#------------------------------------------------------------------------------
#$Date: 2019-12-06 11:36:51 +0200 (Fri, 06 Dec 2019) $
#$Revision: 244930 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556433.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_1556433
loop_
_publ_author_name
'Yang, X.'
'Lunsford, A.'
'Darensbourg, M.Y.'
_publ_section_title
;
 Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via
 the N2S2 Metallo-Ligand Strategy
;
_journal_name_full               Inorganics
_journal_page_first              115
_journal_paper_doi               10.3390/inorganics7090115
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C10 H21 Al N2 S2'
_chemical_formula_sum            'C10 H21 Al N2 S2'
_chemical_formula_weight         260.39
_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
_cell_angle_alpha                94.767(7)
_cell_angle_beta                 98.204(7)
_cell_angle_gamma                115.566(6)
_cell_formula_units_Z            2
_cell_length_a                   7.354(4)
_cell_length_b                   7.723(4)
_cell_length_c                   12.601(6)
_cell_measurement_reflns_used    6296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.99
_cell_measurement_theta_min      3.31
_cell_volume                     630.5(6)
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.1270
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6296
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       needle
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   10
_exptl_transmission_factor_min   -18
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.104
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1437
_reflns_number_total             2333
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            AlMeN2S2.cif
_cod_data_source_block           mo_AlMe_0m
_cod_original_cell_volume        630.6(5)
_cod_database_code               1556433
_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   0.977
_shelx_estimated_absorpt_t_max   0.991
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
S1 S 0.3717(2) -0.0625(2) 0.79646(13) 0.0357(5) Uani 1 1 d . . . . .
S2 S 0.4699(2) 0.2666(2) 0.61992(11) 0.0308(4) Uani 1 1 d . . . . .
Al1 Al 0.6479(2) 0.2065(2) 0.76583(12) 0.0211(4) Uani 1 1 d . . . . .
C4 C 1.0813(8) 0.3668(8) 0.7681(4) 0.0297(14) Uani 1 1 d . . . . .
H4A H 1.1199 0.4971 0.8086 0.036 Uiso 1 1 calc R U . . .
H4B H 1.1964 0.3744 0.7333 0.036 Uiso 1 1 calc R U . . .
C2 C 0.9122(9) -0.0073(8) 0.6411(4) 0.0372(15) Uani 1 1 d . . . . .
H2 H 1.0018 -0.0522 0.6152 0.045 Uiso 1 1 calc R U . . .
C3 C 0.8727(8) 0.1491(7) 0.5981(4) 0.0299(14) Uani 1 1 d . . . . .
H3A H 0.7322 0.0901 0.5531 0.036 Uiso 1 1 calc R U . . .
H3B H 0.9707 0.2092 0.5503 0.036 Uiso 1 1 calc R U . . .
C1 C 0.7996(8) -0.0874(8) 0.7283(4) 0.0379(15) Uani 1 1 d . . . . .
H1A H 0.6519 -0.1666 0.6957 0.045 Uiso 1 1 calc R U . . .
H1B H 0.8511 -0.1745 0.7602 0.045 Uiso 1 1 calc R U . . .
N2 N 0.8919(6) 0.3046(5) 0.6840(3) 0.0203(10) Uani 1 1 d . . . . .
C10 C 0.7407(8) 0.4205(7) 0.8883(4) 0.0288(13) Uani 1 1 d . . . . .
H10A H 0.7951 0.3848 0.9540 0.043 Uiso 1 1 calc R U . . .
H10B H 0.6243 0.4448 0.9003 0.043 Uiso 1 1 calc R U . . .
H10C H 0.8487 0.5384 0.8715 0.043 Uiso 1 1 calc R U . . .
C7 C 0.5147(8) -0.1643(8) 0.8786(5) 0.0359(15) Uani 1 1 d . . . . .
H7A H 0.4589 -0.1941 0.9454 0.043 Uiso 1 1 calc R U . . .
H7B H 0.4956 -0.2877 0.8373 0.043 Uiso 1 1 calc R U . . .
C8 C 0.8895(8) 0.4722(7) 0.6345(4) 0.0299(14) Uani 1 1 d . . . . .
H8A H 1.0025 0.5228 0.5939 0.036 Uiso 1 1 calc R U . . .
H8B H 0.9109 0.5779 0.6923 0.036 Uiso 1 1 calc R U . . .
C9 C 0.6835(8) 0.4076(8) 0.5576(4) 0.0318(14) Uani 1 1 d . . . . .
H9A H 0.6785 0.3282 0.4904 0.038 Uiso 1 1 calc R U . . .
H9B H 0.6708 0.5236 0.5373 0.038 Uiso 1 1 calc R U . . .
C6 C 0.7414(9) -0.0270(8) 0.9096(5) 0.0397(16) Uani 1 1 d . . . . .
H6A H 0.7650 0.0767 0.9693 0.048 Uiso 1 1 calc R U . . .
H6B H 0.8175 -0.0989 0.9362 0.048 Uiso 1 1 calc R U . . .
C5 C 1.0380(8) 0.2140(8) 0.8483(4) 0.0355(15) Uani 1 1 d . . . . .
H5A H 1.1317 0.1530 0.8461 0.043 Uiso 1 1 calc R U . . .
H5B H 1.0628 0.2797 0.9235 0.043 Uiso 1 1 calc R U . . .
N1 N 0.8208(6) 0.0627(6) 0.8153(3) 0.0262(11) Uani 1 1 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
C7 S1 Al1 98.15(19) . .
C9 S2 Al1 99.04(17) . .
C10 Al1 N2 102.2(2) . .
C10 Al1 N1 102.2(2) . .
N2 Al1 N1 74.85(17) . .
C10 Al1 S2 109.41(16) . .
N2 Al1 S2 85.21(12) . .
N1 Al1 S2 145.51(15) . .
C10 Al1 S1 109.84(17) . .
N2 Al1 S1 145.26(13) . .
N1 Al1 S1 85.40(14) . .
S2 Al1 S1 96.23(8) . .
N2 C4 C5 108.6(4) . .
N2 C4 H4A 110.0 . .
C5 C4 H4A 110.0 . .
N2 C4 H4B 110.0 . .
C5 C4 H4B 110.0 . .
H4A C4 H4B 108.3 . .
C3 C2 C1 114.2(5) . .
C3 C2 H2 122.9 . .
C1 C2 H2 122.9 . .
C2 C3 N2 114.0(4) . .
C2 C3 H3A 108.8 . .
N2 C3 H3A 108.8 . .
C2 C3 H3B 108.8 . .
N2 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
N1 C1 C2 113.5(5) . .
N1 C1 H1A 108.9 . .
C2 C1 H1A 108.9 . .
N1 C1 H1B 108.9 . .
C2 C1 H1B 108.9 . .
H1A C1 H1B 107.7 . .
C3 N2 C4 110.7(4) . .
C3 N2 C8 110.2(4) . .
C4 N2 C8 111.2(4) . .
C3 N2 Al1 111.7(3) . .
C4 N2 Al1 105.9(3) . .
C8 N2 Al1 106.9(3) . .
Al1 C10 H10A 109.5 . .
Al1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Al1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C6 C7 S1 112.1(4) . .
C6 C7 H7A 109.2 . .
S1 C7 H7A 109.2 . .
C6 C7 H7B 109.2 . .
S1 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
N2 C8 C9 109.8(4) . .
N2 C8 H8A 109.7 . .
C9 C8 H8A 109.7 . .
N2 C8 H8B 109.7 . .
C9 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
C8 C9 S2 111.4(4) . .
C8 C9 H9A 109.4 . .
S2 C9 H9A 109.4 . .
C8 C9 H9B 109.4 . .
S2 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
N1 C6 C7 111.2(5) . .
N1 C6 H6A 109.4 . .
C7 C6 H6A 109.4 . .
N1 C6 H6B 109.4 . .
C7 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
N1 C5 C4 109.0(4) . .
N1 C5 H5A 109.9 . .
C4 C5 H5A 109.9 . .
N1 C5 H5B 109.9 . .
C4 C5 H5B 109.9 . .
H5A C5 H5B 108.3 . .
C1 N1 C5 110.8(4) . .
C1 N1 C6 110.4(4) . .
C5 N1 C6 111.3(4) . .
C1 N1 Al1 111.9(3) . .
C5 N1 Al1 106.5(3) . .
C6 N1 Al1 105.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C7 1.826(5) .
S1 Al1 2.303(2) .
S2 C9 1.813(5) .
S2 Al1 2.300(2) .
Al1 C10 1.970(5) .
Al1 N2 2.084(4) .
Al1 N1 2.085(4) .
C4 N2 1.487(6) .
C4 C5 1.575(7) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C2 C3 1.484(7) .
C2 C1 1.484(7) .
C2 H2 0.9500 .
C3 N2 1.493(6) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C1 N1 1.468(6) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
N2 C8 1.488(6) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C7 C6 1.508(7) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.527(6) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C6 N1 1.490(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C5 N1 1.486(6) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 C2 C3 N2 48.8(6) . . . .
C3 C2 C1 N1 -49.6(6) . . . .
C2 C3 N2 C4 45.8(6) . . . .
C2 C3 N2 C8 169.3(4) . . . .
C2 C3 N2 Al1 -72.0(5) . . . .
C5 C4 N2 C3 -79.9(5) . . . .
C5 C4 N2 C8 157.1(4) . . . .
C5 C4 N2 Al1 41.3(4) . . . .
Al1 S1 C7 C6 9.2(4) . . . .
C3 N2 C8 C9 62.9(5) . . . .
C4 N2 C8 C9 -174.0(4) . . . .
Al1 N2 C8 C9 -58.7(4) . . . .
N2 C8 C9 S2 47.0(5) . . . .
Al1 S2 C9 C8 -13.6(4) . . . .
S1 C7 C6 N1 -44.0(6) . . . .
N2 C4 C5 N1 -1.9(5) . . . .
C2 C1 N1 C5 -44.7(6) . . . .
C2 C1 N1 C6 -168.5(4) . . . .
C2 C1 N1 Al1 74.0(5) . . . .
C4 C5 N1 C1 83.5(5) . . . .
C4 C5 N1 C6 -153.3(4) . . . .
C4 C5 N1 Al1 -38.4(4) . . . .
C7 C6 N1 C1 -62.7(6) . . . .
C7 C6 N1 C5 173.8(4) . . . .
C7 C6 N1 Al1 58.5(5) . . . .
