#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:04:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178633 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/44/4074445.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_4074445
loop_
_publ_author_name
'Lee, Suh-Jane'
'Shapiro, Pamela J.'
'Twamley, Brendan'
_publ_section_title
;
 Synthesis and Characterization of [(C5Me4H)2Al]+, an Initiator for the
 Polymerization of Isobutene. X-ray Crystal Structures of
 [(C5Me4H)2Al(μ-Cl)]2and [(C5Me4H)2Al][B(C6F5)4]
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5582
_journal_paper_doi               10.1021/om0606439
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C36 H52 Al2 Cl2'
_chemical_formula_sum            'C36 H52 Al2 Cl2'
_chemical_formula_weight         609.64
_chemical_name_common            '[Cp'2Al-mu-Cl]2'
_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                108.88(3)
_cell_angle_beta                 111.74(3)
_cell_angle_gamma                92.98(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6221(17)
_cell_length_b                   10.595(2)
_cell_length_c                   10.614(2)
_cell_measurement_reflns_used    4723
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.22
_cell_volume                     835.7(4)
_computing_cell_refinement       'Bruker SAINTPlus v. 6.02'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPlus v. 6.02'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker/Siemens SMART 1K'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8693
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.9355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0385
_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)+(0.0513P)²+0.4156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                2446
_reflns_number_total             3011
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0606439si20060717_121031.cif
_cod_data_source_block           bt248
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074445
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
Al1 Al 0.48855(8) 0.66409(7) 0.59426(7) 0.03483(19) Uani 1 1 d .
Cl1 Cl 0.29961(6) 0.45626(5) 0.43627(6) 0.03501(17) Uani 1 1 d .
C1 C 0.4604(2) 0.7872(2) 0.4825(2) 0.0303(5) Uani 1 1 d .
H1A H 0.4549 0.8799 0.5403 0.036 Uiso 1 1 calc R
C2 C 0.6016(3) 0.7888(2) 0.4345(2) 0.0315(5) Uani 1 1 d .
C3 C 0.5385(3) 0.7216(2) 0.2885(2) 0.0311(5) Uani 1 1 d .
C4 C 0.3536(3) 0.6821(2) 0.2315(2) 0.0310(5) Uani 1 1 d .
C5 C 0.3047(3) 0.7247(2) 0.3428(2) 0.0309(5) Uani 1 1 d .
C6 C 0.7825(3) 0.8563(3) 0.5380(3) 0.0461(6) Uani 1 1 d .
H6A H 0.8564 0.8331 0.4872 0.069 Uiso 1 1 calc R
H6B H 0.8167 0.8254 0.6191 0.069 Uiso 1 1 calc R
H6C H 0.7912 0.9542 0.5744 0.069 Uiso 1 1 calc R
C7 C 0.6355(3) 0.6900(2) 0.1936(3) 0.0455(6) Uani 1 1 d .
H7A H 0.7541 0.7341 0.2516 0.068 Uiso 1 1 calc R
H7B H 0.5877 0.7232 0.1149 0.068 Uiso 1 1 calc R
H7C H 0.6272 0.5924 0.1530 0.068 Uiso 1 1 calc R
C8 C 0.2407(3) 0.6094(2) 0.0727(2) 0.0432(6) Uani 1 1 d .
H8A H 0.1225 0.6043 0.0587 0.065 Uiso 1 1 calc R
H8B H 0.2627 0.5182 0.0399 0.065 Uiso 1 1 calc R
H8C H 0.2640 0.6587 0.0169 0.065 Uiso 1 1 calc R
C9 C 0.1275(3) 0.7152(3) 0.3344(3) 0.0427(6) Uani 1 1 d .
H9A H 0.0489 0.6538 0.2378 0.064 Uiso 1 1 calc R
H9B H 0.0983 0.8046 0.3530 0.064 Uiso 1 1 calc R
H9C H 0.1202 0.6810 0.4069 0.064 Uiso 1 1 calc R
C10 C 0.5035(3) 0.6646(2) 0.7914(2) 0.0316(5) Uani 1 1 d .
H10A H 0.5121 0.5743 0.7823 0.038 Uiso 1 1 calc R
C11 C 0.3486(3) 0.7162(2) 0.7524(2) 0.0306(5) Uani 1 1 d .
C12 C 0.3934(3) 0.8547(2) 0.7806(2) 0.0315(5) Uani 1 1 d .
C13 C 0.5731(3) 0.8914(2) 0.8382(2) 0.0319(5) Uani 1 1 d .
C14 C 0.6431(3) 0.7764(2) 0.8469(2) 0.0316(5) Uani 1 1 d .
C15 C 0.1722(3) 0.6371(2) 0.7004(2) 0.0392(5) Uani 1 1 d .
H15A H 0.1321 0.6672 0.7774 0.059 Uiso 1 1 calc R
H15B H 0.1750 0.5410 0.6754 0.059 Uiso 1 1 calc R
H15C H 0.0961 0.6521 0.6151 0.059 Uiso 1 1 calc R
C16 C 0.2735(3) 0.9496(2) 0.7518(3) 0.0450(6) Uani 1 1 d .
H16A H 0.2919 1.0213 0.8434 0.067 Uiso 1 1 calc R
H16B H 0.1571 0.8997 0.7060 0.067 Uiso 1 1 calc R
H16C H 0.2939 0.9894 0.6876 0.067 Uiso 1 1 calc R
C17 C 0.6702(3) 1.0305(2) 0.8780(3) 0.0469(6) Uani 1 1 d .
H17A H 0.6289 1.0581 0.7946 0.070 Uiso 1 1 calc R
H17B H 0.7904 1.0283 0.9063 0.070 Uiso 1 1 calc R
H17C H 0.6540 1.0949 0.9589 0.070 Uiso 1 1 calc R
C18 C 0.8289(3) 0.7709(3) 0.9148(2) 0.0435(6) Uani 1 1 d .
H18A H 0.8696 0.8075 1.0203 0.065 Uiso 1 1 calc R
H18B H 0.8935 0.8243 0.8853 0.065 Uiso 1 1 calc R
H18C H 0.8433 0.6772 0.8826 0.065 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'
Al Al 0.0645 0.0514 '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'
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
C1 Al1 C10 140.46(9) . .
C1 Al1 Cl1 107.95(7) . 2_666
C10 Al1 Cl1 101.78(7) . 2_666
C1 Al1 C14 113.61(9) . .
C10 Al1 C14 37.49(8) . .
Cl1 Al1 C14 94.17(7) 2_666 .
C1 Al1 Cl1 107.46(7) . .
C10 Al1 Cl1 100.52(7) . .
Cl1 Al1 Cl1 84.86(4) 2_666 .
C14 Al1 Cl1 136.95(7) . .
C1 Al1 C11 112.03(9) . .
C10 Al1 C11 37.31(8) . .
Cl1 Al1 C11 138.27(6) 2_666 .
C14 Al1 C11 59.19(7) . .
Cl1 Al1 C11 94.11(6) . .
Al1 Cl1 Al1 95.14(4) 2_666 .
C2 C1 C5 103.88(17) . .
C2 C1 Al1 108.86(14) . .
C5 C1 Al1 108.57(14) . .
C2 C1 H1A 111.7 . .
C5 C1 H1A 111.7 . .
Al1 C1 H1A 111.7 . .
C3 C2 C1 108.84(18) . .
C3 C2 C6 128.2(2) . .
C1 C2 C6 123.01(19) . .
C2 C3 C4 109.08(18) . .
C2 C3 C7 127.7(2) . .
C4 C3 C7 123.2(2) . .
C5 C4 C3 109.21(18) . .
C5 C4 C8 127.1(2) . .
C3 C4 C8 123.7(2) . .
C4 C5 C9 127.7(2) . .
C4 C5 C1 108.56(18) . .
C9 C5 C1 123.70(19) . .
C2 C6 H6A 109.5 . .
C2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C5 C9 H9A 109.5 . .
C5 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C5 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C14 107.58(18) . .
C11 C10 Al1 83.09(13) . .
C14 C10 Al1 82.64(13) . .
C11 C10 H10A 126.2 . .
C14 C10 H10A 126.2 . .
Al1 C10 H10A 102.1 . .
C12 C11 C10 107.44(18) . .
C12 C11 C15 126.7(2) . .
C10 C11 C15 125.8(2) . .
C12 C11 Al1 89.48(13) . .
C10 C11 Al1 59.60(11) . .
C15 C11 Al1 118.48(14) . .
C11 C12 C13 108.81(19) . .
C11 C12 C16 126.5(2) . .
C13 C12 C16 124.7(2) . .
C14 C13 C12 108.88(19) . .
C14 C13 C17 126.3(2) . .
C12 C13 C17 124.8(2) . .
C13 C14 C10 107.27(18) . .
C13 C14 C18 127.2(2) . .
C10 C14 C18 125.3(2) . .
C13 C14 Al1 89.54(13) . .
C10 C14 Al1 59.87(11) . .
C18 C14 Al1 119.28(15) . .
C11 C15 H15A 109.5 . .
C11 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C11 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C12 C16 H16A 109.5 . .
C12 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C12 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C13 C17 H17A 109.5 . .
C13 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C13 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C14 C18 H18A 109.5 . .
C14 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C14 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 C1 1.997(2) .
Al1 C10 2.046(2) .
Al1 Cl1 2.3409(11) 2_666
Al1 C14 2.346(2) .
Al1 Cl1 2.3511(15) .
Al1 C11 2.355(2) .
Cl1 Al1 2.3409(11) 2_666
C1 C2 1.485(3) .
C1 C5 1.495(3) .
C1 H1A 0.9900 .
C2 C3 1.351(3) .
C2 C6 1.502(3) .
C3 C4 1.461(3) .
C3 C7 1.503(3) .
C4 C5 1.349(3) .
C4 C8 1.499(3) .
C5 C9 1.494(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 H6C 0.9700 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 H7C 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 H9C 0.9700 .
C10 C11 1.438(3) .
C10 C14 1.440(3) .
C10 H10A 0.9400 .
C11 C12 1.401(3) .
C11 C15 1.505(3) .
C12 C13 1.417(3) .
C12 C16 1.499(3) .
C13 C14 1.402(3) .
C13 C17 1.503(3) .
C14 C18 1.507(3) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 H15C 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 H16C 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 H17C 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 H18C 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 Al1 Cl1 Al1 107.23(7) . 2_666
C10 Al1 Cl1 Al1 -101.05(7) . 2_666
Cl1 Al1 Cl1 Al1 0.0 2_666 2_666
C14 Al1 Cl1 Al1 -90.62(9) . 2_666
C11 Al1 Cl1 Al1 -138.14(6) . 2_666
C10 Al1 C1 C2 126.21(16) . .
Cl1 Al1 C1 C2 -10.63(15) 2_666 .
C14 Al1 C1 C2 92.38(15) . .
Cl1 Al1 C1 C2 -100.82(14) . .
C11 Al1 C1 C2 157.16(13) . .
C10 Al1 C1 C5 -121.32(16) . .
Cl1 Al1 C1 C5 101.84(14) 2_666 .
C14 Al1 C1 C5 -155.15(13) . .
Cl1 Al1 C1 C5 11.66(15) . .
C11 Al1 C1 C5 -90.37(15) . .
C5 C1 C2 C3 -6.4(2) . .
Al1 C1 C2 C3 109.12(17) . .
C5 C1 C2 C6 173.5(2) . .
Al1 C1 C2 C6 -70.9(2) . .
C1 C2 C3 C4 4.4(2) . .
C6 C2 C3 C4 -175.6(2) . .
C1 C2 C3 C7 -176.0(2) . .
C6 C2 C3 C7 4.1(4) . .
C2 C3 C4 C5 -0.3(2) . .
C7 C3 C4 C5 -179.96(19) . .
C2 C3 C4 C8 178.1(2) . .
C7 C3 C4 C8 -1.6(3) . .
C3 C4 C5 C9 175.4(2) . .
C8 C4 C5 C9 -2.8(4) . .
C3 C4 C5 C1 -3.9(2) . .
C8 C4 C5 C1 177.8(2) . .
C2 C1 C5 C4 6.3(2) . .
Al1 C1 C5 C4 -109.49(17) . .
C2 C1 C5 C9 -173.1(2) . .
Al1 C1 C5 C9 71.2(2) . .
C1 Al1 C10 C11 51.86(19) . .
Cl1 Al1 C10 C11 -169.80(11) 2_666 .
C14 Al1 C10 C11 108.81(18) . .
Cl1 Al1 C10 C11 -82.91(12) . .
C1 Al1 C10 C14 -56.95(19) . .
Cl1 Al1 C10 C14 81.39(12) 2_666 .
Cl1 Al1 C10 C14 168.28(11) . .
C11 Al1 C10 C14 -108.81(18) . .
C14 C10 C11 C12 1.3(2) . .
Al1 C10 C11 C12 -78.73(16) . .
C14 C10 C11 C15 -175.00(19) . .
Al1 C10 C11 C15 105.0(2) . .
C14 C10 C11 Al1 79.99(15) . .
C1 Al1 C11 C12 -36.64(15) . .
C10 Al1 C11 C12 110.66(18) . .
Cl1 Al1 C11 C12 125.76(12) 2_666 .
C14 Al1 C11 C12 68.53(13) . .
Cl1 Al1 C11 C12 -147.35(12) . .
C1 Al1 C11 C10 -147.30(13) . .
Cl1 Al1 C11 C10 15.10(16) 2_666 .
C14 Al1 C11 C10 -42.13(12) . .
Cl1 Al1 C11 C10 101.99(12) . .
C1 Al1 C11 C15 95.80(18) . .
C10 Al1 C11 C15 -116.9(2) . .
Cl1 Al1 C11 C15 -101.79(17) 2_666 .
C14 Al1 C11 C15 -159.0(2) . .
Cl1 Al1 C11 C15 -14.91(17) . .
C10 C11 C12 C13 -0.8(2) . .
C15 C11 C12 C13 175.46(19) . .
Al1 C11 C12 C13 -58.53(16) . .
C10 C11 C12 C16 177.8(2) . .
C15 C11 C12 C16 -6.0(3) . .
Al1 C11 C12 C16 120.0(2) . .
C11 C12 C13 C14 0.0(2) . .
C16 C12 C13 C14 -178.60(19) . .
C11 C12 C13 C17 178.1(2) . .
C16 C12 C13 C17 -0.5(3) . .
C12 C13 C14 C10 0.8(2) . .
C17 C13 C14 C10 -177.2(2) . .
C12 C13 C14 C18 -173.6(2) . .
C17 C13 C14 C18 8.3(3) . .
C12 C13 C14 Al1 58.95(16) . .
C17 C13 C14 Al1 -119.1(2) . .
C11 C10 C14 C13 -1.3(2) . .
Al1 C10 C14 C13 79.04(15) . .
C11 C10 C14 C18 173.28(19) . .
Al1 C10 C14 C18 -106.4(2) . .
C11 C10 C14 Al1 -80.32(15) . .
C1 Al1 C14 C13 34.02(15) . .
C10 Al1 C14 C13 -110.36(18) . .
Cl1 Al1 C14 C13 145.69(12) 2_666 .
Cl1 Al1 C14 C13 -127.38(12) . .
C11 Al1 C14 C13 -68.45(13) . .
C1 Al1 C14 C10 144.38(13) . .
Cl1 Al1 C14 C10 -103.95(12) 2_666 .
Cl1 Al1 C14 C10 -17.02(16) . .
C11 Al1 C14 C10 41.91(12) . .
C1 Al1 C14 C18 -99.52(18) . .
C10 Al1 C14 C18 116.1(2) . .
Cl1 Al1 C14 C18 12.14(17) 2_666 .
Cl1 Al1 C14 C18 99.08(18) . .
C11 Al1 C14 C18 158.0(2) . .
