#------------------------------------------------------------------------------
#$Date: 2020-08-06 15:53:56 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/58/7125892.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_7125892
loop_
_publ_author_name
'Kysliak, Oleksandr'
'Görls, Helmar'
'Kretschmer, Robert'
_publ_section_title
;
 C-F bond activation by pentamethylcyclopentadienyl-aluminium(i): a
 combined experimental/computational exercise.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7865
_journal_page_last               7868
_journal_paper_doi               10.1039/d0cc00003e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C34 H30 Al2 F16'
_chemical_formula_sum            'C34 H30 Al2 F16'
_chemical_formula_weight         796.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-12-12 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                115.809(1)
_cell_angle_beta                 98.981(2)
_cell_angle_gamma                92.895(1)
_cell_formula_units_Z            1
_cell_length_a                   8.4379(2)
_cell_length_b                   9.9671(3)
_cell_length_c                   11.3803(3)
_cell_measurement_reflns_used    11683
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.290
_cell_volume                     843.48(4)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11683
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.290
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0363P)²+0.6240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3365
_reflns_number_total             3838
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc00003e2.cif
_cod_data_source_block           FO6953_4b
_cod_depositor_comments
'Adding full bibliography for 7125888--7125892.cif.'
_cod_database_code               7125892
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.985
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.51625(5) 0.65664(5) 0.09215(4) 0.01581(12) Uani 1 1 d . . . . .
F1 F 0.37863(10) 0.48017(9) 0.02869(8) 0.01790(19) Uani 1 1 d . . . . .
F2 F 0.40025(12) 0.62540(12) 0.33479(10) 0.0283(2) Uani 1 1 d . . . . .
F3 F 0.56493(14) 0.65506(12) 0.56495(10) 0.0324(3) Uani 1 1 d . . . . .
F4 F 1.05526(12) 0.72345(14) 0.43211(11) 0.0372(3) Uani 1 1 d . . . . .
F5 F 0.88833(11) 0.70282(12) 0.20691(10) 0.0292(2) Uani 1 1 d . . . . .
F6 F 0.8235(17) 0.623(3) 0.6859(16) 0.080(4) Uani 0.41(2) 1 d . . P A 1
F7 F 1.0440(16) 0.6392(18) 0.6183(11) 0.076(3) Uani 0.41(2) 1 d . . P A 1
F8 F 0.943(2) 0.8316(18) 0.7292(14) 0.078(4) Uani 0.41(2) 1 d . . P A 1
F6A F 0.8563(10) 0.5792(6) 0.6525(7) 0.0485(15) Uani 0.59(2) 1 d . . P A 2
F7A F 1.0630(7) 0.6897(13) 0.6410(9) 0.067(2) Uani 0.59(2) 1 d . . P A 2
F8A F 0.8884(16) 0.8163(13) 0.7351(7) 0.069(2) Uani 0.59(2) 1 d . . P A 2
C1 C 0.63729(19) 0.66153(17) 0.25989(15) 0.0184(3) Uani 1 1 d . . . . .
C2 C 0.56338(19) 0.65048(17) 0.35656(15) 0.0195(3) Uani 1 1 d . . . . .
C3 C 0.6481(2) 0.66295(18) 0.47588(15) 0.0221(3) Uani 1 1 d . . . . .
C4 C 0.8158(2) 0.68430(18) 0.50477(16) 0.0233(3) Uani 1 1 d . . . . .
C5 C 0.89352(19) 0.69775(19) 0.41072(17) 0.0237(3) Uani 1 1 d . . . . .
C6 C 0.80431(19) 0.68657(18) 0.29322(15) 0.0205(3) Uani 1 1 d . . . . .
C7 C 0.9068(2) 0.6930(2) 0.63378(18) 0.0303(4) Uani 1 1 d . . . . .
C8 C 0.5487(2) 0.91899(17) 0.20150(16) 0.0238(3) Uani 1 1 d . . . . .
C9 C 0.59240(19) 0.86412(18) 0.07493(16) 0.0217(3) Uani 1 1 d . . . . .
C10 C 0.4522(2) 0.77685(17) -0.02394(15) 0.0205(3) Uani 1 1 d . . . . .
C11 C 0.32358(19) 0.77529(18) 0.04320(16) 0.0217(3) Uani 1 1 d . . . . .
C12 C 0.3844(2) 0.86202(18) 0.18283(16) 0.0241(3) Uani 1 1 d . . . . .
C13 C 0.6585(3) 1.0159(2) 0.33324(19) 0.0419(5) Uani 1 1 d . . . . .
H13A H 0.634364 1.119717 0.365801 0.063 Uiso 1 1 calc R U . . .
H13B H 0.771462 1.012868 0.322422 0.063 Uiso 1 1 calc R U . . .
H13C H 0.641454 0.978418 0.397490 0.063 Uiso 1 1 calc R U . . .
C14 C 0.7510(2) 0.8982(2) 0.0429(2) 0.0386(5) Uani 1 1 d . . . . .
H14A H 0.740676 0.970865 0.006539 0.058 Uiso 1 1 calc R U . . .
H14B H 0.780974 0.805330 -0.022886 0.058 Uiso 1 1 calc R U . . .
H14C H 0.834890 0.940526 0.124206 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4412(3) 0.7179(2) -0.17131(17) 0.0345(4) Uani 1 1 d . . . . .
H15A H 0.442767 0.802146 -0.194039 0.052 Uiso 1 1 calc R U . . .
H15B H 0.340132 0.649526 -0.218784 0.052 Uiso 1 1 calc R U . . .
H15C H 0.533389 0.663697 -0.197311 0.052 Uiso 1 1 calc R U . . .
C16 C 0.1514(2) 0.7032(2) -0.0212(2) 0.0377(5) Uani 1 1 d . . . . .
H16A H 0.085450 0.778984 -0.027177 0.057 Uiso 1 1 calc R U . . .
H16B H 0.108432 0.660871 0.032431 0.057 Uiso 1 1 calc R U . . .
H16C H 0.148382 0.622854 -0.110807 0.057 Uiso 1 1 calc R U . . .
C17 C 0.2884(3) 0.8948(3) 0.2910(2) 0.0467(6) Uani 1 1 d . . . . .
H17A H 0.234342 0.983444 0.303677 0.070 Uiso 1 1 calc R U . . .
H17B H 0.361313 0.913989 0.374183 0.070 Uiso 1 1 calc R U . . .
H17C H 0.207034 0.808141 0.265404 0.070 Uiso 1 1 calc R U . . .
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'
F F 0.0171 0.0103 '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
F1 Al1 F1 77.61(4) . 2_665
F1 Al1 C1 99.68(5) . .
F1 Al1 C1 99.36(6) 2_665 .
F1 Al1 C10 111.15(5) . .
F1 Al1 C10 95.55(5) 2_665 .
C1 Al1 C10 147.99(6) . .
F1 Al1 C11 92.89(5) . .
F1 Al1 C11 125.33(5) 2_665 .
C1 Al1 C11 135.24(7) . .
C10 Al1 C11 38.09(6) . .
F1 Al1 C9 149.08(6) . .
F1 Al1 C9 100.37(5) 2_665 .
C1 Al1 C9 111.01(6) . .
C10 Al1 C9 37.94(6) . .
C11 Al1 C9 62.73(6) . .
F1 Al1 C12 111.39(6) . .
F1 Al1 C12 157.66(5) 2_665 .
C1 Al1 C12 99.12(6) . .
C10 Al1 C12 62.25(6) . .
C11 Al1 C12 37.04(6) . .
C9 Al1 C12 61.06(6) . .
F1 Al1 C8 147.06(6) . .
F1 Al1 C8 133.05(6) 2_665 .
C1 Al1 C8 87.94(6) . .
C10 Al1 C8 61.51(6) . .
C11 Al1 C8 61.05(6) . .
C9 Al1 C8 36.09(6) . .
C12 Al1 C8 35.72(6) . .
F1 Al1 Al1 38.87(3) . 2_665
F1 Al1 Al1 38.74(3) 2_665 2_665
C1 Al1 Al1 102.25(5) . 2_665
C10 Al1 Al1 107.06(5) . 2_665
C11 Al1 Al1 113.82(5) . 2_665
C9 Al1 Al1 131.70(5) . 2_665
C12 Al1 Al1 145.89(5) . 2_665
C8 Al1 Al1 167.51(5) . 2_665
Al1 F1 Al1 102.39(4) . 2_665
C6 C1 C2 114.02(14) . .
C6 C1 Al1 122.02(11) . .
C2 C1 Al1 123.83(12) . .
F2 C2 C3 117.19(14) . .
F2 C2 C1 119.35(14) . .
C3 C2 C1 123.46(15) . .
F3 C3 C2 118.91(15) . .
F3 C3 C4 120.05(14) . .
C2 C3 C4 121.04(15) . .
C3 C4 C5 116.92(14) . .
C3 C4 C7 120.47(15) . .
C5 C4 C7 122.62(16) . .
F4 C5 C6 118.68(15) . .
F4 C5 C4 121.06(15) . .
C6 C5 C4 120.25(15) . .
F5 C6 C1 118.75(14) . .
F5 C6 C5 116.98(14) . .
C1 C6 C5 124.27(15) . .
F6A C7 F8A 108.0(5) . .
F6A C7 F7A 104.4(5) . .
F8A C7 F7A 106.8(5) . .
F7 C7 F8 106.0(8) . .
F7 C7 F6 108.8(8) . .
F8 C7 F6 103.7(9) . .
F6A C7 C4 111.5(3) . .
F8A C7 C4 110.9(5) . .
F7 C7 C4 110.9(5) . .
F7A C7 C4 114.8(3) . .
F8 C7 C4 112.9(7) . .
F6 C7 C4 113.9(5) . .
C9 C8 C12 108.21(14) . .
C9 C8 C13 126.08(17) . .
C12 C8 C13 125.68(17) . .
C9 C8 Al1 68.06(9) . .
C12 C8 Al1 70.41(9) . .
C13 C8 Al1 125.50(12) . .
C8 C9 C10 108.06(14) . .
C8 C9 C14 128.04(16) . .
C10 C9 C14 123.72(16) . .
C8 C9 Al1 75.85(9) . .
C10 C9 Al1 68.51(9) . .
C14 C9 Al1 124.88(12) . .
C11 C10 C9 107.73(13) . .
C11 C10 C15 127.16(16) . .
C9 C10 C15 124.59(16) . .
C11 C10 Al1 72.20(9) . .
C9 C10 Al1 73.54(9) . .
C15 C10 Al1 126.37(11) . .
C10 C11 C12 107.81(14) . .
C10 C11 C16 126.32(16) . .
C12 C11 C16 125.78(16) . .
C10 C11 Al1 69.71(9) . .
C12 C11 Al1 74.91(9) . .
C16 C11 Al1 123.73(12) . .
C8 C12 C11 108.15(14) . .
C8 C12 C17 125.82(17) . .
C11 C12 C17 125.95(18) . .
C8 C12 Al1 73.87(9) . .
C11 C12 Al1 68.05(9) . .
C17 C12 Al1 126.34(12) . .
C8 C13 H13A 109.5 . .
C8 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C8 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C9 C14 H14A 109.5 . .
C9 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C9 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C10 C15 H15A 109.5 . .
C10 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C10 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C11 C16 H16A 109.5 . .
C11 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C11 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C12 C17 H17A 109.5 . .
C12 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C12 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 F1 1.8410(9) .
Al1 F1 1.8460(10) 2_665
Al1 C1 1.9987(16) .
Al1 C10 2.1665(16) .
Al1 C11 2.1992(16) .
Al1 C9 2.2329(16) .
Al1 C12 2.2894(16) .
Al1 C8 2.3343(16) .
Al1 Al1 2.8733(9) 2_665
F2 C2 1.3503(18) .
F3 C3 1.3460(18) .
F4 C5 1.3394(19) .
F5 C6 1.3558(18) .
F6 C7 1.334(11) .
F7 C7 1.306(9) .
F8 C7 1.315(14) .
F6A C7 1.305(6) .
F7A C7 1.311(7) .
F8A C7 1.305(10) .
C1 C6 1.381(2) .
C1 C2 1.387(2) .
C2 C3 1.383(2) .
C3 C4 1.385(2) .
C4 C5 1.389(2) .
C4 C7 1.511(2) .
C5 C6 1.384(2) .
C8 C9 1.418(2) .
C8 C12 1.419(2) .
C8 C13 1.501(2) .
C9 C10 1.432(2) .
C9 C14 1.501(2) .
C10 C11 1.425(2) .
C10 C15 1.501(2) .
C11 C12 1.428(2) .
C11 C16 1.506(2) .
C12 C17 1.505(2) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
