#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/38/4063853.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_4063853
loop_
_publ_author_name
'Ransom, Paul'
'Ashley, Andrew E.'
'Brown, N. David'
'Thompson, Amber L.'
'O’Hare, Dermot'
_publ_section_title
;
 Synthesis, Characterization, and Polymerization Studies of
 Ethylenebis(hexamethylindenyl) Complexes of Zirconium and Hafnium
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              800
_journal_paper_doi               10.1021/om100986j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C32 H40 Cl2 Zr1'
_chemical_formula_sum            'C32 H40 Cl2 Zr'
_chemical_formula_weight         586.79
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-07-28
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 129.5251(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4750(5)
_cell_length_b                   8.2320(2)
_cell_length_c                   16.4480(4)
_cell_measurement_reflns_used    3186
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2660.61(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18506
_diffrn_reflns_theta_full        27.464
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         5.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3020
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000589
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 4.73P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0949
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0949
_reflns_limit_h_max              25
_reflns_limit_h_min              -32
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2238
_reflns_number_total             3021
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.92
_oxford_diffrn_Wilson_scale      151.16
_oxford_refine_ls_r_factor_ref   0.0665
_oxford_refine_ls_scale          0.08488(3)
_oxford_reflns_number_all        3020
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 5937
_cod_data_source_file            om100986j_si_002.cif
_cod_data_source_block           rac-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C32 H40 Cl2 Zr1'
_cod_database_code               4063853
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zr1 Zr 0.5000 0.88361(4) 0.7500 0.0187 1.0000 Uani S T
Cl2 Cl 0.40803(4) 0.68608(9) 0.65017(6) 0.0272 1.0000 Uani . .
C3 C 0.49855(14) 1.1301(3) 0.8351(2) 0.0214 1.0000 Uani . .
C4 C 0.43526(14) 1.0492(3) 0.7926(2) 0.0208 1.0000 Uani . .
C5 C 0.45147(13) 0.8993(3) 0.8498(2) 0.0194 1.0000 Uani . .
C6 C 0.52425(13) 0.8893(3) 0.9282(2) 0.0205 1.0000 Uani . .
C7 C 0.55191(14) 1.0314(3) 0.9202(2) 0.0225 1.0000 Uani . .
C8 C 0.62680(14) 1.0700(4) 0.9937(2) 0.0289 1.0000 Uani . .
C9 C 0.56615(15) 0.7647(4) 1.0137(2) 0.0279 1.0000 Uani . .
C10 C 0.39876(14) 0.7917(3) 0.8240(2) 0.0221 1.0000 Uani . .
C11 C 0.41729(15) 0.6365(4) 0.8865(3) 0.0312 1.0000 Uani . .
C12 C 0.33209(14) 0.8320(4) 0.7399(2) 0.0254 1.0000 Uani . .
C13 C 0.31573(14) 0.9860(4) 0.6883(2) 0.0258 1.0000 Uani . .
C14 C 0.36520(14) 1.0968(3) 0.7149(2) 0.0232 1.0000 Uani . .
C15 C 0.34568(15) 1.2681(4) 0.6723(2) 0.0321 1.0000 Uani . .
C16 C 0.24114(16) 1.0258(4) 0.6031(3) 0.0379 1.0000 Uani . .
C17 C 0.27444(16) 0.7144(4) 0.7001(3) 0.0402 1.0000 Uani . .
C18 C 0.51029(15) 1.2908(3) 0.8055(2) 0.0275 1.0000 Uani . .
H83 H 0.6458 1.0543 1.0654 0.0416 1.0000 Uiso R .
H82 H 0.6340 1.1801 0.9846 0.0414 1.0000 Uiso R .
H81 H 0.6514 1.0024 0.9803 0.0415 1.0000 Uiso R .
H91 H 0.6138 0.7809 1.0501 0.0411 1.0000 Uiso R .
H92 H 0.5583 0.7722 1.0635 0.0417 1.0000 Uiso R .
H93 H 0.5542 0.6569 0.9841 0.0412 1.0000 Uiso R .
H113 H 0.3777 0.5873 0.8714 0.0482 1.0000 Uiso R .
H112 H 0.4496 0.6577 0.9610 0.0481 1.0000 Uiso R .
H111 H 0.4380 0.5618 0.8702 0.0481 1.0000 Uiso R .
H151 H 0.3166 1.3131 0.6841 0.0480 1.0000 Uiso R .
H152 H 0.3851 1.3354 0.7060 0.0483 1.0000 Uiso R .
H153 H 0.3226 1.2678 0.5980 0.0488 1.0000 Uiso R .
H163 H 0.2330 1.1395 0.5889 0.0514 1.0000 Uiso R .
H162 H 0.2150 0.9886 0.6232 0.0514 1.0000 Uiso R .
H161 H 0.2236 0.9722 0.5389 0.0510 1.0000 Uiso R .
H173 H 0.2437 0.7132 0.6241 0.0561 1.0000 Uiso R .
H172 H 0.2491 0.7486 0.7220 0.0566 1.0000 Uiso R .
H171 H 0.2915 0.6048 0.7254 0.0561 1.0000 Uiso R .
H181 H 0.5581 1.3104 0.8572 0.0339 1.0000 Uiso R .
H182 H 0.4859 1.3774 0.8092 0.0330 1.0000 Uiso R .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 5_656 Zr1 C7 5_656 33.23(9) yes
C3 5_656 Zr1 C4 5_656 33.37(9) yes
C7 5_656 Zr1 C4 5_656 54.01(9) yes
C3 5_656 Zr1 C6 5_656 54.75(9) yes
C7 5_656 Zr1 C6 5_656 32.15(9) yes
C4 5_656 Zr1 C6 5_656 53.81(8) yes
C3 5_656 Zr1 C5 5_656 54.64(8) yes
C7 5_656 Zr1 C5 5_656 53.26(8) yes
C4 5_656 Zr1 C5 5_656 32.40(8) yes
C6 5_656 Zr1 C5 5_656 32.11(8) yes
C3 5_656 Zr1 Cl2 5_656 124.99(6) yes
C7 5_656 Zr1 Cl2 5_656 132.12(6) yes
C4 5_656 Zr1 Cl2 5_656 91.67(6) yes
C6 5_656 Zr1 Cl2 5_656 102.11(6) yes
C5 5_656 Zr1 Cl2 5_656 79.61(6) yes
C3 5_656 Zr1 Cl2 . 121.29(6) yes
C7 5_656 Zr1 Cl2 . 88.50(7) yes
C4 5_656 Zr1 Cl2 . 133.03(6) yes
C6 5_656 Zr1 Cl2 . 79.30(6) yes
C5 5_656 Zr1 Cl2 . 104.26(6) yes
C3 5_656 Zr1 C3 . 70.13(13) yes
C7 5_656 Zr1 C3 . 92.66(9) yes
C4 5_656 Zr1 C3 . 87.86(9) yes
C6 5_656 Zr1 C3 . 123.20(9) yes
C5 5_656 Zr1 C3 . 119.85(9) yes
C3 5_656 Zr1 C4 . 87.86(9) yes
C7 5_656 Zr1 C4 . 94.19(9) yes
C4 5_656 Zr1 C4 . 115.58(12) yes
C6 5_656 Zr1 C4 . 124.84(8) yes
C5 5_656 Zr1 C4 . 142.33(8) yes
C3 5_656 Zr1 C5 . 119.85(9) yes
C7 5_656 Zr1 C5 . 123.39(8) yes
C4 5_656 Zr1 C5 . 142.33(8) yes
C6 5_656 Zr1 C5 . 147.70(8) yes
C5 5_656 Zr1 C5 . 174.33(12) yes
C3 5_656 Zr1 C6 . 123.20(9) yes
C7 5_656 Zr1 C6 . 146.01(9) yes
C4 5_656 Zr1 C6 . 124.84(8) yes
C6 5_656 Zr1 C6 . 177.93(12) yes
C5 5_656 Zr1 C6 . 147.70(8) yes
C3 5_656 Zr1 C7 . 92.66(9) yes
C7 5_656 Zr1 C7 . 122.28(13) yes
C4 5_656 Zr1 C7 . 94.19(9) yes
C6 5_656 Zr1 C7 . 146.01(9) yes
C5 5_656 Zr1 C7 . 123.39(8) yes
Cl2 5_656 Zr1 Cl2 . 96.24(4) yes
Cl2 5_656 Zr1 C3 . 121.29(6) yes
Cl2 . Zr1 C3 . 124.99(6) yes
Cl2 5_656 Zr1 C4 . 133.03(6) yes
Cl2 . Zr1 C4 . 91.67(6) yes
C3 . Zr1 C4 . 33.37(9) yes
Cl2 5_656 Zr1 C5 . 104.26(6) yes
Cl2 . Zr1 C5 . 79.61(6) yes
C3 . Zr1 C5 . 54.64(8) yes
C4 . Zr1 C5 . 32.40(8) yes
Cl2 5_656 Zr1 C6 . 79.30(6) yes
Cl2 . Zr1 C6 . 102.11(6) yes
C3 . Zr1 C6 . 54.75(9) yes
C4 . Zr1 C6 . 53.81(8) yes
C5 . Zr1 C6 . 32.11(8) yes
Cl2 5_656 Zr1 C7 . 88.50(7) yes
Cl2 . Zr1 C7 . 132.12(6) yes
C3 . Zr1 C7 . 33.23(9) yes
C4 . Zr1 C7 . 54.01(9) yes
C5 . Zr1 C7 . 53.26(8) yes
C6 . Zr1 C7 . 32.15(9) yes
Zr1 . C3 C4 . 76.31(15) yes
Zr1 . C3 C7 . 74.97(15) yes
C4 . C3 C7 . 106.5(2) yes
Zr1 . C3 C18 . 117.34(18) yes
C4 . C3 C18 . 129.6(2) yes
C7 . C3 C18 . 123.7(3) yes
C3 . C4 Zr1 . 70.32(14) yes
C3 . C4 C5 . 108.0(2) yes
Zr1 . C4 C5 . 75.86(15) yes
C3 . C4 C14 . 132.4(3) yes
Zr1 . C4 C14 . 123.59(18) yes
C5 . C4 C14 . 119.4(2) yes
C4 . C5 Zr1 . 71.73(14) yes
C4 . C5 C6 . 107.7(2) yes
Zr1 . C5 C6 . 72.81(14) yes
C4 . C5 C10 . 120.8(2) yes
Zr1 . C5 C10 . 120.94(18) yes
C6 . C5 C10 . 131.5(2) yes
C5 . C6 Zr1 . 75.08(15) yes
C5 . C6 C7 . 107.7(2) yes
Zr1 . C6 C7 . 71.50(15) yes
C5 . C6 C9 . 128.4(3) yes
Zr1 . C6 C9 . 124.36(18) yes
C7 . C6 C9 . 123.5(2) yes
Zr1 . C7 C3 . 71.81(15) yes
Zr1 . C7 C6 . 76.34(15) yes
C3 . C7 C6 . 110.0(2) yes
Zr1 . C7 C8 . 119.72(18) yes
C3 . C7 C8 . 126.6(3) yes
C6 . C7 C8 . 123.5(3) yes
C7 . C8 H83 . 110.5 no
C7 . C8 H82 . 110.3 no
H83 . C8 H82 . 109.0 no
C7 . C8 H81 . 111.7 no
H83 . C8 H81 . 108.2 no
H82 . C8 H81 . 107.1 no
C6 . C9 H91 . 110.6 no
C6 . C9 H92 . 110.2 no
H91 . C9 H92 . 109.0 no
C6 . C9 H93 . 110.4 no
H91 . C9 H93 . 108.1 no
H92 . C9 H93 . 108.6 no
C5 . C10 C11 . 119.6(2) yes
C5 . C10 C12 . 118.1(3) yes
C11 . C10 C12 . 122.3(2) yes
C10 . C11 H113 . 110.9 no
C10 . C11 H112 . 110.8 no
H113 . C11 H112 . 108.2 no
C10 . C11 H111 . 110.0 no
H113 . C11 H111 . 109.5 no
H112 . C11 H111 . 107.3 no
C10 . C12 C13 . 120.9(3) yes
C10 . C12 C17 . 120.9(3) yes
C13 . C12 C17 . 118.2(3) yes
C12 . C13 C14 . 122.3(2) yes
C12 . C13 C16 . 117.4(3) yes
C14 . C13 C16 . 120.3(3) yes
C4 . C14 C13 . 117.8(3) yes
C4 . C14 C15 . 121.5(3) yes
C13 . C14 C15 . 120.3(2) yes
C14 . C15 H151 . 109.8 no
C14 . C15 H152 . 110.9 no
H151 . C15 H152 . 108.8 no
C14 . C15 H153 . 110.0 no
H151 . C15 H153 . 109.5 no
H152 . C15 H153 . 107.8 no
C13 . C16 H163 . 112.8 no
C13 . C16 H162 . 110.4 no
H163 . C16 H162 . 107.7 no
C13 . C16 H161 . 110.7 no
H163 . C16 H161 . 107.9 no
H162 . C16 H161 . 107.1 no
C12 . C17 H173 . 109.3 no
C12 . C17 H172 . 110.4 no
H173 . C17 H172 . 107.7 no
C12 . C17 H171 . 111.2 no
H173 . C17 H171 . 108.5 no
H172 . C17 H171 . 109.5 no
C18 5_656 C18 C3 . 113.25(17) yes
C18 5_656 C18 H181 . 109.5 no
C3 . C18 H181 . 105.3 no
C18 5_656 C18 H182 . 108.9 no
C3 . C18 H182 . 111.0 no
H181 . C18 H182 . 108.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 C3 5_656 2.479(3) yes
Zr1 C7 5_656 2.520(3) yes
Zr1 C4 5_656 2.558(3) yes
Zr1 C6 5_656 2.582(3) yes
Zr1 C5 5_656 2.612(3) yes
Zr1 Cl2 5_656 2.4358(7) yes
Zr1 Cl2 . 2.4358(7) yes
Zr1 C3 . 2.479(3) yes
Zr1 C4 . 2.558(3) yes
Zr1 C5 . 2.612(3) yes
Zr1 C6 . 2.582(3) yes
Zr1 C7 . 2.520(3) yes
C3 C4 . 1.448(4) yes
C3 C7 . 1.430(4) yes
C3 C18 . 1.504(4) yes
C4 C5 . 1.443(4) yes
C4 C14 . 1.439(4) yes
C5 C6 . 1.437(4) yes
C5 C10 . 1.430(4) yes
C6 C7 . 1.414(4) yes
C6 C9 . 1.503(4) yes
C7 C8 . 1.506(4) yes
C8 H83 . 0.956 no
C8 H82 . 0.955 no
C8 H81 . 0.963 no
C9 H91 . 0.962 no
C9 H92 . 0.962 no
C9 H93 . 0.964 no
C10 C11 . 1.514(4) yes
C10 C12 . 1.385(4) yes
C11 H113 . 0.962 no
C11 H112 . 0.963 no
C11 H111 . 0.953 no
C12 C13 . 1.432(4) yes
C12 C17 . 1.516(4) yes
C13 C14 . 1.382(4) yes
C13 C16 . 1.514(4) yes
C14 C15 . 1.510(4) yes
C15 H151 . 0.953 no
C15 H152 . 0.957 no
C15 H153 . 0.961 no
C16 H163 . 0.955 no
C16 H162 . 0.963 no
C16 H161 . 0.952 no
C17 H173 . 0.964 no
C17 H172 . 0.960 no
C17 H171 . 0.973 no
C18 C18 5_656 1.546(6) yes
C18 H181 . 0.956 no
C18 H182 . 0.973 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C15 H152 C18 136 0.96 2.52 3.275(5) yes
