#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:09:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178937 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/66/4116682.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_4116682
loop_
_publ_author_name
'Roland A. Fischer'
'Markus M. Schulte'
'Jurij Weiss'
'Laszlo Zsolnai'
'Albrecht Jacobi'
'Gottfried Huttner'
'Gernot Frenking'
'Christian Boehme'
'Sergei F. Vyboishchikov'
_publ_section_title
;
 Transition Metal Coordinated Al(X)L2 and Ga(X)L2 Fragments
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1237
_journal_page_last               1248
_journal_paper_doi               10.1021/ja9716463
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C12 H18 Al Cl N2 O5 W'
_chemical_formula_weight         516.56
_chemical_name_systematic
;                                                                          
       
 ?                                                                         
       
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.990(6)
_cell_length_b                   9.044(3)
_cell_length_c                   15.871(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3443.5(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3777
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    6.937
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_obs          0.0442
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0877
_refine_ls_wR_factor_obs         0.0739
_reflns_number_observed          2457
_reflns_number_total             3777
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9716463_2.cif
_cod_data_source_block           juri
_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'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116682
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
W W 0.338633(14) 0.03142(4) 0.17457(2) 0.01718(9) Uani 1 d .
Al Al 0.40175(9) -0.0173(3) 0.30838(13) 0.0160(5) Uani 1 d .
Cl Cl 0.49179(8) -0.0619(3) 0.30307(13) 0.0301(5) Uani 1 d .
C1 C 0.3517(3) 0.2530(11) 0.1840(5) 0.025(2) Uani 1 d .
C2 C 0.2887(4) 0.0538(10) 0.0740(5) 0.026(2) Uani 1 d .
C3 C 0.2740(4) 0.0459(10) 0.2567(5) 0.024(2) Uani 1 d .
C4 C 0.3246(3) -0.1889(10) 0.1634(5) 0.026(2) Uani 1 d .
C5 C 0.4133(4) 0.0203(10) 0.1150(5) 0.024(2) Uani 1 d .
O1 O 0.3602(3) 0.3778(7) 0.1874(4) 0.041(2) Uani 1 d .
O2 O 0.2596(3) 0.0583(8) 0.0178(4) 0.048(2) Uani 1 d .
O3 O 0.2387(3) 0.0543(7) 0.3053(4) 0.033(2) Uani 1 d .
O4 O 0.3149(3) -0.3118(7) 0.1556(4) 0.041(2) Uani 1 d .
O5 O 0.4565(3) 0.0164(8) 0.0838(4) 0.041(2) Uani 1 d .
N1 N 0.3818(3) -0.1946(7) 0.3856(4) 0.023(2) Uani 1 d .
N2 N 0.4054(3) 0.1412(7) 0.4010(4) 0.0163(14) Uani 1 d .
C6 C 0.3211(3) -0.2072(10) 0.3982(6) 0.028(2) Uani 1 d .
H6A H 0.3028(3) -0.2103(10) 0.3444(6) 0.031(11) Uiso 1 calc R
H6B H 0.3080(3) -0.1233(10) 0.4295(6) 0.031(11) Uiso 1 calc R
H6C H 0.3130(3) -0.2961(10) 0.4288(6) 0.031(11) Uiso 1 calc R
C7 C 0.4005(4) -0.3329(9) 0.3423(6) 0.034(2) Uani 1 d .
H7A H 0.4399(4) -0.3284(9) 0.3326(6) 0.031(11) Uiso 1 calc R
H7B H 0.3814(4) -0.3422(9) 0.2894(6) 0.031(11) Uiso 1 calc R
H7C H 0.3920(4) -0.4167(9) 0.3771(6) 0.031(11) Uiso 1 calc R
C8 C 0.4110(4) -0.1900(9) 0.4682(5) 0.025(2) Uani 1 d .
H8A H 0.4507(4) -0.2012(9) 0.4587(5) 0.016(9) Uiso 1 calc R
H8B H 0.3987(4) -0.2733(9) 0.5019(5) 0.016(9) Uiso 1 calc R
C9 C 0.4011(4) -0.0479(9) 0.5180(5) 0.030(2) Uani 1 d .
H9A H 0.3613(4) -0.0297(9) 0.5208(5) 0.016(9) Uiso 1 calc R
H9B H 0.4143(4) -0.0624(9) 0.5752(5) 0.016(9) Uiso 1 calc R
C10 C 0.4292(4) 0.0880(10) 0.4818(5) 0.022(2) Uani 1 d .
H10A H 0.4269(4) 0.1672(10) 0.5228(5) 0.016(9) Uiso 1 calc R
H10B H 0.4684(4) 0.0660(10) 0.4732(5) 0.016(9) Uiso 1 calc R
C11 C 0.3493(3) 0.2094(9) 0.4159(5) 0.022(2) Uani 1 d .
H11A H 0.3240(3) 0.1354(9) 0.4364(5) 0.024(9) Uiso 1 calc R
H11B H 0.3353(3) 0.2494(9) 0.3640(5) 0.024(9) Uiso 1 calc R
H11C H 0.3527(3) 0.2871(9) 0.4568(5) 0.024(9) Uiso 1 calc R
C12 C 0.4413(3) 0.2619(10) 0.3697(5) 0.023(2) Uani 1 d .
H12A H 0.4268(3) 0.2984(10) 0.3173(5) 0.024(9) Uiso 1 calc R
H12B H 0.4784(3) 0.2251(10) 0.3611(5) 0.024(9) Uiso 1 calc R
H12C H 0.4421(3) 0.3405(10) 0.4103(5) 0.024(9) Uiso 1 calc R
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C2 W C5 99.3(3)
C2 W C4 86.0(4)
C5 W C4 93.3(4)
C2 W C3 92.7(3)
C5 W C3 167.8(3)
C4 W C3 89.6(3)
C2 W C1 93.0(3)
C5 W C1 87.0(3)
C4 W C1 179.0(3)
C3 W C1 90.4(3)
C2 W Al 175.9(3)
C5 W Al 82.0(2)
C4 W Al 90.1(2)
C3 W Al 86.2(2)
C1 W Al 90.9(2)
N2 Al N1 97.3(3)
N2 Al Cl 96.5(2)
N1 Al Cl 96.2(2)
N2 Al W 118.8(2)
N1 Al W 118.1(2)
Cl Al W 124.20(10)
O1 C1 W 177.9(7)
O2 C2 W 176.1(8)
O3 C3 W 177.6(7)
O4 C4 W 177.4(8)
O5 C5 W 177.5(7)
C6 N1 C8 110.3(7)
C6 N1 C7 107.0(7)
C8 N1 C7 106.7(7)
C6 N1 Al 111.6(5)
C8 N1 Al 113.0(5)
C7 N1 Al 107.8(5)
C12 N2 C10 107.8(6)
C12 N2 C11 105.8(6)
C10 N2 C11 110.0(6)
C12 N2 Al 107.4(5)
C10 N2 Al 114.1(5)
C11 N2 Al 111.2(5)
N1 C8 C9 114.0(7)
C10 C9 C8 114.6(7)
N2 C10 C9 114.7(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W C2 2.007(8)
W C5 2.029(9)
W C4 2.028(9)
W C3 2.030(9)
W C1 2.033(10)
W Al 2.645(2)
Al N2 2.055(7)
Al N1 2.074(7)
Al Cl 2.199(3)
C1 O1 1.149(11)
C2 O2 1.134(10)
C3 O3 1.147(10)
C4 O4 1.143(9)
C5 O5 1.148(10)
N1 C6 1.475(11)
N1 C8 1.487(10)
N1 C7 1.495(10)
N2 C12 1.477(10)
N2 C10 1.484(9)
N2 C11 1.499(10)
C8 C9 1.527(11)
C9 C10 1.515(11)
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
C2 W Al N2 -133.8(36)
C5 W Al N2 117.3(4)
C4 W Al N2 -149.4(3)
C3 W Al N2 -59.8(3)
C1 W Al N2 30.5(3)
C2 W Al N1 -16.5(36)
C5 W Al N1 -125.5(4)
C4 W Al N1 -32.2(3)
C3 W Al N1 57.4(3)
C1 W Al N1 147.7(3)
C2 W Al Cl 104.2(36)
C5 W Al Cl -4.8(3)
C4 W Al Cl 88.5(3)
C3 W Al Cl 178.1(3)
C1 W Al Cl -91.6(3)
C2 W C1 O1 -78.3(214)
C5 W C1 O1 20.9(214)
C4 W C1 O1 -82.6(300)
C3 W C1 O1 -171.0(214)
Al W C1 O1 102.8(214)
C5 W C2 O2 104.5(115)
C4 W C2 O2 11.8(115)
C3 W C2 O2 -77.6(115)
C1 W C2 O2 -168.1(115)
Al W C2 O2 -3.9(148)
C2 W C3 O3 -171.3(199)
C5 W C3 O3 -0.9(210)
C4 W C3 O3 102.7(199)
C1 W C3 O3 -78.3(199)
Al W C3 O3 12.6(198)
C2 W C4 O4 -23.4(169)
C5 W C4 O4 -122.6(169)
C3 W C4 O4 69.3(169)
C1 W C4 O4 -19.1(323)
Al W C4 O4 155.5(169)
C2 W C5 O5 149.4(198)
C4 W C5 O5 -124.1(198)
C3 W C5 O5 -20.8(210)
C1 W C5 O5 56.9(198)
Al W C5 O5 -34.4(198)
N2 Al N1 C6 87.0(6)
Cl Al N1 C6 -175.5(5)
W Al N1 C6 -41.2(6)
N2 Al N1 C8 -38.0(6)
Cl Al N1 C8 59.4(6)
W Al N1 C8 -166.2(5)
N2 Al N1 C7 -155.7(5)
Cl Al N1 C7 -58.3(6)
W Al N1 C7 76.0(6)
N1 Al N2 C12 156.3(5)
Cl Al N2 C12 59.2(5)
W Al N2 C12 -75.9(5)
N1 Al N2 C10 36.9(6)
Cl Al N2 C10 -60.2(5)
W Al N2 C10 164.7(5)
N1 Al N2 C11 -88.3(5)
Cl Al N2 C11 174.6(5)
W Al N2 C11 39.5(5)
C6 N1 C8 C9 -69.5(9)
C7 N1 C8 C9 174.5(7)
Al N1 C8 C9 56.2(9)
N1 C8 C9 C10 -70.9(10)
C12 N2 C10 C9 -173.5(7)
C11 N2 C10 C9 71.6(8)
Al N2 C10 C9 -54.3(8)
C8 C9 C10 N2 69.5(10)
