#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:57:57 +0100 (mar 22 de mar de 2016) $
#$Revision: 178926 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/55/4115560.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_4115560
loop_
_publ_author_name
'John A. Ewen'
'Michael J. Elder'
'Robert L. Jones'
'Arnold L. Rheingold'
'Louise M. Liable-Sands'
'Roger D. Sommer'
_publ_section_title
;
 Chiral Ansa Metallocenes with Cp Ring-Fused to Thiophenes and Pyrroles:
 Syntheses, Crystal Structures, and Isotactic Polypropylene Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4763
_journal_page_last               4773
_journal_paper_doi               10.1021/ja004266h
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C35 H36 Cl4 S2 Si Zr'
_chemical_formula_weight         781.87
_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                96.9974(7)
_cell_angle_beta                 106.8513(5)
_cell_angle_gamma                100.2661(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7096(2)
_cell_length_b                   12.6751(2)
_cell_length_c                   12.7721(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1754.64(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16715
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.8259
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.746
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                7603
_reflns_number_total             8065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004266h_3.cif
_cod_data_source_block           hmnt12
_cod_original_cell_volume        1754.65(3)
_cod_database_code               4115560
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
Zr1 Zr 0.767727(18) 0.788535(17) 0.048031(17) 0.01498(13) Uani 1 1 d .
S1' S 0.94076(6) 0.96565(5) 0.32584(6) 0.02404(18) Uani 1 1 d .
S1 S 0.43750(6) 0.72441(6) -0.12329(5) 0.02364(18) Uani 1 1 d .
Si1 Si 0.59411(6) 0.90264(6) 0.16897(6) 0.01931(18) Uani 1 1 d .
Cl1' Cl 0.97833(6) 0.84817(6) 0.05414(6) 0.02903(19) Uani 1 1 d .
Cl1 Cl 0.71417(6) 0.61476(5) -0.07676(5) 0.02680(18) Uani 1 1 d .
Cl2 Cl 0.13870(16) 0.57649(14) 0.96484(9) 0.0849(5) Uani 1 1 d .
Cl3 Cl 0.09545(9) 0.64726(9) 0.75485(8) 0.0530(3) Uani 1 1 d .
C2' C 1.0591(2) 0.8952(2) 0.3428(2) 0.0223(5) Uani 1 1 d .
C2 C 0.4760(2) 0.6967(2) -0.2460(2) 0.0242(5) Uani 1 1 d .
C3 C 0.5818(2) 0.7642(2) -0.2446(2) 0.0204(5) Uani 1 1 d .
C3' C 1.0189(2) 0.7862(2) 0.29960(19) 0.0183(5) Uani 1 1 d .
C4' C 0.7938(2) 0.6633(2) 0.1967(2) 0.0187(5) Uani 1 1 d .
H4'A H 0.8054 0.5870 0.1848 0.022 Uiso 1 1 calc R
C4 C 0.7411(2) 0.9264(2) -0.0871(2) 0.0197(5) Uani 1 1 d .
H4A H 0.8032 0.9572 -0.1215 0.024 Uiso 1 1 calc R
C5' C 0.6791(2) 0.6933(2) 0.1776(2) 0.0205(5) Uani 1 1 d .
C5 C 0.7309(2) 0.9729(2) 0.0158(2) 0.0202(5) Uani 1 1 d .
C6 C 0.6233(2) 0.9118(2) 0.0329(2) 0.0189(5) Uani 1 1 d .
C6' C 0.6998(2) 0.8097(2) 0.21352(19) 0.0184(5) Uani 1 1 d .
C7 C 0.6376(2) 0.8386(2) -0.1403(2) 0.0196(5) Uani 1 1 d .
C7' C 0.8877(2) 0.7571(2) 0.2492(2) 0.0174(5) Uani 1 1 d .
C8' C 0.8313(2) 0.8470(2) 0.25677(18) 0.0166(4) Uani 1 1 d .
C8 C 0.5684(2) 0.8286(2) -0.0652(2) 0.0190(5) Uani 1 1 d .
C10' C 1.0992(2) 0.7066(2) 0.3083(2) 0.0202(5) Uani 1 1 d .
C10 C 0.6360(3) 0.7597(2) -0.3365(2) 0.0226(5) Uani 1 1 d .
C9 C 0.3935(3) 0.6039(3) -0.3344(3) 0.0365(7) Uani 1 1 d .
H9A H 0.4246 0.5973 -0.3978 0.055 Uiso 1 1 calc R
H9B H 0.3108 0.6175 -0.3589 0.055 Uiso 1 1 calc R
H9C H 0.3908 0.5362 -0.3046 0.055 Uiso 1 1 calc R
C9' C 1.1870(3) 0.9570(3) 0.4004(3) 0.0346(7) Uani 1 1 d .
H9'A H 1.2426 0.9072 0.4036 0.052 Uiso 1 1 calc R
H9'B H 1.1947 0.9905 0.4762 0.052 Uiso 1 1 calc R
H9'C H 1.2082 1.0140 0.3595 0.052 Uiso 1 1 calc R
C11 C 0.7570(3) 0.7430(2) -0.3130(2) 0.0293(6) Uani 1 1 d .
H11A H 0.8013 0.7374 -0.2395 0.035 Uiso 1 1 calc R
C11' C 1.1745(3) 0.7021(2) 0.2402(2) 0.0258(5) Uani 1 1 d .
H11B H 1.1745 0.7504 0.1888 0.031 Uiso 1 1 calc R
C12' C 1.2491(3) 0.6267(2) 0.2482(2) 0.0277(6) Uani 1 1 d .
H12A H 1.3001 0.6240 0.2026 0.033 Uiso 1 1 calc R
C12 C 0.8107(3) 0.7348(3) -0.3953(3) 0.0383(7) Uani 1 1 d .
H12B H 0.8914 0.7228 -0.3788 0.046 Uiso 1 1 calc R
C13' C 1.2486(3) 0.5570(2) 0.3217(2) 0.0286(6) Uani 1 1 d .
H13A H 1.2989 0.5055 0.3267 0.034 Uiso 1 1 calc R
C13 C 0.7461(3) 0.7441(3) -0.5036(3) 0.0360(7) Uani 1 1 d .
H13B H 0.7827 0.7376 -0.5607 0.043 Uiso 1 1 calc R
C14' C 1.1748(3) 0.5610(2) 0.3894(2) 0.0245(5) Uani 1 1 d .
H14A H 1.1754 0.5120 0.4401 0.029 Uiso 1 1 calc R
C14 C 0.6321(3) 0.7622(2) -0.5269(2) 0.0319(6) Uani 1 1 d .
H14B H 0.5897 0.7685 -0.6007 0.038 Uiso 1 1 calc R
C15' C 1.1003(2) 0.6353(2) 0.3844(2) 0.0232(5) Uani 1 1 d .
C15 C 0.5740(3) 0.7720(2) -0.4446(2) 0.0237(5) Uani 1 1 d .
C16 C 0.4510(3) 0.8033(3) -0.4754(2) 0.0334(7) Uani 1 1 d .
H16A H 0.4215 0.8070 -0.4110 0.050 Uiso 1 1 calc R
H16B H 0.3921 0.7485 -0.5371 0.050 Uiso 1 1 calc R
H16C H 0.4600 0.8747 -0.4981 0.050 Uiso 1 1 calc R
C16' C 1.0224(3) 0.6406(3) 0.4592(3) 0.0394(8) Uani 1 1 d .
H16D H 1.0341 0.5857 0.5067 0.059 Uiso 1 1 calc R
H16E H 0.9360 0.6263 0.4138 0.059 Uiso 1 1 calc R
H16F H 1.0462 0.7133 0.5058 0.059 Uiso 1 1 calc R
C17' C 0.5580(2) 0.6134(2) 0.1333(2) 0.0257(5) Uani 1 1 d .
H17A H 0.5375 0.5841 0.1948 0.039 Uiso 1 1 calc R
H17B H 0.5625 0.5536 0.0793 0.039 Uiso 1 1 calc R
H17C H 0.4947 0.6502 0.0968 0.039 Uiso 1 1 calc R
C17 C 0.8143(3) 1.0752(2) 0.0889(2) 0.0256(5) Uani 1 1 d .
H17D H 0.7850 1.1385 0.0637 0.038 Uiso 1 1 calc R
H17E H 0.8973 1.0792 0.0850 0.038 Uiso 1 1 calc R
H17F H 0.8152 1.0751 0.1659 0.038 Uiso 1 1 calc R
C18 C 0.4301(3) 0.8452(3) 0.1487(3) 0.0311(6) Uani 1 1 d .
H18A H 0.4184 0.8419 0.2213 0.047 Uiso 1 1 calc R
H18B H 0.4052 0.7717 0.1037 0.047 Uiso 1 1 calc R
H18C H 0.3800 0.8919 0.1104 0.047 Uiso 1 1 calc R
C18' C 0.6433(3) 1.0316(2) 0.2718(2) 0.0307(6) Uani 1 1 d .
H18D H 0.6243 1.0180 0.3395 0.046 Uiso 1 1 calc R
H18E H 0.5999 1.0855 0.2402 0.046 Uiso 1 1 calc R
H18F H 0.7317 1.0594 0.2900 0.046 Uiso 1 1 calc R
C19 C 0.0333(3) 0.6196(3) 0.8625(3) 0.0425(8) Uani 1 1 d .
H19A H 0.0135 0.6863 0.8950 0.051 Uiso 1 1 calc R
H19B H -0.0433 0.5622 0.8317 0.051 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'
S S 0.1246 0.1234 '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
Cl1 Zr1 Cl1' 99.44(3)
Cl1 Zr1 C6' 121.35(6)
Cl1' Zr1 C6' 123.46(6)
Cl1 Zr1 C6 121.34(6)
Cl1' Zr1 C6 123.11(6)
C6' Zr1 C6 68.42(8)
Cl1 Zr1 C5 131.91(6)
Cl1' Zr1 C5 89.80(6)
C6' Zr1 C5 89.70(8)
C6 Zr1 C5 33.64(8)
Cl1 Zr1 C5' 88.49(6)
Cl1' Zr1 C5' 130.75(6)
C6' Zr1 C5' 33.72(8)
C6 Zr1 C5' 91.06(8)
C5 Zr1 C5' 120.09(8)
Cl1 Zr1 C8' 134.49(6)
Cl1' Zr1 C8' 89.96(6)
C6' Zr1 C8' 33.58(8)
C6 Zr1 C8' 87.65(8)
C5 Zr1 C8' 92.16(8)
C5' Zr1 C8' 54.00(8)
Cl1 Zr1 C8 88.51(6)
Cl1' Zr1 C8 132.79(6)
C6' Zr1 C8 88.81(8)
C6 Zr1 C8 33.23(8)
C5 Zr1 C8 53.65(8)
C5' Zr1 C8 95.63(8)
C8' Zr1 C8 116.86(8)
Cl1 Zr1 C4 102.96(6)
Cl1' Zr1 C4 80.16(6)
C6' Zr1 C4 120.71(8)
C6 Zr1 C4 54.89(8)
C5 Zr1 C4 32.24(8)
C5' Zr1 C4 145.28(8)
C8' Zr1 C4 122.53(8)
C8 Zr1 C4 52.82(8)
Cl1 Zr1 C4' 81.71(6)
Cl1' Zr1 C4' 100.65(6)
C6' Zr1 C4' 54.82(8)
C6 Zr1 C4' 121.47(8)
C5 Zr1 C4' 142.88(8)
C5' Zr1 C4' 32.20(8)
C8' Zr1 C4' 52.78(8)
C8 Zr1 C4' 126.56(8)
C4 Zr1 C4' 175.11(8)
Cl1 Zr1 C7' 106.82(6)
Cl1' Zr1 C7' 78.84(5)
C6' Zr1 C7' 54.28(8)
C6 Zr1 C7' 118.61(8)
C5 Zr1 C7' 121.27(8)
C5' Zr1 C7' 52.61(8)
C8' Zr1 C7' 31.66(7)
C8 Zr1 C7' 142.94(8)
C4 Zr1 C7' 145.85(8)
C4' Zr1 C7' 31.01(7)
Cl1 Zr1 C7 79.27(6)
Cl1' Zr1 C7 104.06(6)
C6' Zr1 C7 119.60(8)
C6 Zr1 C7 54.35(8)
C5 Zr1 C7 52.79(8)
C5' Zr1 C7 125.13(8)
C8' Zr1 C7 141.28(8)
C8 Zr1 C7 31.71(8)
C4 Zr1 C7 31.34(8)
C4' Zr1 C7 150.88(8)
C7' Zr1 C7 172.90(8)
C8' S1' C2' 91.44(12)
C8 S1 C2 91.14(12)
C18' Si1 C18 107.93(15)
C18' Si1 C6' 110.13(13)
C18 Si1 C6' 115.26(13)
C18' Si1 C6 115.91(12)
C18 Si1 C6 111.83(12)
C6' Si1 C6 95.64(11)
C3' C2' C9' 127.8(3)
C3' C2' S1' 113.53(19)
C9' C2' S1' 118.7(2)
C3 C2 C9 129.0(3)
C3 C2 S1 113.5(2)
C9 C2 S1 117.5(2)
C2 C3 C7 111.2(2)
C2 C3 C10 125.2(2)
C7 C3 C10 123.6(2)
C2' C3' C7' 111.2(2)
C2' C3' C10' 124.6(2)
C7' C3' C10' 124.2(2)
C7' C4' C5' 108.4(2)
C7' C4' Zr1 76.75(14)
C5' C4' Zr1 70.27(14)
C5 C4 C7 108.3(2)
C5 C4 Zr1 70.54(14)
C7 C4 Zr1 76.96(14)
C4' C5' C6' 109.3(2)
C4' C5' C17' 123.9(2)
C6' C5' C17' 126.7(2)
C4' C5' Zr1 77.53(14)
C6' C5' Zr1 71.42(14)
C17' C5' Zr1 120.26(17)
C4 C5 C6 109.7(2)
C4 C5 C17 124.0(2)
C6 C5 C17 126.1(2)
C4 C5 Zr1 77.22(15)
C6 C5 Zr1 72.10(14)
C17 C5 Zr1 121.34(18)
C8 C6 C5 104.5(2)
C8 C6 Si1 124.02(18)
C5 C6 Si1 127.40(18)
C8 C6 Zr1 75.50(14)
C5 C6 Zr1 74.27(14)
Si1 C6 Zr1 97.65(10)
C8' C6' C5' 104.7(2)
C8' C6' Si1 123.03(18)
C5' C6' Si1 128.63(18)
C8' C6' Zr1 75.48(13)
C5' C6' Zr1 74.86(13)
Si1 C6' Zr1 98.27(10)
C4 C7 C8 106.6(2)
C4 C7 C3 139.7(2)
C8 C7 C3 113.6(2)
C4 C7 Zr1 71.70(14)
C8 C7 Zr1 69.23(13)
C3 C7 Zr1 125.13(17)
C4' C7' C8' 107.4(2)
C4' C7' C3' 139.1(2)
C8' C7' C3' 113.4(2)
C4' C7' Zr1 72.24(13)
C8' C7' Zr1 68.87(13)
C3' C7' Zr1 124.81(16)
C7' C8' C6' 110.0(2)
C7' C8' S1' 110.44(17)
C6' C8' S1' 139.3(2)
C7' C8' Zr1 79.48(14)
C6' C8' Zr1 70.93(13)
S1' C8' Zr1 121.67(11)
C7 C8 C6 110.8(2)
C7 C8 S1 110.48(19)
C6 C8 S1 138.6(2)
C7 C8 Zr1 79.06(14)
C6 C8 Zr1 71.27(14)
S1 C8 Zr1 120.44(12)
C15' C10' C11' 119.5(2)
C15' C10' C3' 120.3(2)
C11' C10' C3' 120.3(2)
C15 C10 C11 118.6(2)
C15 C10 C3 123.3(2)
C11 C10 C3 118.1(2)
C12 C11 C10 120.9(3)
C12' C11' C10' 120.1(3)
C13' C12' C11' 119.9(3)
C11 C12 C13 119.7(3)
C12' C13' C14' 120.4(3)
C14 C13 C12 120.2(3)
C15' C14' C13' 121.3(3)
C13 C14 C15 121.8(3)
C14' C15' C10' 118.8(3)
C14' C15' C16' 121.1(3)
C10' C15' C16' 120.1(3)
C10 C15 C14 118.7(3)
C10 C15 C16 123.0(2)
C14 C15 C16 118.2(3)
Cl2 C19 Cl3 109.5(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zr1 Cl1 2.4204(6)
Zr1 Cl1' 2.4225(6)
Zr1 C6' 2.466(2)
Zr1 C6 2.483(2)
Zr1 C5 2.511(2)
Zr1 C5' 2.512(2)
Zr1 C8' 2.526(2)
Zr1 C8 2.538(2)
Zr1 C4 2.598(2)
Zr1 C4' 2.605(2)
Zr1 C7' 2.663(2)
Zr1 C7 2.665(2)
S1' C8' 1.737(2)
S1' C2' 1.754(3)
S1 C8 1.739(3)
S1 C2 1.765(3)
Si1 C18' 1.852(3)
Si1 C18 1.858(3)
Si1 C6' 1.876(3)
Si1 C6 1.879(3)
Cl2 C19 1.735(4)
Cl3 C19 1.775(4)
C2' C3' 1.366(4)
C2' C9' 1.484(4)
C2 C3 1.368(4)
C2 C9 1.494(4)
C3 C7 1.435(3)
C3 C10 1.488(4)
C3' C7' 1.441(3)
C3' C10' 1.489(3)
C4' C7' 1.409(3)
C4' C5' 1.422(4)
C4 C5 1.421(3)
C4 C7 1.423(4)
C5' C6' 1.444(3)
C5' C17' 1.497(4)
C5 C6 1.445(3)
C5 C17 1.494(4)
C6 C8 1.437(3)
C6' C8' 1.444(3)
C7 C8 1.427(3)
C7' C8' 1.422(3)
C10' C15' 1.404(3)
C10' C11' 1.410(4)
C10 C15 1.404(4)
C10 C11 1.420(4)
C11 C12 1.376(4)
C11' C12' 1.400(4)
C12' C13' 1.366(4)
C12 C13 1.401(5)
C13' C14' 1.391(4)
C13 C14 1.348(5)
C14' C15' 1.388(4)
C14 C15 1.413(4)
C15' C16' 1.504(4)
C15 C16 1.516(4)
