#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:34:44 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178905 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/34/4113450.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_4113450
loop_
_publ_author_name
'Vojtech Jancik'
'Ying Peng'
'Herbert W. Roesky'
'Jiyang Li'
'Dante Neculai'
'Ana M. Neculai'
'Regine Herbst-Irmer'
_publ_section_title
;
 The First Structurally Characterized Aluminum Compound with Two SH
 Groups: [LAl(SH)2] (L = N(Ar)C(Me)CHC(Me)N(Ar), Ar = 2,6-i-Pr2C6H3) and
 the Catalytic Properties of the Sulfur P(NMe2)3 System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1452
_journal_page_last               1453
_journal_paper_doi               10.1021/ja028801k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C29 H43 Al N2 S2'
_chemical_formula_weight         510.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.685(2)
_cell_length_b                   22.058(3)
_cell_length_c                   10.448(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2923.4(8)
_computing_cell_refinement       saint
_computing_data_collection       saint
_computing_data_reduction        sadabs
_computing_molecular_graphics    xp
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  '3-circle goniometer ccd detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13243
_diffrn_reflns_theta_full        59.61
_diffrn_reflns_theta_max         59.61
_diffrn_reflns_theta_min         4.68
_diffrn_source                   'rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.8196
_exptl_absorpt_correction_T_min  0.5660
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2190
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0403P)²+1.8819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                2008
_reflns_number_total             2190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028801k_s2.cif
_cod_data_source_block           als
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2923.5(10)
_cod_database_code               4113450
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.12443(5) 0.7500 0.11131(5) 0.02381(18) Uani 1 2 d SD
N1 N 0.06360(10) 0.68565(6) 0.40436(12) 0.0169(3) Uani 1 1 d .
S2 S 0.30756(5) 0.7500 0.36579(6) 0.02883(19) Uani 1 2 d SD
C5 C 0.08588(12) 0.58158(7) 0.31916(16) 0.0201(4) Uani 1 1 d .
Al1 Al 0.13629(5) 0.7500 0.32361(6) 0.01608(18) Uani 1 2 d S
C6 C 0.12524(13) 0.52329(8) 0.33715(17) 0.0254(4) Uani 1 1 d .
H6 H 0.1114 0.4931 0.2745 0.030 Uiso 1 1 calc R
C2 C -0.03339(12) 0.69336(8) 0.45334(15) 0.0196(4) Uani 1 1 d .
C3 C -0.07993(18) 0.7500 0.4684(2) 0.0207(5) Uani 1 2 d S
H3 H -0.1523 0.7500 0.4919 0.025 Uiso 1 2 calc SR
C11 C 0.02035(14) 0.59479(8) 0.20092(15) 0.0242(4) Uani 1 1 d .
H11 H -0.0048 0.6377 0.2061 0.029 Uiso 1 1 calc R
C4 C 0.10797(12) 0.62503(7) 0.41342(15) 0.0189(4) Uani 1 1 d .
C8 C 0.20518(13) 0.55172(8) 0.53461(17) 0.0263(4) Uani 1 1 d .
H8 H 0.2452 0.5410 0.6080 0.032 Uiso 1 1 calc R
C7 C 0.18377(13) 0.50828(8) 0.44360(18) 0.0275(4) Uani 1 1 d .
H7 H 0.2093 0.4681 0.4542 0.033 Uiso 1 1 calc R
C9 C 0.16947(13) 0.61099(8) 0.52146(16) 0.0218(4) Uani 1 1 d .
C1 C -0.09654(14) 0.63946(8) 0.49621(18) 0.0284(4) Uani 1 1 d .
H1A H -0.1160 0.6150 0.4216 0.043 Uiso 1 1 calc R
H1B H -0.1605 0.6533 0.5399 0.043 Uiso 1 1 calc R
H1C H -0.0543 0.6149 0.5552 0.043 Uiso 1 1 calc R
C10 C 0.19537(15) 0.65722(8) 0.62469(16) 0.0283(4) Uani 1 1 d .
H10 H 0.1768 0.6982 0.5907 0.034 Uiso 1 1 calc R
C13 C 0.08648(16) 0.58804(9) 0.07899(17) 0.0347(5) Uani 1 1 d .
H13A H 0.1488 0.6141 0.0848 0.052 Uiso 1 1 calc R
H13B H 0.0442 0.5999 0.0046 0.052 Uiso 1 1 calc R
H13C H 0.1087 0.5457 0.0696 0.052 Uiso 1 1 calc R
C15 C 0.31301(16) 0.65748(9) 0.6570(2) 0.0386(5) Uani 1 1 d .
H15A H 0.3320 0.6191 0.6983 0.058 Uiso 1 1 calc R
H15B H 0.3284 0.6912 0.7151 0.058 Uiso 1 1 calc R
H15C H 0.3541 0.6623 0.5782 0.058 Uiso 1 1 calc R
C12 C -0.07620(15) 0.55337(9) 0.19082(19) 0.0371(5) Uani 1 1 d .
H12A H -0.0531 0.5114 0.1777 0.056 Uiso 1 1 calc R
H12B H -0.1199 0.5662 0.1183 0.056 Uiso 1 1 calc R
H12C H -0.1174 0.5560 0.2700 0.056 Uiso 1 1 calc R
C14 C 0.13008(18) 0.64660(11) 0.7455(2) 0.0486(6) Uani 1 1 d .
H14A H 0.0550 0.6501 0.7249 0.073 Uiso 1 1 calc R
H14B H 0.1488 0.6769 0.8102 0.073 Uiso 1 1 calc R
H14C H 0.1446 0.6059 0.7790 0.073 Uiso 1 1 calc R
H1 H 0.0297(18) 0.7500 0.105(3) 0.036(8) Uiso 1 2 d SD
H2 H 0.328(3) 0.7500 0.253(3) 0.073(11) Uiso 1 2 d SD
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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 '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
C2 N1 C4 116.49(13) . .
C2 N1 Al1 121.44(11) . .
C4 N1 Al1 122.05(10) . .
C6 C5 C4 117.69(15) . .
C6 C5 C11 118.93(15) . .
C4 C5 C11 123.37(15) . .
N1 Al1 N1 97.27(8) . 7_575
N1 Al1 S2 112.90(5) . .
N1 Al1 S2 112.90(5) 7_575 .
N1 Al1 S1 114.34(5) . .
N1 Al1 S1 114.34(4) 7_575 .
S2 Al1 S1 105.35(3) . .
C7 C6 C5 121.63(16) . .
N1 C2 C3 123.06(16) . .
N1 C2 C1 120.14(15) . .
C3 C2 C1 116.80(15) . .
C2 C3 C2 127.9(2) 7_575 .
C5 C11 C12 112.32(15) . .
C5 C11 C13 111.00(14) . .
C12 C11 C13 108.81(15) . .
C5 C4 C9 121.60(15) . .
C5 C4 N1 120.36(14) . .
C9 C4 N1 118.00(14) . .
C7 C8 C9 121.45(17) . .
C8 C7 C6 119.77(16) . .
C8 C9 C4 117.84(16) . .
C8 C9 C10 119.35(15) . .
C4 C9 C10 122.79(15) . .
C9 C10 C14 111.48(15) . .
C9 C10 C15 111.71(15) . .
C14 C10 C15 110.31(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 Al1 2.2232(9) .
N1 C2 1.343(2) .
N1 C4 1.454(2) .
N1 Al1 1.8912(14) .
S2 Al1 2.2169(9) .
C5 C6 1.392(2) .
C5 C4 1.403(2) .
C5 C11 1.517(2) .
Al1 N1 1.8912(14) 7_575
C6 C7 1.378(3) .
C2 C3 1.3908(19) .
C2 C1 1.502(2) .
C3 C2 1.3908(19) 7_575
C11 C12 1.532(3) .
C11 C13 1.533(2) .
C4 C9 1.407(2) .
C8 C7 1.377(3) .
C8 C9 1.391(2) .
C9 C10 1.520(2) .
C10 C14 1.528(3) .
C10 C15 1.530(3) .
