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#$Date: 2020-08-06 15:53:56 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/58/7125890.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_7125890
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         'C32 H34 Al2 F8'
_chemical_formula_sum            'C32 H34 Al2 F8'
_chemical_formula_weight         624.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 99.315(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1825(4)
_cell_length_b                   10.7930(5)
_cell_length_c                   14.8825(7)
_cell_measurement_reflns_used    16706
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.479
_cell_measurement_theta_min      2.774
_cell_volume                     1455.51(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16706
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.774
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5539
_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    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0582
_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)+(0.0344P)²+1.8975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2837
_reflns_number_total             3318
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc00003e2.cif
_cod_data_source_block           FO6981_4e
_cod_depositor_comments
'Adding full bibliography for 7125888--7125892.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7125890
_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   0.982
_shelx_estimated_absorpt_t_max   0.985
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_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 0.51588(7) 0.39165(6) 0.44552(5) 0.02262(18) Uani 1 1 d . . . . .
F1 F 0.48020(14) 0.55966(12) 0.43460(8) 0.0247(3) Uani 1 1 d . . . . .
F2 F 0.26349(18) 0.43272(15) 0.27813(10) 0.0420(4) Uani 1 1 d . . . . .
F3 F 0.34221(16) 0.19955(13) 0.54892(10) 0.0373(4) Uani 1 1 d . . . . .
F4 F -0.0112(4) 0.3161(4) 0.2445(3) 0.0464(13) Uani 0.405(4) 1 d . . P A 1
F4A F 0.0649(3) 0.1087(2) 0.5002(2) 0.0433(8) Uani 0.595(4) 1 d . . P A 2
C1 C 0.3132(3) 0.3217(2) 0.41561(17) 0.0274(5) Uani 1 1 d . . . . .
C2 C 0.2178(3) 0.3490(2) 0.33649(18) 0.0334(6) Uani 1 1 d . . . . .
C3 C 0.0783(3) 0.2984(3) 0.3123(2) 0.0451(7) Uani 1 1 d . . . . .
H3A H 0.018914 0.320149 0.256165 0.054 Uiso 0.405(4) 1 calc R U P A 2
C4 C 0.0267(3) 0.2159(3) 0.3707(2) 0.0463(8) Uani 1 1 d . . . . .
H4A H -0.069705 0.181809 0.356350 0.056 Uiso 1 1 calc R U . . .
C5 C 0.1168(3) 0.1844(3) 0.4492(2) 0.0426(7) Uani 1 1 d . . . . .
H5A H 0.083668 0.127012 0.489903 0.051 Uiso 0.595(4) 1 calc R U P A 1
C6 C 0.2564(3) 0.2356(2) 0.47002(18) 0.0311(5) Uani 1 1 d . . . . .
C7 C 0.6018(2) 0.2158(2) 0.37151(16) 0.0256(5) Uani 1 1 d . . . . .
C8 C 0.6769(2) 0.2317(2) 0.46156(15) 0.0246(5) Uani 1 1 d . . . . .
C9 C 0.7491(2) 0.3504(2) 0.46682(15) 0.0241(5) Uani 1 1 d . . . . .
C10 C 0.7128(2) 0.4080(2) 0.38010(15) 0.0246(5) Uani 1 1 d . . . . .
C11 C 0.6205(3) 0.3250(2) 0.32141(16) 0.0260(5) Uani 1 1 d . . . . .
C12 C 0.5112(3) 0.1043(2) 0.33768(19) 0.0344(6) Uani 1 1 d . . . . .
H12A H 0.574827 0.030952 0.341887 0.052 Uiso 1 1 calc R U . . .
H12B H 0.465935 0.117387 0.274108 0.052 Uiso 1 1 calc R U . . .
H12C H 0.433692 0.091874 0.374980 0.052 Uiso 1 1 calc R U . . .
C13 C 0.6899(3) 0.1391(2) 0.53808(18) 0.0338(6) Uani 1 1 d . . . . .
H13A H 0.789855 0.104311 0.548665 0.051 Uiso 1 1 calc R U . . .
H13B H 0.618141 0.072334 0.521804 0.051 Uiso 1 1 calc R U . . .
H13C H 0.670298 0.180247 0.593570 0.051 Uiso 1 1 calc R U . . .
C14 C 0.8559(3) 0.3948(2) 0.54697(17) 0.0300(5) Uani 1 1 d . . . . .
H14A H 0.946306 0.345225 0.552898 0.045 Uiso 1 1 calc R U . . .
H14B H 0.811644 0.386266 0.602335 0.045 Uiso 1 1 calc R U . . .
H14C H 0.879577 0.482065 0.538229 0.045 Uiso 1 1 calc R U . . .
C15 C 0.7686(3) 0.5307(2) 0.35143(18) 0.0318(5) Uani 1 1 d . . . . .
H15A H 0.856481 0.517194 0.323059 0.048 Uiso 1 1 calc R U . . .
H15B H 0.794012 0.584032 0.404950 0.048 Uiso 1 1 calc R U . . .
H15C H 0.691731 0.570596 0.307616 0.048 Uiso 1 1 calc R U . . .
C16 C 0.5641(3) 0.3478(3) 0.22269(17) 0.0370(6) Uani 1 1 d . . . . .
H16A H 0.640853 0.326409 0.186633 0.056 Uiso 1 1 calc R U . . .
H16B H 0.537998 0.435485 0.213560 0.056 Uiso 1 1 calc R U . . .
H16C H 0.476581 0.296583 0.203261 0.056 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 77.39(7) . 3_666
F1 Al1 C1 101.93(8) . .
F1 Al1 C1 101.21(8) 3_666 .
F1 Al1 C9 111.92(8) . .
F1 Al1 C9 93.03(8) 3_666 .
C1 Al1 C9 145.43(10) . .
F1 Al1 C10 91.67(8) . .
F1 Al1 C10 120.98(8) 3_666 .
C1 Al1 C10 137.62(10) . .
C9 Al1 C10 38.13(9) . .
F1 Al1 C8 149.72(8) . .
F1 Al1 C8 101.79(7) 3_666 .
C1 Al1 C8 107.82(9) . .
C9 Al1 C8 37.89(8) . .
C10 Al1 C8 62.38(8) . .
F1 Al1 C11 108.91(8) . .
F1 Al1 C11 154.69(8) 3_666 .
C1 Al1 C11 101.31(9) . .
C9 Al1 C11 61.73(8) . .
C10 Al1 C11 36.70(8) . .
C8 Al1 C11 60.07(8) . .
F1 Al1 C7 143.75(8) . .
F1 Al1 C7 135.35(8) 3_666 .
C1 Al1 C7 87.85(9) . .
C9 Al1 C7 60.71(8) . .
C10 Al1 C7 60.18(8) . .
C8 Al1 C7 35.27(8) . .
C11 Al1 C7 34.96(8) . .
F1 Al1 Al1 38.82(4) . 3_666
F1 Al1 Al1 38.58(4) 3_666 3_666
C1 Al1 Al1 104.88(7) . 3_666
C9 Al1 Al1 105.81(7) . 3_666
C10 Al1 Al1 110.44(7) . 3_666
C8 Al1 Al1 133.09(7) . 3_666
C11 Al1 Al1 141.97(7) . 3_666
C7 Al1 Al1 166.48(7) . 3_666
Al1 F1 Al1 102.60(7) . 3_666
C2 C1 C6 113.2(2) . .
C2 C1 Al1 123.43(19) . .
C6 C1 Al1 123.29(18) . .
F2 C2 C1 117.8(2) . .
F2 C2 C3 117.5(2) . .
C1 C2 C3 124.7(3) . .
F4 C3 C4 111.8(3) . .
F4 C3 C2 129.0(4) . .
C4 C3 C2 119.2(3) . .
C4 C3 H3A 120.4 . .
C2 C3 H3A 120.4 . .
C5 C4 C3 118.6(3) . .
C5 C4 H4A 120.7 . .
C3 C4 H4A 120.7 . .
F4A C5 C4 116.3(3) . .
F4A C5 C6 123.4(3) . .
C4 C5 C6 120.3(3) . .
C4 C5 H5A 119.8 . .
C6 C5 H5A 119.8 . .
F3 C6 C5 117.7(2) . .
F3 C6 C1 118.4(2) . .
C5 C6 C1 123.9(3) . .
C8 C7 C11 108.4(2) . .
C8 C7 C12 125.0(2) . .
C11 C7 C12 126.6(2) . .
C8 C7 Al1 67.31(12) . .
C11 C7 Al1 70.14(13) . .
C12 C7 Al1 125.71(16) . .
C7 C8 C9 108.0(2) . .
C7 C8 C13 127.1(2) . .
C9 C8 C13 124.8(2) . .
C7 C8 Al1 77.42(13) . .
C9 C8 Al1 67.26(12) . .
C13 C8 Al1 123.88(16) . .
C10 C9 C8 107.6(2) . .
C10 C9 C14 127.6(2) . .
C8 C9 C14 124.5(2) . .
C10 C9 Al1 72.27(13) . .
C8 C9 Al1 74.85(13) . .
C14 C9 Al1 123.88(16) . .
C9 C10 C11 108.0(2) . .
C9 C10 C15 126.9(2) . .
C11 C10 C15 125.0(2) . .
C9 C10 Al1 69.60(13) . .
C11 C10 Al1 76.77(13) . .
C15 C10 Al1 122.62(16) . .
C7 C11 C10 108.0(2) . .
C7 C11 C16 126.9(2) . .
C10 C11 C16 124.9(2) . .
C7 C11 Al1 74.90(13) . .
C10 C11 Al1 66.53(12) . .
C16 C11 Al1 127.27(17) . .
C7 C12 H12A 109.5 . .
C7 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C7 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 F1 1.8452(14) .
Al1 F1 1.8545(14) 3_666
Al1 C1 1.991(2) .
Al1 C9 2.160(2) .
Al1 C10 2.195(2) .
Al1 C8 2.261(2) .
Al1 C11 2.330(2) .
Al1 C7 2.391(2) .
Al1 Al1 2.8875(13) 3_666
F2 C2 1.366(3) .
F3 C6 1.361(3) .
F4 C3 1.209(5) .
F4A C5 1.260(4) .
C1 C2 1.381(4) .
C1 C6 1.388(4) .
C2 C3 1.386(4) .
C3 C4 1.381(5) .
C3 H3A 0.9500 .
C4 C5 1.361(4) .
C4 H4A 0.9500 .
C5 C6 1.385(4) .
C5 H5A 0.9500 .
C7 C8 1.415(3) .
C7 C11 1.419(3) .
C7 C12 1.503(3) .
C8 C9 1.438(3) .
C8 C13 1.506(3) .
C9 C10 1.423(3) .
C9 C14 1.495(3) .
C10 C11 1.430(3) .
C10 C15 1.506(3) .
C11 C16 1.497(3) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
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 .
