#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/38/4063855.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_4063855
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 Hf1'
_chemical_formula_sum            'C32 H40 Cl2 Hf'
_chemical_formula_weight         674.07
_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
_cell_angle_alpha                90
_cell_angle_beta                 129.4663(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4431(3)
_cell_length_b                   8.2319(2)
_cell_length_c                   16.4078(3)
_cell_measurement_reflns_used    3181
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2653.00(9)
_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  0.037
_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            19769
_diffrn_reflns_theta_full        27.486
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         5.209
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.154
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.18
_refine_diff_density_min         -1.24
_refine_ls_extinction_coef       43(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.000213
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² +14.93P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0554
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0554
_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                2861
_reflns_number_total             3018
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.25
_oxford_diffrn_Wilson_scale      61.02
_oxford_refine_ls_r_factor_ref   0.0257
_oxford_refine_ls_scale          0.12792(5)
_oxford_reflns_number_all        3017
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 5993
_cod_data_source_file            om100986j_si_002.cif
_cod_data_source_block           rac-3
_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 Hf1'
_cod_database_code               4063855
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
Hf1 Hf 0.5000 0.614802(18) 0.2500 0.0149 1.0000 Uani S T
Cl2 Cl 0.59054(4) 0.81192(9) 0.34814(6) 0.0225 1.0000 Uani . .
C3 C 0.44830(15) 0.4691(4) 0.0807(2) 0.0186 1.0000 Uani . .
C4 C 0.50157(15) 0.3702(3) 0.1652(2) 0.0178 1.0000 Uani . .
C5 C 0.56495(14) 0.4508(3) 0.2084(2) 0.0166 1.0000 Uani . .
C6 C 0.54847(15) 0.6010(3) 0.1506(2) 0.0162 1.0000 Uani . .
C7 C 0.47586(14) 0.6115(3) 0.0722(2) 0.0165 1.0000 Uani . .
C8 C 0.43387(16) 0.7361(4) -0.0135(2) 0.0244 1.0000 Uani . .
C9 C 0.60134(15) 0.7085(4) 0.1761(2) 0.0192 1.0000 Uani . .
C10 C 0.66780(15) 0.6688(4) 0.2599(2) 0.0222 1.0000 Uani . .
C11 C 0.68453(15) 0.5143(4) 0.3125(2) 0.0224 1.0000 Uani . .
C12 C 0.63520(15) 0.4034(4) 0.2856(2) 0.0200 1.0000 Uani . .
C13 C 0.65467(17) 0.2322(4) 0.3280(3) 0.0292 1.0000 Uani . .
C14 C 0.75915(17) 0.4740(5) 0.3978(3) 0.0343 1.0000 Uani . .
C15 C 0.72560(18) 0.7861(5) 0.3001(3) 0.0362 1.0000 Uani . .
C16 C 0.58277(17) 0.8625(4) 0.1135(3) 0.0270 1.0000 Uani . .
C17 C 0.37320(15) 0.4291(4) 0.0065(2) 0.0246 1.0000 Uani . .
C41 C 0.48978(17) 0.2084(4) 0.1942(3) 0.0238 1.0000 Uani . .
H83 H 0.4462 0.8443 0.0172 0.0341 1.0000 Uiso R .
H82 H 0.4410 0.7318 -0.0648 0.0344 1.0000 Uiso R .
H81 H 0.3865 0.7226 -0.0489 0.0345 1.0000 Uiso R .
H131 H 0.6877 0.1901 0.3216 0.0444 1.0000 Uiso R .
H132 H 0.6148 0.1628 0.2879 0.0448 1.0000 Uiso R .
H133 H 0.6746 0.2328 0.4021 0.0445 1.0000 Uiso R .
H143 H 0.7659 0.3592 0.4108 0.0455 1.0000 Uiso R .
H142 H 0.7849 0.5145 0.3769 0.0453 1.0000 Uiso R .
H141 H 0.7756 0.5306 0.4622 0.0454 1.0000 Uiso R .
H151 H 0.7567 0.7814 0.3765 0.0521 1.0000 Uiso R .
H152 H 0.7494 0.7480 0.2754 0.0520 1.0000 Uiso R .
H153 H 0.7089 0.8956 0.2760 0.0522 1.0000 Uiso R .
H163 H 0.6227 0.9165 0.1319 0.0423 1.0000 Uiso R .
H162 H 0.5520 0.8359 0.0390 0.0420 1.0000 Uiso R .
H161 H 0.5598 0.9345 0.1287 0.0423 1.0000 Uiso R .
H173 H 0.3550 0.4361 -0.0661 0.0351 1.0000 Uiso R .
H172 H 0.3665 0.3210 0.0179 0.0353 1.0000 Uiso R .
H171 H 0.3485 0.4973 0.0177 0.0355 1.0000 Uiso R .
H411 H 0.5148 0.1229 0.1895 0.0322 1.0000 Uiso R .
H412 H 0.4408 0.1870 0.1432 0.0322 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'
Hf -0.5830 6.1852 29.1440 1.8326 15.1726 9.5999 14.7586 0.2751 4.3001 72.0290
8.5815 '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
C4 5_655 Hf1 C3 5_655 33.40(9) yes
C4 5_655 Hf1 C5 5_655 33.54(9) yes
C3 5_655 Hf1 C5 5_655 54.45(9) yes
C4 5_655 Hf1 C7 5_655 55.12(9) yes
C3 5_655 Hf1 C7 5_655 32.43(9) yes
C5 5_655 Hf1 C7 5_655 54.30(9) yes
C4 5_655 Hf1 C6 5_655 54.88(9) yes
C3 5_655 Hf1 C6 5_655 53.52(9) yes
C5 5_655 Hf1 C6 5_655 32.71(8) yes
C7 5_655 Hf1 C6 5_655 32.19(9) yes
C4 5_655 Hf1 Cl2 5_655 125.16(7) yes
C3 5_655 Hf1 Cl2 5_655 132.05(7) yes
C5 5_655 Hf1 Cl2 5_655 91.64(7) yes
C7 5_655 Hf1 Cl2 5_655 101.69(6) yes
C6 5_655 Hf1 Cl2 5_655 79.37(6) yes
C4 5_655 Hf1 Cl2 . 121.64(7) yes
C3 5_655 Hf1 Cl2 . 88.64(7) yes
C5 5_655 Hf1 Cl2 . 133.35(6) yes
C7 5_655 Hf1 Cl2 . 79.14(6) yes
C6 5_655 Hf1 Cl2 . 104.09(6) yes
C4 5_655 Hf1 C3 . 92.85(10) yes
C3 5_655 Hf1 C3 . 122.62(14) yes
C5 5_655 Hf1 C3 . 94.08(9) yes
C7 5_655 Hf1 C3 . 146.50(9) yes
C6 5_655 Hf1 C3 . 123.54(9) yes
C4 5_655 Hf1 C4 . 70.28(14) yes
C3 5_655 Hf1 C4 . 92.85(10) yes
C5 5_655 Hf1 C4 . 87.95(10) yes
C7 5_655 Hf1 C4 . 123.68(9) yes
C6 5_655 Hf1 C4 . 120.23(9) yes
C4 5_655 Hf1 C5 . 87.95(10) yes
C3 5_655 Hf1 C5 . 94.08(9) yes
C5 5_655 Hf1 C5 . 115.79(13) yes
C7 5_655 Hf1 C5 . 124.91(9) yes
C6 5_655 Hf1 C5 . 142.64(9) yes
C4 5_655 Hf1 C6 . 120.23(9) yes
C3 5_655 Hf1 C6 . 123.54(9) yes
C5 5_655 Hf1 C6 . 142.64(9) yes
C7 5_655 Hf1 C6 . 147.71(9) yes
C6 5_655 Hf1 C6 . 174.98(12) yes
C4 5_655 Hf1 C7 . 123.68(9) yes
C3 5_655 Hf1 C7 . 146.50(9) yes
C5 5_655 Hf1 C7 . 124.91(9) yes
C7 5_655 Hf1 C7 . 178.79(12) yes
C6 5_655 Hf1 C7 . 147.71(9) yes
Cl2 5_655 Hf1 Cl2 . 95.43(4) yes
Cl2 5_655 Hf1 C3 . 88.64(7) yes
Cl2 . Hf1 C3 . 132.05(7) yes
Cl2 5_655 Hf1 C4 . 121.64(7) yes
Cl2 . Hf1 C4 . 125.16(7) yes
C3 . Hf1 C4 . 33.40(9) yes
Cl2 5_655 Hf1 C5 . 133.35(6) yes
Cl2 . Hf1 C5 . 91.64(7) yes
C3 . Hf1 C5 . 54.45(9) yes
C4 . Hf1 C5 . 33.54(9) yes
Cl2 5_655 Hf1 C6 . 104.09(6) yes
Cl2 . Hf1 C6 . 79.37(6) yes
C3 . Hf1 C6 . 53.52(9) yes
C4 . Hf1 C6 . 54.88(9) yes
C5 . Hf1 C6 . 32.71(8) yes
Cl2 5_655 Hf1 C7 . 79.14(6) yes
Cl2 . Hf1 C7 . 101.69(6) yes
C3 . Hf1 C7 . 32.43(9) yes
C4 . Hf1 C7 . 55.12(9) yes
C5 . Hf1 C7 . 54.30(9) yes
C6 . Hf1 C7 . 32.19(9) yes
Hf1 . C3 C4 . 71.91(16) yes
Hf1 . C3 C7 . 76.58(16) yes
C4 . C3 C7 . 110.1(2) yes
Hf1 . C3 C17 . 120.2(2) yes
C4 . C3 C17 . 126.3(3) yes
C7 . C3 C17 . 123.5(3) yes
Hf1 . C4 C3 . 74.68(16) yes
Hf1 . C4 C5 . 76.20(16) yes
C3 . C4 C5 . 106.8(2) yes
Hf1 . C4 C41 . 117.78(19) yes
C3 . C4 C41 . 123.7(3) yes
C5 . C4 C41 . 129.4(3) yes
C4 . C5 Hf1 . 70.25(15) yes
C4 . C5 C6 . 107.6(2) yes
Hf1 . C5 C6 . 75.80(16) yes
C4 . C5 C12 . 132.9(3) yes
Hf1 . C5 C12 . 124.23(19) yes
C6 . C5 C12 . 119.2(3) yes
C5 . C6 Hf1 . 71.49(16) yes
C5 . C6 C7 . 108.1(2) yes
Hf1 . C6 C7 . 72.86(16) yes
C5 . C6 C9 . 120.6(3) yes
Hf1 . C6 C9 . 121.48(19) yes
C7 . C6 C9 . 131.3(3) yes
C6 . C7 C3 . 107.3(2) yes
C6 . C7 Hf1 . 74.94(16) yes
C3 . C7 Hf1 . 70.99(16) yes
C6 . C7 C8 . 128.7(3) yes
C3 . C7 C8 . 123.6(3) yes
Hf1 . C7 C8 . 124.73(19) yes
C7 . C8 H83 . 109.6 no
C7 . C8 H82 . 112.0 no
H83 . C8 H82 . 108.0 no
C7 . C8 H81 . 111.2 no
H83 . C8 H81 . 106.7 no
H82 . C8 H81 . 109.2 no
C6 . C9 C10 . 118.3(3) yes
C6 . C9 C16 . 119.4(3) yes
C10 . C9 C16 . 122.3(3) yes
C9 . C10 C11 . 121.0(3) yes
C9 . C10 C15 . 121.3(3) yes
C11 . C10 C15 . 117.8(3) yes
C10 . C11 C12 . 122.1(3) yes
C10 . C11 C14 . 117.8(3) yes
C12 . C11 C14 . 120.1(3) yes
C5 . C12 C11 . 118.1(3) yes
C5 . C12 C13 . 121.2(3) yes
C11 . C12 C13 . 120.4(3) yes
C12 . C13 H131 . 109.6 no
C12 . C13 H132 . 110.0 no
H131 . C13 H132 . 108.7 no
C12 . C13 H133 . 109.1 no
H131 . C13 H133 . 109.6 no
H132 . C13 H133 . 109.8 no
C11 . C14 H143 . 111.3 no
C11 . C14 H142 . 109.1 no
H143 . C14 H142 . 110.5 no
C11 . C14 H141 . 108.7 no
H143 . C14 H141 . 109.8 no
H142 . C14 H141 . 107.2 no
C10 . C15 H151 . 107.9 no
C10 . C15 H152 . 107.7 no
H151 . C15 H152 . 108.3 no
C10 . C15 H153 . 111.3 no
H151 . C15 H153 . 110.5 no
H152 . C15 H153 . 111.1 no
C9 . C16 H163 . 111.3 no
C9 . C16 H162 . 108.8 no
H163 . C16 H162 . 110.2 no
C9 . C16 H161 . 108.5 no
H163 . C16 H161 . 108.9 no
H162 . C16 H161 . 109.0 no
C3 . C17 H173 . 110.5 no
C3 . C17 H172 . 109.9 no
H173 . C17 H172 . 107.1 no
C3 . C17 H171 . 111.8 no
H173 . C17 H171 . 110.3 no
H172 . C17 H171 . 107.1 no
C41 5_655 C41 C4 . 112.81(18) yes
C41 5_655 C41 H411 . 110.1 no
C4 . C41 H411 . 109.9 no
C41 5_655 C41 H412 . 107.3 no
C4 . C41 H412 . 106.8 no
H411 . C41 H412 . 109.8 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
Hf1 C4 5_655 2.462(3) yes
Hf1 C3 5_655 2.498(3) yes
Hf1 C5 5_655 2.541(3) yes
Hf1 C7 5_655 2.571(3) yes
Hf1 C6 5_655 2.598(3) yes
Hf1 Cl2 5_655 2.4118(7) yes
Hf1 Cl2 . 2.4118(7) yes
Hf1 C3 . 2.498(3) yes
Hf1 C4 . 2.462(3) yes
Hf1 C5 . 2.541(3) yes
Hf1 C6 . 2.598(3) yes
Hf1 C7 . 2.571(3) yes
C3 C4 . 1.426(4) yes
C3 C7 . 1.417(4) yes
C3 C17 . 1.511(4) yes
C4 C5 . 1.446(4) yes
C4 C41 . 1.507(4) yes
C5 C6 . 1.448(4) yes
C5 C12 . 1.440(4) yes
C6 C7 . 1.433(4) yes
C6 C9 . 1.433(4) yes
C7 C8 . 1.504(4) yes
C8 H83 . 0.972 no
C8 H82 . 0.967 no
C8 H81 . 0.956 no
C9 C10 . 1.379(4) yes
C9 C16 . 1.506(4) yes
C10 C11 . 1.441(4) yes
C10 C15 . 1.515(4) yes
C11 C12 . 1.378(4) yes
C11 C14 . 1.515(4) yes
C12 C13 . 1.509(4) yes
C13 H131 . 0.973 no
C13 H132 . 0.970 no
C13 H133 . 0.976 no
C14 H143 . 0.960 no
C14 H142 . 0.971 no
C14 H141 . 0.972 no
C15 H151 . 0.968 no
C15 H152 . 0.971 no
C15 H153 . 0.968 no
C16 H163 . 0.965 no
C16 H162 . 0.969 no
C16 H161 . 0.971 no
C17 H173 . 0.966 no
C17 H172 . 0.947 no
C17 H171 . 0.944 no
C41 C41 5_655 1.554(6) yes
C41 H411 . 0.984 no
C41 H412 . 0.980 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
C13 H132 C41 134 0.97 2.53 3.279(5) yes
