#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:10:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179526 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/23/4342309.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_4342309
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         'C75 H84 Sn5'
_chemical_formula_sum            'C75 H84 Sn5'
_chemical_formula_weight         1578.97
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.1973(9)
_cell_length_b                   13.1973(9)
_cell_length_c                   22.4007(15)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.55
_cell_volume                     3378.8(4)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2013.6-2) (Bruker, 2013)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.782
_exptl_absorpt_coefficient_mu    1.862
_exptl_absorpt_correction_T_max  0.4697
_exptl_absorpt_correction_T_min  0.3266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.748
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2663
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0407P)²+3.1193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2422
_reflns_number_total             2663
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic502824w_si_002.cif
_cod_data_source_block           je22fmi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4342304--4342310.cif.
;
_cod_original_cell_volume        3378.8(5)
_cod_database_code               4342309
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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   0.493
_shelx_estimated_absorpt_t_max   0.833
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Sn2 Sn 0.47265(2) 0.26784(2) 0.7500 0.01940(8) Uani 1 2 d S T P
Sn1 Sn 0.6667 0.3333 0.67215(2) 0.01951(9) Uani 1 3 d S T P
C1 C 0.3438(3) 0.0824(3) 0.7500 0.0308(7) Uani 1 2 d S T P
H1A H 0.385(3) 0.039(3) 0.7500 0.017(9) Uiso 1 2 d S . P
H1B H 0.292(3) 0.059(3) 0.7842(14) 0.041(9) Uiso 1 1 d . . .
C2 C 0.3770(3) 0.3640(3) 0.7500 0.0218(6) Uani 1 2 d S T P
C3 C 0.3439(2) 0.3934(2) 0.80412(10) 0.0234(5) Uani 1 1 d . . .
C4 C 0.2819(2) 0.4540(2) 0.80350(11) 0.0279(5) Uani 1 1 d . . .
H4 H 0.266(3) 0.478(3) 0.8396(15) 0.035(8) Uiso 1 1 d . . .
C5 C 0.2513(3) 0.4848(3) 0.7500 0.0306(7) Uani 1 2 d S T P
H5 H 0.207(4) 0.526(4) 0.7500 0.047(13) Uiso 1 2 d S . P
C6 C 0.3641(2) 0.3504(2) 0.86263(10) 0.0238(5) Uani 1 1 d . . .
C7 C 0.2805(2) 0.2364(2) 0.88141(11) 0.0292(5) Uani 1 1 d . . .
C8 C 0.3005(3) 0.1921(2) 0.93365(12) 0.0339(6) Uani 1 1 d . . .
H8 H 0.245(3) 0.116(3) 0.9458(15) 0.037(8) Uiso 1 1 d . . .
C9 C 0.3993(3) 0.2571(2) 0.96848(12) 0.0339(6) Uani 1 1 d . . .
C10 C 0.4782(2) 0.3707(2) 0.95065(11) 0.0305(5) Uani 1 1 d . . .
H10 H 0.543(3) 0.416(3) 0.9752(14) 0.035(8) Uiso 1 1 d . . .
C11 C 0.4624(2) 0.4191(2) 0.89816(10) 0.0250(5) Uani 1 1 d . . .
C12 C 0.1680(2) 0.1661(2) 0.84715(14) 0.0386(6) Uani 1 1 d D . .
H12A H 0.125(2) 0.0877(10) 0.8647(11) 0.062(11) Uiso 1 1 d D . .
H12B H 0.182(3) 0.160(2) 0.8046(3) 0.055(10) Uiso 1 1 d D . .
H12C H 0.122(2) 0.206(2) 0.8519(12) 0.063(12) Uiso 1 1 d D . .
C13 C 0.4178(4) 0.2070(3) 1.02556(14) 0.0445(7) Uani 1 1 d . . .
H13A H 0.505(3) 0.261(3) 1.0360(16) 0.040(9) Uiso 1 1 d . . .
H13B H 0.399(3) 0.130(3) 1.0166(17) 0.053(10) Uiso 1 1 d . . .
H13C H 0.370(4) 0.211(4) 1.057(2) 0.078(14) Uiso 1 1 d . . .
C14 C 0.5510(2) 0.5427(2) 0.88085(12) 0.0314(5) Uani 1 1 d D . .
H14A H 0.601(2) 0.545(3) 0.8479(8) 0.077(14) Uiso 1 1 d D . .
H14B H 0.6060(18) 0.594(2) 0.9112(10) 0.063(11) Uiso 1 1 d D . .
H14C H 0.514(3) 0.586(2) 0.8658(12) 0.084(15) Uiso 1 1 d D . .
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'
Sn Sn -0.6537 1.4246 '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 Sn2 C2 107.41(14) . .
C1 Sn2 Sn1 114.83(8) . 12_667
C2 Sn2 Sn1 120.94(6) . 12_667
C1 Sn2 Sn1 114.83(8) . 11_657
C2 Sn2 Sn1 120.94(6) . 11_657
Sn1 Sn2 Sn1 0.000(8) 12_667 11_657
C1 Sn2 Sn1 114.83(8) . 10_557
C2 Sn2 Sn1 120.94(6) . 10_557
Sn1 Sn2 Sn1 0.000(8) 12_667 10_557
Sn1 Sn2 Sn1 0.000(8) 11_657 10_557
C1 Sn2 Sn1 114.83(8) . .
C2 Sn2 Sn1 120.94(6) . .
Sn1 Sn2 Sn1 75.406(11) 12_667 .
Sn1 Sn2 Sn1 75.406(11) 11_657 .
Sn1 Sn2 Sn1 75.406(11) 10_557 .
Sn2 Sn1 Sn2 86.501(8) 2_655 3_665
Sn2 Sn1 Sn2 86.501(8) 2_655 .
Sn2 Sn1 Sn2 86.501(8) 3_665 .
Sn2 C1 H1A 108(2) . .
Sn2 C1 H1B 113(2) . .
H1A C1 H1B 109(2) . .
C3 C2 C3 119.0(3) 10_557 .
C3 C2 Sn2 120.48(15) 10_557 .
C3 C2 Sn2 120.48(15) . .
C4 C3 C2 119.9(2) . .
C4 C3 C6 119.3(2) . .
C2 C3 C6 120.6(2) . .
C5 C4 C3 120.9(2) . .
C5 C4 H4 120(2) . .
C3 C4 H4 119(2) . .
C4 C5 C4 119.3(3) 10_557 .
C4 C5 H5 120.32(17) 10_557 .
C4 C5 H5 120.33(17) . .
C11 C6 C7 119.9(2) . .
C11 C6 C3 122.1(2) . .
C7 C6 C3 118.0(2) . .
C8 C7 C6 119.1(2) . .
C8 C7 C12 120.3(2) . .
C6 C7 C12 120.5(2) . .
C9 C8 C7 122.0(3) . .
C9 C8 H8 119(2) . .
C7 C8 H8 119(2) . .
C8 C9 C10 118.1(2) . .
C8 C9 C13 120.8(3) . .
C10 C9 C13 121.1(3) . .
C9 C10 C11 122.1(3) . .
C9 C10 H10 118(2) . .
C11 C10 H10 120(2) . .
C6 C11 C10 118.8(2) . .
C6 C11 C14 121.4(2) . .
C10 C11 C14 119.8(2) . .
C7 C12 H12A 108(2) . .
C7 C12 H12B 112(2) . .
H12A C12 H12B 109.7(11) . .
C7 C12 H12C 107.2(19) . .
H12A C12 H12C 109.7(12) . .
H12B C12 H12C 109.6(12) . .
C9 C13 H13A 105(2) . .
C9 C13 H13B 106(2) . .
H13A C13 H13B 113(3) . .
C9 C13 H13C 109(3) . .
H13A C13 H13C 110(4) . .
H13B C13 H13C 113(4) . .
C11 C14 H14A 112(2) . .
C11 C14 H14B 119(2) . .
H14A C14 H14B 104.3(14) . .
C11 C14 H14C 112(2) . .
H14A C14 H14C 104.3(14) . .
H14B C14 H14C 104.3(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn2 C1 2.172(4) .
Sn2 C2 2.193(3) .
Sn2 Sn1 2.8515(3) 12_667
Sn2 Sn1 2.8515(3) 11_657
Sn2 Sn1 2.8515(3) 10_557
Sn2 Sn1 2.8515(3) .
Sn1 Sn2 2.8515(3) 2_655
Sn1 Sn2 2.8515(3) 3_665
C1 H1A 0.97(4) .
C1 H1B 0.97(3) .
C2 C3 1.407(3) 10_557
C2 C3 1.407(3) .
C3 C4 1.401(3) .
C3 C6 1.504(3) .
C4 C5 1.388(3) .
C4 H4 0.93(3) .
C5 C4 1.388(3) 10_557
C5 H5 0.97(5) .
C6 C11 1.401(4) .
C6 C7 1.413(3) .
C7 C8 1.392(4) .
C7 C12 1.509(4) .
C8 C9 1.387(4) .
C8 H8 0.94(4) .
C9 C10 1.389(4) .
C9 C13 1.514(4) .
C10 C11 1.402(3) .
C10 H10 0.94(3) .
C11 C14 1.506(4) .
C12 H12A 0.980(2) .
C12 H12B 0.980(2) .
C12 H12C 0.980(2) .
C13 H13A 1.04(4) .
C13 H13B 0.94(4) .
C13 H13C 0.96(5) .
C14 H14A 0.980(2) .
C14 H14B 0.980(2) .
C14 H14C 0.980(2) .
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 -1.9(5) 10_557 .
Sn2 C2 C3 C4 -179.48(19) . .
C3 C2 C3 C6 172.23(18) 10_557 .
Sn2 C2 C3 C6 -5.4(3) . .
C2 C3 C4 C5 0.7(4) . .
C6 C3 C4 C5 -173.5(3) . .
C3 C4 C5 C4 0.5(5) . 10_557
C4 C3 C6 C11 -89.3(3) . .
C2 C3 C6 C11 96.5(3) . .
C4 C3 C6 C7 91.0(3) . .
C2 C3 C6 C7 -83.2(3) . .
C11 C6 C7 C8 -3.3(4) . .
C3 C6 C7 C8 176.4(2) . .
C11 C6 C7 C12 173.5(2) . .
C3 C6 C7 C12 -6.9(3) . .
C6 C7 C8 C9 1.1(4) . .
C12 C7 C8 C9 -175.7(3) . .
C7 C8 C9 C10 1.5(4) . .
C7 C8 C9 C13 179.2(3) . .
C8 C9 C10 C11 -2.0(4) . .
C13 C9 C10 C11 -179.6(3) . .
C7 C6 C11 C10 2.8(3) . .
C3 C6 C11 C10 -176.8(2) . .
C7 C6 C11 C14 -177.6(2) . .
C3 C6 C11 C14 2.8(3) . .
C9 C10 C11 C6 -0.2(4) . .
C9 C10 C11 C14 -179.8(2) . .
