0.3781(5) 0.1761(6) 0.28031(16) 0.0322(13) Uani 1 1 d .
H12A H 0.3576 0.1278 0.2541 0.039 Uiso 1 1 calc R
C13 C 0.5656(6) 0.2500 0.5524(2) 0.0226(14) Uani 1 2 d S
C14 C 0.6996(6) 0.2500 0.5622(2) 0.0319(18) Uani 1 2 d S
H14A H 0.7636 0.2500 0.5396 0.038 Uiso 1 2 calc SR
C15 C 0.7360(7) 0.2500 0.6061(2) 0.0368(19) Uani 1 2 d S
H15A H 0.8265 0.2500 0.6135 0.044 Uiso 1 2 calc SR
C16 C 0.6440(7) 0.2500 0.6394(2) 0.0347(18) Uani 1 2 d S
H16A H 0.6720 0.2500 0.6690 0.042 Uiso 1 2 calc SR
C17 C 0.5109(7) 0.2500 0.6297(2) 0.0295(17) Uani 1 2 d S
H17A H 0.4472 0.2500 0.6524 0.035 Uiso 1 2 calc SR
C18 C 0.4736(6) 0.2500 0.5861(2) 0.0202(14) Uani 1 2 d S
C19 C 0.3414(7) 0.2500 0.5663(2) 0.0245(15) Uani 1 2 d S
C20 C 0.2185(7) 0.2500 0.5855(2) 0.0331(18) Uani 1 2 d S
H20A H 0.2091 0.2500 0.6164 0.040 Uiso 1 2 calc SR
C21 C 0.1099(7) 0.2500 0.5586(3) 0.043(2) Uani 1 2 d S
H21A H 0.0250 0.2500 0.5713 0.052 Uiso 1 2 calc SR
C22 C 0.1220(7) 0.2500 0.5136(3) 0.044(2) Uani 1 2 d S
H22A H 0.0454 0.2500 0.4959 0.053 Uiso 1 2 calc SR
C23 C 0.2444(7) 0.2500 0.4938(2) 0.0341(19) Uani 1 2 d S
H23A H 0.2524 0.2500 0.4629 0.041 Uiso 1 2 calc SR
C24 C 0.3550(6) 0.2500 0.5203(2) 0.0221(14) Uani 1 2 d S
C25 C 0.9915(6) 0.1798(8) 0.6932(2) 0.070(3) Uani 1 1 d D
H25A H 1.0500 0.1305 0.6747 0.084 Uiso 1 1 calc R
C26 C 0.9071(7) 0.1096(7) 0.7198(3) 0.082(3) Uani 1 1 d D
H26A H 0.9063 0.0112 0.7202 0.098 Uiso 1 1 calc R
C27 C 0.8241(7) 0.1828(8) 0.7459(2) 0.079(3) Uani 1 1 d D
H27A H 0.7649 0.1346 0.7644 0.095 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
Cl1 Zr1 Cl1 103.96(8) 7_565 .
Cl1 Zr1 C8 122.71(6) 7_565 .
Cl1 Zr1 C8 122.71(7) . .
Cl1 Zr1 C3 122.46(6) 7_565 .
Cl1 Zr1 C3 122.46(6) . .
C8 Zr1 C3 58.1(2) . .
Cl1 Zr1 C9 89.53(12) 7_565 7_565
Cl1 Zr1 C9 137.14(12) . 7_565
C8 Zr1 C9 33.72(13) . 7_565
C3 Zr1 C9 79.05(16) . 7_565
Cl1 Zr1 C9 137.14(12) 7_565 .
Cl1 Zr1 C9 89.53(12) . .
C8 Zr1 C9 33.72(13) . .
C3 Zr1 C9 79.05(16) . .
C9 Zr1 C9 56.1(2) 7_565 .
Cl1 Zr1 C4 136.62(12) 7_565 .
Cl1 Zr1 C4 89.41(12) . .
C8 Zr1 C4 78.99(16) . .
C3 Zr1 C4 33.55(13) . .
C9 Zr1 C4 108.39(15) 7_565 .
C9 Zr1 C4 82.84(15) . .
Cl1 Zr1 C4 89.41(12) 7_565 7_565
Cl1 Zr1 C4 136.62(12) . 7_565
C8 Zr1 C4 78.99(16) . 7_565
C3 Zr1 C4 33.55(13) . 7_565
C9 Zr1 C4 82.84(15) 7_565 7_565
C9 Zr1 C4 108.39(15) . 7_565
C4 Zr1 C4 55.8(2) . 7_565
Cl1 Zr1 C10 82.92(11) 7_565 7_565
Cl1 Zr1 C10 107.65(11) . 7_565
C8 Zr1 C10 54.22(16) . 7_565
C3 Zr1 C10 109.85(17) . 7_565
C9 Zr1 C10 32.96(14) 7_565 7_565
C9 Zr1 C10 54.24(15) . 7_565
C4 Zr1 C10 132.44(14) . 7_565
C4 Zr1 C10 114.94(15) 7_565 7_565
Cl1 Zr1 C10 107.65(11) 7_565 .
Cl1 Zr1 C10 82.92(11) . .
C8 Zr1 C10 54.22(16) . .
C3 Zr1 C10 109.85(17) . .
C9 Zr1 C10 54.24(16) 7_565 .
C9 Zr1 C10 32.96(14) . .
C4 Zr1 C10 114.94(15) . .
C4 Zr1 C10 132.44(14) 7_565 .
C10 Zr1 C10 31.4(2) 7_565 .
Cl1 Zr1 C5 82.74(12) 7_565 7_565
Cl1 Zr1 C5 107.49(12) . 7_565
C8 Zr1 C5 109.43(17) . 7_565
C3 Zr1 C5 53.81(17) . 7_565
C9 Zr1 C5 114.55(16) 7_565 7_565
C9 Zr1 C5 132.10(15) . 7_565
C4 Zr1 C5 53.90(16) . 7_565
C4 Zr1 C5 32.58(14) 7_565 7_565
C10 Zr1 C5 144.29(16) 7_565 7_565
C10 Zr1 C5 163.47(14) . 7_565
Cl1 Zr1 C5 107.49(12) 7_565 .
Cl1 Zr1 C5 82.74(12) . .
C8 Zr1 C5 109.43(17) . .
C3 Zr1 C5 53.81(17) . .
C9 Zr1 C5 132.10(15) 7_565 .
C9 Zr1 C5 114.55(16) . .
C4 Zr1 C5 32.58(14) . .
C4 Zr1 C5 53.90(16) 7_565 .
C10 Zr1 C5 163.47(14) 7_565 .
C10 Zr1 C5 144.29(16) . .
C5 Zr1 C5 31.4(3) 7_565 .
C2 C1 C24 126.6(6) . .
C2 C1 C13 128.3(6) . .
C24 C1 C13 105.1(5) . .
C1 C2 C8 128.5(6) . .
C1 C2 C3 126.9(6) . .
C8 C2 C3 104.5(5) . .
C4 C3 C4 109.2(6) 7_565 .
C4 C3 C2 123.1(3) 7_565 .
C4 C3 C2 123.1(3) . .
C4 C3 Zr1 74.4(3) 7_565 .
C4 C3 Zr1 74.4(3) . .
C2 C3 Zr1 98.3(4) . .
C3 C4 C5 107.1(5) . .
C3 C4 Zr1 72.1(3) . .
C5 C4 Zr1 79.3(3) . .
C5 C5 C6 120.1(4) 7_565 .
C5 C5 C4 108.2(3) 7_565 .
C6 C5 C4 131.7(6) . .
C5 C5 Zr1 74.28(12) 7_565 .
C6 C5 Zr1 122.0(3) . .
C4 C5 Zr1 68.1(2) . .
C7 C6 C5 118.5(6) . .
C6 C7 C7 121.4(4) . 7_565
C9 C8 C9 109.2(6) . 7_565
C9 C8 C2 123.2(3) . .
C9 C8 C2 123.2(3) 7_565 .
C9 C8 Zr1 74.2(3) . .
C9 C8 Zr1 74.2(3) 7_565 .
C2 C8 Zr1 99.1(4) . .
C8 C9 C10 107.0(4) . .
C8 C9 Zr1 72.1(3) . .
C10 C9 Zr1 79.1(3) . .
C10 C10 C11 120.2(3) 7_565 .
C10 C10 C9 108.2(3) 7_565 .
C11 C10 C9 131.6(5) . .
C10 C10 Zr1 74.30(11) 7_565 .
C11 C10 Zr1 122.9(3) . .
C9 C10 Zr1 68.0(2) . .
C12 C11 C10 118.6(5) . .
C11 C12 C12 121.2(3) . 7_565
C18 C13 C14 120.0(6) . .
C18 C13 C1 109.6(6) . .
C14 C13 C1 130.4(6) . .
C15 C14 C13 117.8(7) . .
C16 C15 C14 121.8(7) . .
C15 C16 C17 120.5(7) . .
C18 C17 C16 118.2(7) . .
C17 C18 C13 121.7(6) . .
C17 C18 C19 130.1(6) . .
C13 C18 C19 108.2(5) . .
C20 C19 C24 120.7(6) . .
C20 C19 C18 130.8(6) . .
C24 C19 C18 108.5(6) . .
C19 C20 C21 118.4(7) . .
C22 C21 C20 121.4(7) . .
C21 C22 C23 121.0(7) . .
C22 C23 C24 118.5(7) . .
C23 C24 C19 120.0(6) . .
C23 C24 C1 131.4(6) . .
C19 C24 C1 108.6(6) . .
C26 C25 C25 119.8(5) . 7_565
C25 C26 C27 118.9(7) . .
C26 C27 C27 121.3(5) . 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 Cl1 2.4071(15) 7_565
Zr1 Cl1 2.4071(15) .
Zr1 C8 2.448(6) .
Zr1 C3 2.451(6) .
Zr1 C9 2.475(4) 7_565
Zr1 C9 2.475(4) .
Zr1 C4 2.480(5) .
Zr1 C4 2.480(5) 7_565
Zr1 C10 2.621(4) 7_565
Zr1 C10 2.621(4) .
Zr1 C5 2.626(5) 7_565
Zr1 C5 2.626(5) .
C1 C2 1.324(9) .
C1 C24 1.487(8) .
C1 C13 1.487(9) .
C2 C8 1.492(9) .
C2 C3 1.514(8) .
C3 C4 1.424(6) 7_565
C3 C4 1.424(6) .
C4 C5 1.439(6) .
C5 C5 1.423(12) 7_565
C5 C6 1.422(7) .
C6 C7 1.362(8) .
C7 C7 1.433(14) 7_565
C8 C9 1.428(6) .
C8 C9 1.428(6) 7_565
C9 C10 1.452(6) .
C10 C10 1.419(10) 7_565
C10 C11 1.412(7) .
C11 C12 1.361(7) .
C12 C12 1.427(11) 7_565
C13 C18 1.393(9) .
C13 C14 1.399(9) .
C14 C15 1.393(10) .
C15 C16 1.382(10) .
C16 C17 1.390(10) .
C17 C18 1.385(9) .
C18 C19 1.478(9) .
C19 C20 1.384(9) .
C19 C24 1.410(9) .
C20 C21 1.379(10) .
C21 C22 1.378(11) .
C22 C23 1.387(10) .
C23 C24 1.388(9) .
C25 C26 1.365(8) .
C25 C25 1.355(16) 7_565
C26 C27 1.360(8) .
C27 C27 1.297(16) 7_565
