#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:03:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179522 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/19/4341944.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_4341944
loop_
_publ_author_name
'Czympiel, Lisa'
'Pfrommer, Johannes'
'Tyrra, Wieland'
'Schäfer, Mathias'
'Mathur, Sanjay'
_publ_section_title
;
 Ligand-Modulated Chemical and Structural Implications in Four-, Five-,
 and Six-fold Coordinated Aluminum Heteroaryl Alkenolates.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              25
_journal_page_last               37
_journal_paper_doi               10.1021/ic502549m
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C32 H28 Al2 F12 N4 O5 S4'
_chemical_formula_sum            'C32 H28 Al2 F12 N4 O5 S4'
_chemical_formula_weight         958.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.469(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6761(18)
_cell_length_b                   26.194(6)
_cell_length_c                   15.456(3)
_cell_measurement_reflns_used    13683
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.3
_cell_measurement_theta_min      3.1
_cell_volume                     4099.6(14)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       'ω and φ scans'
_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  0.1814
_diffrn_reflns_av_sigmaI/netI    0.2688
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20735
_diffrn_reflns_theta_full        29.64
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.8336
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001)
was performed after optimizing the crystal shape
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.675
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.675
_refine_ls_R_factor_all          0.2439
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0146P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                1303
_reflns_number_total             5514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502549m_si_002.cif
_cod_data_source_block           Al{DMTTFP}2O
_cod_depositor_comments
'Adding full bibliography for 4341940--4341945.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341944
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.36142(13) 0.18188(4) 0.12794(10) 0.0598(4) Uani 1 1 d .
S2 S 0.39278(16) 0.52994(4) 0.10590(11) 0.0727(5) Uani 1 1 d .
Al1 Al 0.39988(13) 0.35559(5) 0.14075(10) 0.0426(4) Uani 1 1 d .
F1 F 0.5142(3) 0.34535(12) -0.1119(2) 0.0909(11) Uani 1 1 d .
F2 F 0.5602(3) 0.26697(13) -0.1059(2) 0.1043(12) Uani 1 1 d .
F3 F 0.6843(3) 0.31891(15) -0.0114(2) 0.1088(12) Uani 1 1 d .
F4 F -0.0410(3) 0.37381(17) 0.0004(3) 0.1483(19) Uani 1 1 d .
F5 F -0.0601(3) 0.44245(14) 0.0642(3) 0.1209(15) Uani 1 1 d .
F6 F -0.0134(4) 0.37460(18) 0.1390(4) 0.150(2) Uani 1 1 d .
O1 O 0.4632(3) 0.34243(10) 0.0484(2) 0.0469(8) Uani 1 1 d .
O2 O 0.2256(3) 0.36825(10) 0.1067(2) 0.0540(9) Uani 1 1 d .
O3 O 0.5000 0.35667(14) 0.2500 0.0430(11) Uani 1 2 d S
N1 N 0.3523(3) 0.27864(12) 0.1456(3) 0.0422(10) Uani 1 1 d .
N2 N 0.4314(3) 0.43339(12) 0.1211(3) 0.0451(11) Uani 1 1 d .
C1 C 0.2996(4) 0.25663(16) 0.2096(3) 0.0443(12) Uani 1 1 d .
C2 C 0.3017(5) 0.20520(18) 0.2108(3) 0.0517(13) Uani 1 1 d .
C3 C 0.2465(5) 0.28942(17) 0.2689(4) 0.0630(16) Uani 1 1 d .
H3A H 0.2549 0.3247 0.2547 0.094 Uiso 1 1 calc R
H3B H 0.2954 0.2832 0.3317 0.094 Uiso 1 1 calc R
H3C H 0.1551 0.2814 0.2583 0.094 Uiso 1 1 calc R
C4 C 0.2634(5) 0.17063(17) 0.2758(4) 0.0767(18) Uani 1 1 d .
H4A H 0.2754 0.1357 0.2613 0.115 Uiso 1 1 calc R
H4B H 0.1725 0.1763 0.2706 0.115 Uiso 1 1 calc R
H4C H 0.3179 0.1778 0.3371 0.115 Uiso 1 1 calc R
C5 C 0.3883(4) 0.24311(15) 0.0970(4) 0.0458(13) Uani 1 1 d .
C6 C 0.4486(4) 0.25288(16) 0.0278(3) 0.0518(14) Uani 1 1 d .
H6 H 0.4647 0.2257 -0.0059 0.062 Uiso 1 1 calc R
C7 C 0.4820(5) 0.29978(18) 0.0107(3) 0.0478(13) Uani 1 1 d .
C8 C 0.5594(6) 0.3073(2) -0.0539(4) 0.0641(16) Uani 1 1 d .
C9 C 0.5531(5) 0.45685(15) 0.1322(3) 0.0474(13) Uani 1 1 d .
C10 C 0.5490(5) 0.50897(15) 0.1253(4) 0.0605(15) Uani 1 1 d .
C11 C 0.6736(5) 0.42432(15) 0.1487(4) 0.0627(16) Uani 1 1 d .
H11A H 0.6501 0.3891 0.1506 0.094 Uiso 1 1 calc R
H11B H 0.7375 0.4337 0.2057 0.094 Uiso 1 1 calc R
H11C H 0.7107 0.4294 0.1003 0.094 Uiso 1 1 calc R
C12 C 0.6620(5) 0.54467(18) 0.1331(4) 0.086(2) Uani 1 1 d .
H12A H 0.6305 0.5792 0.1265 0.129 Uiso 1 1 calc R
H12B H 0.7002 0.5371 0.0861 0.129 Uiso 1 1 calc R
H12C H 0.7277 0.5405 0.1917 0.129 Uiso 1 1 calc R
C13 C 0.3370(5) 0.46843(16) 0.1064(3) 0.0540(15) Uani 1 1 d .
C14 C 0.2012(5) 0.45774(16) 0.0923(4) 0.0575(15) Uani 1 1 d .
H14 H 0.1419 0.4848 0.0824 0.069 Uiso 1 1 calc R
C15 C 0.1556(5) 0.40977(18) 0.0928(4) 0.0520(13) Uani 1 1 d .
C16 C 0.0116(6) 0.4008(2) 0.0752(5) 0.0793(19) 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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_3
C2 S1 C5 90.5(2) .
C10 S2 C13 91.1(2) .
O3 Al1 O1 121.32(12) .
O3 Al1 O2 123.96(15) .
O1 Al1 O2 114.70(16) .
O3 Al1 N1 93.70(17) .
O1 Al1 N1 90.03(15) .
O2 Al1 N1 86.98(14) .
O3 Al1 N2 92.77(17) .
O1 Al1 N2 87.35(15) .
O2 Al1 N2 88.68(14) .
N1 Al1 N2 173.47(16) .
C7 O1 Al1 132.0(3) .
C15 O2 Al1 133.7(3) .
Al1 O3 Al1 178.1(3) 2_655
C5 N1 C1 111.2(4) .
C5 N1 Al1 122.7(3) .
C1 N1 Al1 125.3(3) .
C13 N2 C9 110.0(4) .
C13 N2 Al1 123.1(3) .
C9 N2 Al1 126.4(3) .
C2 C1 N1 114.2(4) .
C2 C1 C3 125.1(5) .
N1 C1 C3 120.6(4) .
C1 C2 C4 127.2(5) .
C1 C2 S1 110.8(4) .
C4 C2 S1 122.0(4) .
C1 C3 H3A 109.5 .
C1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
C1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C2 C4 H4A 109.5 .
C2 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C2 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
N1 C5 C6 125.1(4) .
N1 C5 S1 113.1(4) .
C6 C5 S1 121.7(4) .
C7 C6 C5 121.7(4) .
C7 C6 H6 119.2 .
C5 C6 H6 119.2 .
O1 C7 C6 127.9(5) .
O1 C7 C8 112.3(4) .
C6 C7 C8 119.6(5) .
F3 C8 F1 104.9(5) .
F3 C8 F2 106.5(5) .
F1 C8 F2 105.0(5) .
F3 C8 C7 112.5(5) .
F1 C8 C7 113.0(5) .
F2 C8 C7 114.1(5) .
C10 C9 N2 115.0(4) .
C10 C9 C11 125.9(4) .
N2 C9 C11 119.1(4) .
C9 C10 C12 127.6(5) .
C9 C10 S2 110.1(4) .
C12 C10 S2 122.3(3) .
C9 C11 H11A 109.5 .
C9 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C9 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C10 C12 H12A 109.5 .
C10 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C10 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
N2 C13 C14 124.8(4) .
N2 C13 S2 113.8(3) .
C14 C13 S2 121.4(3) .
C15 C14 C13 122.3(4) .
C15 C14 H14 118.9 .
C13 C14 H14 118.9 .
O2 C15 C14 126.3(4) .
O2 C15 C16 113.8(4) .
C14 C15 C16 119.9(5) .
F6 C16 F5 106.6(6) .
F6 C16 F4 104.5(6) .
F5 C16 F4 105.3(6) .
F6 C16 C15 113.1(6) .
F5 C16 C15 114.7(5) .
F4 C16 C15 111.9(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C2 1.713(5) .
S1 C5 1.723(4) .
S2 C10 1.690(5) .
S2 C13 1.719(4) .
Al1 O3 1.6885(14) .
Al1 O1 1.796(3) .
Al1 O2 1.797(3) .
Al1 N1 2.086(4) .
Al1 N2 2.103(4) .
F1 C8 1.325(6) .
F2 C8 1.329(6) .
F3 C8 1.321(6) .
F4 C16 1.319(7) .
F5 C16 1.313(6) .
F6 C16 1.296(7) .
O1 C7 1.304(5) .
O2 C15 1.298(5) .
O3 Al1 1.6885(14) 2_655
N1 C5 1.327(5) .
N1 C1 1.407(6) .
N2 C13 1.329(5) .
N2 C9 1.398(5) .
C1 C2 1.347(5) .
C1 C3 1.492(6) .
C2 C4 1.503(6) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.436(6) .
C6 C7 1.329(6) .
C6 H6 0.9300 .
C7 C8 1.497(7) .
C9 C10 1.369(5) .
C9 C11 1.496(6) .
C10 C12 1.501(6) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.423(6) .
C14 C15 1.349(5) .
C14 H14 0.9300 .
C15 C16 1.493(7) .
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_4
O3 Al1 O1 C7 87.7(4) .
O2 Al1 O1 C7 -93.4(4) .
N1 Al1 O1 C7 -6.7(4) .
N2 Al1 O1 C7 179.3(4) .
O3 Al1 O2 C15 81.7(5) .
O1 Al1 O2 C15 -97.2(5) .
N1 Al1 O2 C15 174.1(5) .
N2 Al1 O2 C15 -10.8(5) .
O1 Al1 O3 Al1 -77.62(15) 2_655
O2 Al1 O3 Al1 103.53(16) 2_655
N1 Al1 O3 Al1 14.67(11) 2_655
N2 Al1 O3 Al1 -166.20(11) 2_655
O3 Al1 N1 C5 -113.7(3) .
O1 Al1 N1 C5 7.7(3) .
O2 Al1 N1 C5 122.4(3) .
N2 Al1 N1 C5 74.0(16) .
O3 Al1 N1 C1 55.1(3) .
O1 Al1 N1 C1 176.5(3) .
O2 Al1 N1 C1 -68.8(3) .
N2 Al1 N1 C1 -117.2(15) .
O3 Al1 N2 C13 -113.9(4) .
O1 Al1 N2 C13 124.8(4) .
O2 Al1 N2 C13 10.0(4) .
N1 Al1 N2 C13 58.4(17) .
O3 Al1 N2 C9 57.9(4) .
O1 Al1 N2 C9 -63.4(4) .
O2 Al1 N2 C9 -178.2(4) .
N1 Al1 N2 C9 -129.8(15) .
C5 N1 C1 C2 2.5(5) .
Al1 N1 C1 C2 -167.4(3) .
C5 N1 C1 C3 -177.1(4) .
Al1 N1 C1 C3 13.1(6) .
N1 C1 C2 C4 174.6(4) .
C3 C1 C2 C4 -5.8(8) .
N1 C1 C2 S1 -3.2(5) .
C3 C1 C2 S1 176.4(4) .
C5 S1 C2 C1 2.3(4) .
C5 S1 C2 C4 -175.6(4) .
C1 N1 C5 C6 -178.3(4) .
Al1 N1 C5 C6 -8.1(6) .
C1 N1 C5 S1 -0.7(5) .
Al1 N1 C5 S1 169.52(19) .
C2 S1 C5 N1 -0.9(4) .
C2 S1 C5 C6 176.8(4) .
N1 C5 C6 C7 4.6(7) .
S1 C5 C6 C7 -172.8(4) .
Al1 O1 C7 C6 5.6(7) .
Al1 O1 C7 C8 -169.9(3) .
C5 C6 C7 O1 -2.6(8) .
C5 C6 C7 C8 172.6(5) .
O1 C7 C8 F3 70.2(6) .
C6 C7 C8 F3 -105.7(5) .
O1 C7 C8 F1 -48.4(6) .
C6 C7 C8 F1 135.8(5) .
O1 C7 C8 F2 -168.3(4) .
C6 C7 C8 F2 15.8(7) .
C13 N2 C9 C10 -0.2(6) .
Al1 N2 C9 C10 -172.9(3) .
C13 N2 C9 C11 -179.4(4) .
Al1 N2 C9 C11 7.9(7) .
N2 C9 C10 C12 -179.4(5) .
C11 C9 C10 C12 -0.3(9) .
N2 C9 C10 S2 0.5(6) .
C11 C9 C10 S2 179.7(4) .
C13 S2 C10 C9 -0.5(4) .
C13 S2 C10 C12 179.5(5) .
C9 N2 C13 C14 180.0(5) .
Al1 N2 C13 C14 -7.0(7) .
C9 N2 C13 S2 -0.2(5) .
Al1 N2 C13 S2 172.8(2) .
C10 S2 C13 N2 0.4(4) .
C10 S2 C13 C14 -179.7(5) .
N2 C13 C14 C15 0.1(9) .
S2 C13 C14 C15 -179.7(4) .
Al1 O2 C15 C14 7.5(8) .
Al1 O2 C15 C16 -173.2(4) .
C13 C14 C15 O2 0.8(9) .
C13 C14 C15 C16 -178.4(6) .
O2 C15 C16 F6 55.1(8) .
C14 C15 C16 F6 -125.6(6) .
O2 C15 C16 F5 177.7(5) .
C14 C15 C16 F5 -3.0(10) .
O2 C15 C16 F4 -62.5(8) .
C14 C15 C16 F4 116.8(6) .
