#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:48:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178535 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/41/4064116.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_4064116
loop_
_publ_author_name
'Burlakov, Vladimir V.'
'Kaleta, Katharina'
'Beweries, Torsten'
'Arndt, Perdita'
'Baumann, Wolfgang'
'Spannenberg, Anke'
'Shur, Vladimir B.'
'Rosenthal, Uwe'
_publ_section_title
;
 Reactions of Five-Membered Metallacyclocumulenes Cp2M(η4-t-Bu-C4-t-Bu)
 (M = Ti, Zr) with Diisobutylaluminum Hydride
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1157
_journal_paper_doi               10.1021/om1011374
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C48 H96 Al4'
_chemical_formula_weight         781.17
_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                112.794(3)
_cell_angle_beta                 104.407(3)
_cell_angle_gamma                90.464(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1515(4)
_cell_length_b                   11.5730(5)
_cell_length_c                   14.0031(6)
_cell_measurement_reflns_used    6574
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.83
_cell_volume                     1315.16(11)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       ω
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21815
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.7351
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6033
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0595
_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)+(0.1116P)²+0.1035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                4418
_reflns_number_total             6033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1011374_si_003.cif
_cod_data_source_block           ks1095
_cod_original_cell_volume        1315.15(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064116
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.74228(7) 1.08373(6) 0.28503(5) 0.03039(18) Uani 1 1 d . . .
Al2 Al 0.49365(6) 1.10521(5) 0.08997(5) 0.02453(17) Uani 1 1 d . . .
C1 C 0.4415(2) 0.91094(18) 0.04459(16) 0.0249(4) Uani 1 1 d . . .
C2 C 0.5741(2) 0.89544(17) 0.10626(16) 0.0246(4) Uani 1 1 d . . .
C3 C 0.7043(2) 0.90332(19) 0.16923(17) 0.0282(4) Uani 1 1 d . . .
C4 C 0.8232(2) 0.8121(2) 0.1595(2) 0.0357(5) Uani 1 1 d . B .
H4A H 0.9248 0.8617 0.1899 0.043 Uiso 1 1 calc R . .
H4B H 0.8116 0.7615 0.0820 0.043 Uiso 1 1 calc R . .
C5 C 0.8190(3) 0.7219(3) 0.2142(2) 0.0620(9) Uani 1 1 d D . .
C9 C 0.2899(2) 0.8509(2) 0.04762(19) 0.0320(5) Uani 1 1 d . . .
C10 C 0.2878(3) 0.8848(3) 0.1636(2) 0.0561(7) Uani 1 1 d . . .
H10A H 0.3750 0.8546 0.2001 0.084 Uiso 1 1 calc R . .
H10B H 0.1936 0.8451 0.1646 0.084 Uiso 1 1 calc R . .
H10C H 0.2935 0.9767 0.2009 0.084 Uiso 1 1 calc R . .
C11 C 0.2786(3) 0.7080(3) -0.0122(3) 0.0565(8) Uani 1 1 d . . .
H11A H 0.2788 0.6872 -0.0870 0.085 Uiso 1 1 calc R . .
H11B H 0.1843 0.6687 -0.0109 0.085 Uiso 1 1 calc R . .
H11C H 0.3656 0.6762 0.0229 0.085 Uiso 1 1 calc R . .
C12 C 0.1539(3) 0.8968(3) -0.0096(3) 0.0479(6) Uani 1 1 d . . .
H12A H 0.1561 0.9880 0.0294 0.072 Uiso 1 1 calc R . .
H12B H 0.0599 0.8534 -0.0119 0.072 Uiso 1 1 calc R . .
H12C H 0.1582 0.8785 -0.0832 0.072 Uiso 1 1 calc R . .
C13 C 0.9611(3) 1.1405(2) 0.3261(2) 0.0416(5) Uani 1 1 d . . .
H13A H 1.0148 1.0886 0.3626 0.050 Uiso 1 1 calc R . .
H13B H 0.9911 1.1185 0.2585 0.050 Uiso 1 1 calc R . .
C14 C 1.0245(3) 1.2780(3) 0.3974(2) 0.0452(6) Uani 1 1 d . . .
H14 H 0.9914 1.3029 0.4649 0.054 Uiso 1 1 calc R . .
C15 C 0.9624(4) 1.3652(3) 0.3420(3) 0.0652(8) Uani 1 1 d . . .
H15A H 0.9904 1.3405 0.2742 0.098 Uiso 1 1 calc R . .
H15B H 1.0056 1.4525 0.3891 0.098 Uiso 1 1 calc R . .
H15C H 0.8515 1.3584 0.3271 0.098 Uiso 1 1 calc R . .
C16 C 1.1982(3) 1.2966(4) 0.4290(3) 0.0631(8) Uani 1 1 d . . .
H16A H 1.2330 1.2814 0.3648 0.095 Uiso 1 1 calc R . .
H16B H 1.2379 1.2372 0.4605 0.095 Uiso 1 1 calc R . .
H16C H 1.2348 1.3832 0.4818 0.095 Uiso 1 1 calc R . .
C17 C 0.6219(3) 1.1150(3) 0.3891(2) 0.0497(6) Uani 1 1 d . A .
H17A H 0.5285 1.1488 0.3626 0.060 Uiso 1 1 calc R . .
H17B H 0.5898 1.0325 0.3879 0.060 Uiso 1 1 calc R . .
C18 C 0.6933(3) 1.2029(3) 0.5053(2) 0.0554(7) Uani 1 1 d D . .
H18A H 0.8029 1.1908 0.5261 0.067 Uiso 0.726(8) 1 calc PR A 1
H18B H 0.7635 1.2778 0.5192 0.067 Uiso 0.274(8) 1 calc PR A 2
C21 C 0.3383(2) 1.2166(2) 0.12795(19) 0.0329(5) Uani 1 1 d . . .
H21A H 0.2460 1.1863 0.0663 0.039 Uiso 1 1 calc R . .
H21B H 0.3117 1.2080 0.1894 0.039 Uiso 1 1 calc R . .
C22 C 0.3799(3) 1.3576(2) 0.1581(2) 0.0395(5) Uani 1 1 d . . .
H22 H 0.4268 1.3651 0.1031 0.047 Uiso 1 1 calc R . .
C23 C 0.4955(3) 1.4177(3) 0.2670(3) 0.0585(8) Uani 1 1 d . . .
H23A H 0.4556 1.4045 0.3212 0.088 Uiso 1 1 calc R . .
H23B H 0.5155 1.5084 0.2864 0.088 Uiso 1 1 calc R . .
H23C H 0.5900 1.3791 0.2638 0.088 Uiso 1 1 calc R . .
C24 C 0.2398(4) 1.4289(3) 0.1575(3) 0.0576(8) Uani 1 1 d . . .
H24A H 0.1935 1.4250 0.2124 0.086 Uiso 1 1 calc R . .
H24B H 0.1661 1.3902 0.0865 0.086 Uiso 1 1 calc R . .
H24C H 0.2700 1.5173 0.1732 0.086 Uiso 1 1 calc R . .
H1 H 0.648(3) 1.146(2) 0.195(2) 0.032(6) Uiso 1 1 d . . .
C6A C 0.6730(5) 0.6297(5) 0.1458(5) 0.0528(17) Uiso 0.547(11) 1 d PD B 1
H6A1 H 0.6616 0.5686 0.1769 0.079 Uiso 0.547(11) 1 calc PR B 1
H6A2 H 0.6800 0.5849 0.0719 0.079 Uiso 0.547(11) 1 calc PR B 1
H6A3 H 0.5848 0.6771 0.1451 0.079 Uiso 0.547(11) 1 calc PR B 1
C7A C 0.9624(6) 0.6536(7) 0.2153(7) 0.0568(19) Uiso 0.547(11) 1 d PD B 1
H7A1 H 0.9599 0.5962 0.2512 0.085 Uiso 0.547(11) 1 calc PR B 1
H7A2 H 1.0527 0.7159 0.2542 0.085 Uiso 0.547(11) 1 calc PR B 1
H7A3 H 0.9662 0.6053 0.1411 0.085 Uiso 0.547(11) 1 calc PR B 1
C8A C 0.8030(10) 0.7767(8) 0.3296(4) 0.073(2) Uiso 0.547(11) 1 d PD B 1
H8A1 H 0.7998 0.7087 0.3546 0.109 Uiso 0.547(11) 1 calc PR B 1
H8A2 H 0.7091 0.8166 0.3307 0.109 Uiso 0.547(11) 1 calc PR B 1
H8A3 H 0.8901 0.8397 0.3770 0.109 Uiso 0.547(11) 1 calc PR B 1
C6B C 0.6656(6) 0.6571(9) 0.2044(10) 0.081(3) Uiso 0.453(11) 1 d PD B 2
H6B1 H 0.6824 0.6027 0.2442 0.121 Uiso 0.453(11) 1 calc PR B 2
H6B2 H 0.6151 0.6058 0.1284 0.121 Uiso 0.453(11) 1 calc PR B 2
H6B3 H 0.6015 0.7213 0.2344 0.121 Uiso 0.453(11) 1 calc PR B 2
C7B C 0.9358(8) 0.6289(6) 0.1838(7) 0.0448(18) Uiso 0.453(11) 1 d PD B 2
H7B1 H 0.9365 0.5698 0.2185 0.067 Uiso 0.453(11) 1 calc PR B 2
H7B2 H 1.0370 0.6759 0.2082 0.067 Uiso 0.453(11) 1 calc PR B 2
H7B3 H 0.9083 0.5820 0.1055 0.067 Uiso 0.453(11) 1 calc PR B 2
C8B C 0.8731(11) 0.8120(7) 0.3345(4) 0.069(2) Uiso 0.453(11) 1 d PD B 2
H8B1 H 0.8759 0.7638 0.3789 0.103 Uiso 0.453(11) 1 calc PR B 2
H8B2 H 0.8027 0.8757 0.3507 0.103 Uiso 0.453(11) 1 calc PR B 2
H8B3 H 0.9750 0.8538 0.3501 0.103 Uiso 0.453(11) 1 calc PR B 2
C19A C 0.6806(5) 1.3389(4) 0.5123(4) 0.0581(13) Uiso 0.726(8) 1 d PD A 1
H19A H 0.7266 1.3991 0.5865 0.087 Uiso 0.726(8) 1 calc PR A 1
H19B H 0.5733 1.3504 0.4903 0.087 Uiso 0.726(8) 1 calc PR A 1
H19C H 0.7338 1.3532 0.4645 0.087 Uiso 0.726(8) 1 calc PR A 1
C20A C 0.6154(6) 1.1867(6) 0.5857(4) 0.0654(14) Uiso 0.726(8) 1 d PD A 1
H20A H 0.6685 1.2462 0.6589 0.098 Uiso 0.726(8) 1 calc PR A 1
H20B H 0.6188 1.1002 0.5813 0.098 Uiso 0.726(8) 1 calc PR A 1
H20C H 0.5094 1.2034 0.5681 0.098 Uiso 0.726(8) 1 calc PR A 1
C19B C 0.7651(19) 1.0953(12) 0.5325(15) 0.096(6) Uiso 0.274(8) 1 d PD A 2
H19D H 0.8232 1.1289 0.6085 0.144 Uiso 0.274(8) 1 calc PR A 2
H19E H 0.8331 1.0587 0.4873 0.144 Uiso 0.274(8) 1 calc PR A 2
H19F H 0.6848 1.0299 0.5191 0.144 Uiso 0.274(8) 1 calc PR A 2
C20B C 0.5837(12) 1.2231(12) 0.5767(8) 0.051(3) Uiso 0.274(8) 1 d PD A 2
H20D H 0.6361 1.2804 0.6508 0.077 Uiso 0.274(8) 1 calc PR A 2
H20E H 0.5499 1.1419 0.5754 0.077 Uiso 0.274(8) 1 calc PR A 2
H20F H 0.4954 1.2599 0.5491 0.077 Uiso 0.274(8) 1 calc PR A 2
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'
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
C17 Al1 C13 123.69(12) . .
C17 Al1 C3 114.46(11) . .
C13 Al1 C3 107.72(10) . .
C21 Al2 C1 117.50(9) . 2_675
C21 Al2 C1 118.45(9) . .
C1 Al2 C1 96.29(7) 2_675 .
C21 Al2 Al2 134.68(8) . 2_675
C1 Al2 Al2 48.84(6) 2_675 2_675
C1 Al2 Al2 47.45(6) . 2_675
C2 C1 C9 117.91(17) . .
C2 C1 Al2 100.26(13) . 2_675
C9 C1 Al2 126.97(15) . 2_675
C2 C1 Al2 96.01(13) . .
C9 C1 Al2 123.68(13) . .
Al2 C1 Al2 83.71(7) 2_675 .
C3 C2 C1 169.1(2) . .
C2 C3 C4 130.6(2) . .
C2 C3 Al1 105.26(14) . .
C4 C3 Al1 123.58(16) . .
C3 C4 C5 116.07(18) . .
C4 C5 C8A 117.8(4) . .
C4 C5 C6B 119.6(4) . .
C8A C5 C6B 75.9(5) . .
C4 C5 C7A 109.6(3) . .
C8A C5 C7A 107.6(4) . .
C6B C5 C7A 121.7(5) . .
C4 C5 C7B 107.5(3) . .
C8A C5 C7B 120.5(5) . .
C6B C5 C7B 113.3(5) . .
C4 C5 C8B 101.8(4) . .
C6B C5 C8B 103.3(5) . .
C7A C5 C8B 94.8(5) . .
C7B C5 C8B 110.6(5) . .
C4 C5 C6A 104.6(3) . .
C8A C5 C6A 105.1(4) . .
C7A C5 C6A 112.1(4) . .
C7B C5 C6A 98.2(4) . .
C8B C5 C6A 132.5(4) . .
C10 C9 C12 109.6(2) . .
C10 C9 C11 110.2(2) . .
C12 C9 C11 108.0(2) . .
C10 C9 C1 110.12(19) . .
C12 C9 C1 110.50(17) . .
C11 C9 C1 108.37(18) . .
C14 C13 Al1 121.30(18) . .
C13 C14 C16 111.9(2) . .
C13 C14 C15 111.2(2) . .
C16 C14 C15 109.4(2) . .
C18 C17 Al1 118.84(19) . .
C17 C18 C20A 114.4(3) . .
C17 C18 C20B 113.2(5) . .
C17 C18 C19B 92.2(7) . .
C20A C18 C19B 74.3(7) . .
C20B C18 C19B 94.9(9) . .
C17 C18 C19A 106.8(3) . .
C20A C18 C19A 107.7(3) . .
C20B C18 C19A 89.3(6) . .
C19B C18 C19A 157.1(8) . .
C22 C21 Al2 116.72(15) . .
C23 C22 C24 110.0(2) . .
C23 C22 C21 110.9(2) . .
C24 C22 C21 111.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 C17 1.966(3) .
Al1 C13 1.971(2) .
Al1 C3 2.048(2) .
Al2 C21 1.960(2) .
Al2 C1 2.055(2) 2_675
Al2 C1 2.100(2) .
Al2 Al2 2.7728(12) 2_675
C1 C2 1.361(3) .
C1 C9 1.564(3) .
C1 Al2 2.055(2) 2_675
C2 C3 1.272(3) .
C3 C4 1.516(3) .
C4 C5 1.521(3) .
C5 C8A 1.535(3) .
C5 C6B 1.536(3) .
C5 C7A 1.538(3) .
C5 C7B 1.540(3) .
C5 C8B 1.544(3) .
C5 C6A 1.546(3) .
C9 C10 1.521(4) .
C9 C12 1.522(3) .
C9 C11 1.526(3) .
C13 C14 1.527(4) .
C14 C16 1.529(4) .
C14 C15 1.530(4) .
C17 C18 1.513(4) .
C18 C20A 1.540(3) .
C18 C20B 1.542(4) .
C18 C19B 1.545(4) .
C18 C19A 1.545(3) .
C21 C22 1.537(3) .
C22 C23 1.513(4) .
C22 C24 1.531(3) .
