#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:10:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179526 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/23/4342310.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_4342310
loop_
_publ_author_name
'Erickson, Jeremy D.'
'Fettinger, James C.'
'Power, Philip P.'
_publ_section_title
;
 Reaction of a germylene, stannylene, or plumbylene with trimethylaluminum
 and trimethylgallium: insertion into Al-C or ga-C bonds, a reversible
 metal-carbon insertion equilibrium, and a new route to diplumbenes.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1940
_journal_page_last               1948
_journal_paper_doi               10.1021/ic502824w
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C26 H31 Al'
_chemical_formula_sum            'C26 H31 Al'
_chemical_formula_weight         370.49
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.1406(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1913(6)
_cell_length_b                   9.7004(4)
_cell_length_c                   16.6409(7)
_cell_measurement_reflns_used    7149
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      71.73
_cell_measurement_theta_min      5.54
_cell_volume                     2271.41(16)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2013.6-2) (Bruker, 2013)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.111
_diffrn_reflns_theta_min         5.539
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.93169
_exptl_absorpt_correction_T_min  0.75356
_exptl_absorpt_correction_type   Multi-scan,TWINABS
_exptl_absorpt_process_details   'TWINABS V2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       Block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0392
_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)+(0.0589P)²+1.4526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1929
_reflns_number_total             2063
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic502824w_si_002.cif
_cod_data_source_block           JE26FF
_cod_depositor_comments
'Adding full bibliography for 4342304--4342310.cif.'
_cod_database_code               4342310
#BEGIN Tags that were not found in dictionaries:
_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   0.898
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Al1 Al 0.0000 0.45253(6) 0.2500 0.02976(19) Uani 1 2 d S T P
C1 C 0.04732(12) 0.35406(16) 0.17265(11) 0.0426(4) Uani 1 1 d . . .
H1A H 0.0479 0.2549 0.1840 0.064 Uiso 1 1 calc R U .
H1B H 0.1120 0.3852 0.1826 0.064 Uiso 1 1 calc R U .
H1C H 0.0059 0.3725 0.1123 0.064 Uiso 1 1 calc R U .
C2 C 0.0000 0.65559(19) 0.2500 0.0271(4) Uani 1 2 d S T P
C3 C 0.08209(9) 0.72911(14) 0.29977(8) 0.0276(3) Uani 1 1 d . . .
C4 C 0.08178(9) 0.87276(14) 0.29988(9) 0.0315(3) Uani 1 1 d . . .
H4 H 0.1374 0.9219 0.3340 0.038 Uiso 1 1 calc R U .
C5 C 0.0000 0.9442(2) 0.2500 0.0341(5) Uani 1 2 d S T P
H5 H 0.0000 1.0421 0.2500 0.041 Uiso 1 2 calc R U P
C6 C 0.16781(9) 0.64548(14) 0.35097(8) 0.0286(3) Uani 1 1 d . . .
C7 C 0.23484(9) 0.61036(14) 0.31466(9) 0.0312(3) Uani 1 1 d . . .
C8 C 0.31023(10) 0.52401(15) 0.36058(10) 0.0359(3) Uani 1 1 d . . .
H8 H 0.3565 0.5030 0.3368 0.043 Uiso 1 1 calc R U .
C9 C 0.31981(11) 0.46761(15) 0.44033(10) 0.0381(4) Uani 1 1 d . . .
C10 C 0.25273(11) 0.50298(16) 0.47486(9) 0.0376(4) Uani 1 1 d . . .
H10 H 0.2581 0.4648 0.5291 0.045 Uiso 1 1 calc R U .
C11 C 0.17773(10) 0.59253(15) 0.43263(9) 0.0326(3) Uani 1 1 d . . .
C12 C 0.22422(11) 0.66327(16) 0.22621(10) 0.0385(4) Uani 1 1 d . . .
H12A H 0.2759 0.6270 0.2107 0.058 Uiso 1 1 calc R U .
H12B H 0.2267 0.7642 0.2273 0.058 Uiso 1 1 calc R U .
H12C H 0.1631 0.6329 0.1832 0.058 Uiso 1 1 calc R U .
C13 C 0.40016(12) 0.37032(19) 0.48783(13) 0.0532(5) Uani 1 1 d . . .
H13A H 0.4395 0.4104 0.5440 0.080 Uiso 1 1 calc R U .
H13B H 0.4391 0.3552 0.4532 0.080 Uiso 1 1 calc R U .
H13C H 0.3741 0.2821 0.4972 0.080 Uiso 1 1 calc R U .
C14 C 0.11059(11) 0.63403(18) 0.47595(10) 0.0411(4) Uani 1 1 d . . .
H14A H 0.1160 0.5685 0.5224 0.062 Uiso 1 1 calc R U .
H14B H 0.0452 0.6338 0.4331 0.062 Uiso 1 1 calc R U .
H14C H 0.1269 0.7267 0.5005 0.062 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 0.0181 0.0091 '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 0.2130 0.2455 '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 C1 121.18(10) . 2
C1 Al1 C2 119.41(5) . .
C1 Al1 C2 119.41(5) 2 .
Al1 C1 H1A 109.5 . .
Al1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Al1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 C3 118.94(17) . 2
C3 C2 Al1 120.53(8) . .
C3 C2 Al1 120.53(8) 2 .
C4 C3 C2 120.40(12) . .
C4 C3 C6 122.92(12) . .
C2 C3 C6 116.68(12) . .
C5 C4 C3 119.99(13) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C4 120.27(18) . 2
C4 C5 H5 119.9 . .
C4 C5 H5 119.9 2 .
C11 C6 C7 119.66(13) . .
C11 C6 C3 120.05(12) . .
C7 C6 C3 120.10(12) . .
C8 C7 C6 119.25(13) . .
C8 C7 C12 120.23(13) . .
C6 C7 C12 120.51(12) . .
C9 C8 C7 121.93(14) . .
C9 C8 H8 119.0 . .
C7 C8 H8 119.0 . .
C10 C9 C8 117.92(13) . .
C10 C9 C13 120.84(15) . .
C8 C9 C13 121.24(15) . .
C9 C10 C11 122.23(14) . .
C9 C10 H10 118.9 . .
C11 C10 H10 118.9 . .
C10 C11 C6 118.96(13) . .
C10 C11 C14 119.78(13) . .
C6 C11 C14 121.24(13) . .
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 . .
C9 C13 H13A 109.5 . .
C9 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C9 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 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 1.9450(15) .
Al1 C1 1.9450(15) 2
Al1 C2 1.9698(19) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.4039(16) .
C2 C3 1.4040(16) 2
C3 C4 1.394(2) .
C3 C6 1.4979(18) .
C4 C5 1.3911(17) .
C4 H4 0.9500 .
C5 C4 1.3911(17) 2
C5 H5 0.9500 .
C6 C11 1.407(2) .
C6 C7 1.4076(19) .
C7 C8 1.392(2) .
C7 C12 1.509(2) .
C8 C9 1.391(2) .
C8 H8 0.9500 .
C9 C10 1.388(2) .
C9 C13 1.509(2) .
C10 C11 1.394(2) .
C10 H10 0.9500 .
C11 C14 1.509(2) .
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 .
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
C3 C2 C3 C4 0.22(8) 2 .
Al1 C2 C3 C4 -179.78(8) . .
C3 C2 C3 C6 -179.46(12) 2 .
Al1 C2 C3 C6 0.54(12) . .
C2 C3 C4 C5 -0.43(17) . .
C6 C3 C4 C5 179.22(10) . .
C3 C4 C5 C4 0.21(8) . 2
C4 C3 C6 C11 97.20(16) . .
C2 C3 C6 C11 -83.14(14) . .
C4 C3 C6 C7 -87.89(16) . .
C2 C3 C6 C7 91.78(14) . .
C11 C6 C7 C8 -0.3(2) . .
C3 C6 C7 C8 -175.21(12) . .
C11 C6 C7 C12 178.53(12) . .
C3 C6 C7 C12 3.6(2) . .
C6 C7 C8 C9 2.1(2) . .
C12 C7 C8 C9 -176.74(13) . .
C7 C8 C9 C10 -1.7(2) . .
C7 C8 C9 C13 177.89(14) . .
C8 C9 C10 C11 -0.4(2) . .
C13 C9 C10 C11 179.98(14) . .
C9 C10 C11 C6 2.1(2) . .
C9 C10 C11 C14 -176.20(14) . .
C7 C6 C11 C10 -1.7(2) . .
C3 C6 C11 C10 173.20(12) . .
C7 C6 C11 C14 176.53(13) . .
C3 C6 C11 C14 -8.5(2) . .
