#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320243.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_4320243
loop_
_publ_author_name
'Marilena Ferbinteanu'
'Herbert W. Roesky'
'Fanica Cimpoesu'
'Mihail Atanasov'
'Sinje Köpke'
'Regine Herbst-Irmer'
_publ_contact_author
;
     Dr. Regine Herbst-Irmer
     Institut für Anorganische Chemie
     Universität Göttingen
     Tammannstr. 4
     37077 Göttingen
     Germany
;
_publ_contact_author_email       rherbst@shelx.uni-ac.gwdg.de
_publ_contact_author_fax         '049 551 392582'
_publ_contact_author_phone       '049 551 393007'
_publ_section_title
;
 New Synthetic and Structural Aspects in the Chemistry of Alkylaluminum
 Fluorides. The Mutual Influence of Hard and Soft Ligands and the
 Hybridization as Rigorous Structural Criterion#
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4947
_journal_page_last               4955
_journal_paper_doi               10.1021/ic010131g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H20 Al F4 P'
_chemical_formula_weight         442.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            8
_cell_length_a                   17.220(2)
_cell_length_b                   17.220(2)
_cell_length_c                   14.000(3)
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      1.67
_cell_volume                     4151.4(11)
_computing_cell_refinement       'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            60925
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0397
_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)+(0.0456P)²+1.9006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3898
_reflns_number_total             4819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010131g_1.cif
_cod_data_source_block           merg2
_cod_database_code               4320243
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.25102(6) 0.24117(3) 0.12628(4) 0.01790(12) Uani 1 1 d . . .
Al1 Al 0.5000 0.0000 0.2500 0.0255(3) Uani 1 4 d SDU . .
Al2 Al 0.0000 0.5000 0.2500 0.0241(3) Uani 1 4 d SDU . .
F2 F 0.0511(14) 0.5659(12) 0.302(2) 0.112(8) Uani 0.25 1 d PDU A -1
F2A F -0.0695(15) 0.4670(11) 0.316(2) 0.101(7) Uani 0.25 1 d PDU A -1
F2B F -0.0368(12) 0.5304(7) 0.1489(10) 0.087(5) Uani 0.25 1 d PDU A -1
F2C F 0.0560(12) 0.4256(12) 0.2238(13) 0.096(6) Uani 0.25 1 d PDU A -1
Al3 Al 0.0072(10) -0.0032(16) 0.0023(12) 0.0253(19) Uani 0.25 1 d PDU B -1
F3 F 0.0991(8) 0.0036(11) 0.0288(13) 0.058(4) Uani 0.25 1 d PDU B -1
F3A F -0.0398(10) -0.0076(12) 0.1027(9) 0.088(4) Uani 0.25 1 d PDU B -1
F3B F -0.0204(12) 0.073(3) -0.056(3) 0.105(8) Uani 0.25 1 d PDU B -1
F3C F -0.0061(14) -0.081(3) -0.061(3) 0.113(10) Uani 0.25 1 d PDU B -1
F4 F 0.44810(11) 0.44272(11) 0.06925(15) 0.0714(6) Uani 1 1 d DU . .
F1 F 0.48862(11) 0.07682(11) 0.18138(14) 0.0703(6) Uani 1 1 d DU . .
Al4 Al 0.5000 0.5000 0.0000 0.0235(3) Uani 1 4 d SDU . .
C10 C 0.26812(14) 0.16124(11) 0.04627(15) 0.0226(4) Uani 1 1 d . . .
C11 C 0.21144(17) 0.14555(12) -0.02286(16) 0.0322(5) Uani 1 1 d . . .
H11 H 0.1652 0.1756 -0.0254 0.039 Uiso 1 1 calc R . .
C12 C 0.22336(19) 0.08569(13) -0.08752(18) 0.0396(6) Uani 1 1 d . . .
H12 H 0.1846 0.0739 -0.1336 0.047 Uiso 1 1 calc R . .
C13 C 0.29155(17) 0.04313(13) -0.08506(18) 0.0353(6) Uani 1 1 d . . .
H13 H 0.2997 0.0027 -0.1301 0.042 Uiso 1 1 calc R . .
C14 C 0.34771(16) 0.05919(12) -0.01751(18) 0.0317(5) Uani 1 1 d . . .
H14 H 0.3945 0.0300 -0.0167 0.038 Uiso 1 1 calc R . .
C15 C 0.33620(14) 0.11809(11) 0.04953(16) 0.0253(5) Uani 1 1 d . . .
H15 H 0.3744 0.1285 0.0968 0.030 Uiso 1 1 calc R . .
C20 C 0.16650(12) 0.22384(11) 0.19850(15) 0.0213(4) Uani 1 1 d . . .
C21 C 0.12169(12) 0.15661(12) 0.18957(17) 0.0253(5) Uani 1 1 d . . .
H21 H 0.1338 0.1189 0.1424 0.030 Uiso 1 1 calc R . .
C22 C 0.05869(12) 0.14576(13) 0.25120(19) 0.0325(5) Uani 1 1 d . . .
H22 H 0.0283 0.0999 0.2466 0.039 Uiso 1 1 calc R . .
C23 C 0.04037(12) 0.20129(15) 0.31859(18) 0.0329(5) Uani 1 1 d . . .
H23 H -0.0028 0.1934 0.3597 0.039 Uiso 1 1 calc R . .
C24 C 0.08437(12) 0.26867(15) 0.32695(18) 0.0331(5) Uani 1 1 d . . .
H24 H 0.0709 0.3071 0.3728 0.040 Uiso 1 1 calc R . .
C25 C 0.14804(12) 0.27927(13) 0.26784(15) 0.0262(5) Uani 1 1 d . . .
H25 H 0.1793 0.3244 0.2745 0.031 Uiso 1 1 calc R . .
C30 C 0.23838(13) 0.32671(11) 0.05455(15) 0.0204(4) Uani 1 1 d . . .
C31 C 0.17272(13) 0.37374(11) 0.06191(16) 0.0222(4) Uani 1 1 d . . .
H31 H 0.1332 0.3619 0.1069 0.027 Uiso 1 1 calc R . .
C32 C 0.16574(14) 0.43827(12) 0.00261(17) 0.0286(5) Uani 1 1 d . . .
H32 H 0.1208 0.4701 0.0066 0.034 Uiso 1 1 calc R . .
C33 C 0.22363(15) 0.45636(12) -0.06204(17) 0.0281(5) Uani 1 1 d . . .
H33 H 0.2183 0.5005 -0.1022 0.034 Uiso 1 1 calc R . .
C34 C 0.28960(15) 0.41028(12) -0.06846(16) 0.0280(5) Uani 1 1 d . . .
H34 H 0.3297 0.4235 -0.1122 0.034 Uiso 1 1 calc R . .
C35 C 0.29711(14) 0.34505(11) -0.01122(15) 0.0238(4) Uani 1 1 d . . .
H35 H 0.3418 0.3129 -0.0165 0.029 Uiso 1 1 calc R . .
C40 C 0.33209(12) 0.25320(11) 0.20518(14) 0.0196(4) Uani 1 1 d . . .
C41 C 0.34779(12) 0.19427(13) 0.27119(16) 0.0262(5) Uani 1 1 d . . .
H41 H 0.3163 0.1490 0.2730 0.031 Uiso 1 1 calc R . .
C42 C 0.40971(12) 0.20240(14) 0.33402(17) 0.0297(5) Uani 1 1 d . . .
H42 H 0.4213 0.1621 0.3780 0.036 Uiso 1 1 calc R . .
C43 C 0.45454(12) 0.26924(13) 0.33265(17) 0.0286(5) Uani 1 1 d . . .
H43 H 0.4962 0.2749 0.3766 0.034 Uiso 1 1 calc R . .
C44 C 0.43902(12) 0.32781(13) 0.26776(17) 0.0262(5) Uani 1 1 d . . .
H44 H 0.4700 0.3734 0.2673 0.031 Uiso 1 1 calc R . .
C45 C 0.37797(11) 0.31997(11) 0.20303(15) 0.0219(4) Uani 1 1 d . . .
H45 H 0.3677 0.3598 0.1578 0.026 Uiso 1 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C40 P1 C30 110.13(9) . . ?
C40 P1 C20 107.66(10) . . ?
C30 P1 C20 110.65(9) . . ?
C40 P1 C10 110.16(10) . . ?
C30 P1 C10 107.41(10) . . ?
C20 P1 C10 110.85(9) . . ?
F1 Al1 F1 109.90(8) 8_545 . ?
F1 Al1 F1 108.61(16) 8_545 7 ?
F1 Al1 F1 109.90(8) . 7 ?
F1 Al1 F1 109.91(8) 8_545 2_655 ?
F1 Al1 F1 108.61(16) . 2_655 ?
F1 Al1 F1 109.90(8) 7 2_655 ?
F2 Al2 F2A 113.3(7) . . ?
F2 Al2 F2B 112.1(12) . . ?
F2A Al2 F2B 108.6(11) . . ?
F2 Al2 F2C 109.2(13) . . ?
F2A Al2 F2C 106.7(13) . . ?
F2B Al2 F2C 106.5(7) . . ?
F3B Al3 F3A 109.0(15) . . ?
F3B Al3 F3C 111.2(12) . . ?
F3A Al3 F3C 111.1(16) . . ?
F3B Al3 F3 109.9(16) . . ?
F3A Al3 F3 106.9(11) . . ?
F3C Al3 F3 108.6(15) . . ?
F4 Al4 F4 110.28(8) 3_565 . ?
F4 Al4 F4 110.28(8) 3_565 2_665 ?
F4 Al4 F4 107.86(16) . 2_665 ?
F4 Al4 F4 107.86(16) 3_565 4_655 ?
F4 Al4 F4 110.28(8) . 4_655 ?
F4 Al4 F4 110.28(8) 2_665 4_655 ?
C15 C10 C11 120.5(2) . . ?
C15 C10 P1 121.81(16) . . ?
C11 C10 P1 117.63(16) . . ?
C12 C11 C10 119.4(2) . . ?
C13 C12 C11 120.2(2) . . ?
C14 C13 C12 120.3(2) . . ?
C13 C14 C15 120.4(2) . . ?
C10 C15 C14 119.1(2) . . ?
C21 C20 C25 120.16(19) . . ?
C21 C20 P1 122.32(16) . . ?
C25 C20 P1 117.48(15) . . ?
C20 C21 C22 118.9(2) . . ?
C23 C22 C21 120.4(2) . . ?
C22 C23 C24 120.7(2) . . ?
C25 C24 C23 119.4(2) . . ?
C24 C25 C20 120.3(2) . . ?
C31 C30 C35 120.13(19) . . ?
C31 C30 P1 122.22(16) . . ?
C35 C30 P1 117.65(15) . . ?
C32 C31 C30 119.3(2) . . ?
C33 C32 C31 120.5(2) . . ?
C32 C33 C34 120.2(2) . . ?
C35 C34 C33 120.1(2) . . ?
C34 C35 C30 119.6(2) . . ?
C45 C40 C41 120.18(18) . . ?
C45 C40 P1 121.53(15) . . ?
C41 C40 P1 118.28(15) . . ?
C42 C41 C40 119.57(19) . . ?
C43 C42 C41 120.2(2) . . ?
C44 C43 C42 120.5(2) . . ?
C43 C44 C45 120.1(2) . . ?
C44 C45 C40 119.50(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C40 1.792(2) . ?
P1 C30 1.796(2) . ?
P1 C20 1.797(2) . ?
P1 C10 1.799(2) . ?
Al1 F1 1.6465(15) 8_545 ?
Al1 F1 1.6466(15) . ?
Al1 F1 1.6466(15) 7 ?
Al1 F1 1.6466(15) 2_655 ?
Al2 F2 1.610(10) . ?
Al2 F2A 1.615(10) . ?
Al2 F2B 1.637(9) . ?
Al2 F2C 1.646(10) . ?
Al3 F3B 1.620(13) . ?
Al3 F3A 1.623(13) . ?
Al3 F3C 1.624(13) . ?
Al3 F3 1.630(13) . ?
F4 Al4 1.6466(16) . ?
Al4 F4 1.6466(16) 3_565 ?
Al4 F4 1.6466(16) 2_665 ?
Al4 F4 1.6466(16) 4_655 ?
C10 C15 1.389(3) . ?
C10 C11 1.401(3) . ?
C11 C12 1.387(3) . ?
C12 C13 1.385(4) . ?
C13 C14 1.381(3) . ?
C14 C15 1.396(3) . ?
C20 C21 1.397(3) . ?
C20 C25 1.398(3) . ?
C21 C22 1.399(3) . ?
C22 C23 1.380(3) . ?
C23 C24 1.391(3) . ?
C24 C25 1.386(3) . ?
C30 C31 1.395(3) . ?
C30 C35 1.404(3) . ?
C31 C32 1.392(3) . ?
C32 C33 1.382(3) . ?
C33 C34 1.389(3) . ?
C34 C35 1.386(3) . ?
C40 C45 1.395(3) . ?
C40 C41 1.399(3) . ?
C41 C42 1.389(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.383(3) . ?
C44 C45 1.395(3) . ?
