#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/38/2203888.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2203888
loop_
_publ_author_name
'Nassar, Roger'
'Noll, Bruce C.'
'Henderson, Kenneth W.'
_publ_section_title
;Bis[μ²-bis(diphenylphosphinoyl)methanido-κ²O:O']hexamethyldi-μ³-oxo-tetraaluminium(III)
 tetrahydrofuran disolvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1023
_journal_page_last               m1024
_journal_paper_doi               10.1107/S1600536804011523
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Al4 (C H3)6 O2 (C25 H21 O2 P2)2], 2C4 H8 O1'
_chemical_formula_moiety         'C56 H60 Al4 O6 P4, 2C4 H8 O1'
_chemical_formula_sum            'C64 H76 Al4 O8 P4'
_chemical_formula_weight         1205.12
_chemical_name_systematic
;
Bis[μ²-bis(diphenylphosphinoyl)methanido-κ²O:O']hexamethyldi-μ³-oxo-
dialuminium(III) tetrahydrofuran disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.1170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0087(2)
_cell_length_b                   18.5644(3)
_cell_length_c                   13.7312(2)
_cell_measurement_reflns_used    5174
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.19
_cell_volume                     3242.19(9)
_computing_cell_refinement       'APEX2 and SAINT (Bruker--Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT and XPREP (Sheldrick, 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47479
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9712
_exptl_absorpt_correction_T_min  0.9603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0936P)²+2.8045P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1734
_reflns_number_gt                5264
_reflns_number_total             6623
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn6136.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2203888
_cod_database_fobs_code          2203888
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Al1 0.51781(7) 0.13590(5) -0.11532(6) 0.0421(2) Uani d . 1 Al
Al2 0.46736(6) 0.03576(4) 0.06943(6) 0.0316(2) Uani d . 1 Al
O1 0.64524(18) 0.17197(12) -0.05762(14) 0.0479(5) Uani d . 1 O
O2 0.56631(16) 0.06409(11) 0.16889(13) 0.0424(5) Uani d . 1 O
O3 0.50657(14) 0.05647(10) -0.04522(13) 0.0326(4) Uani d . 1 O
P1 0.70468(6) 0.20492(4) 0.04047(5) 0.03228(19) Uani d . 1 P
P2 0.64366(5) 0.12372(4) 0.21474(5) 0.03026(18) Uani d . 1 P
C1 0.7173(2) 0.29943(14) 0.0162(2) 0.0356(6) Uani d . 1 C
C2 0.7097(3) 0.32284(18) -0.0811(2) 0.0494(8) Uani d . 1 C
H2 0.6966 0.2891 -0.1343 0.059 Uiso calc R 1 H
C3 0.7211(3) 0.39511(19) -0.1007(3) 0.0597(9) Uani d . 1 C
H3 0.7163 0.4108 -0.1674 0.072 Uiso calc R 1 H
C4 0.7392(3) 0.44428(18) -0.0248(3) 0.0576(9) Uani d . 1 C
H4 0.7459 0.4939 -0.0390 0.069 Uiso calc R 1 H
C5 0.7476(3) 0.42214(17) 0.0710(3) 0.0529(8) Uani d . 1 C
H5 0.7608 0.4564 0.1236 0.063 Uiso calc R 1 H
C6 0.7370(2) 0.34969(15) 0.0925(2) 0.0433(7) Uani d . 1 C
H6 0.7432 0.3346 0.1596 0.052 Uiso calc R 1 H
C7 0.8343(2) 0.16606(14) 0.0614(2) 0.0389(6) Uani d . 1 C
C8 0.9078(2) 0.18236(17) 0.1462(3) 0.0472(8) Uani d . 1 C
H8 0.8904 0.2146 0.1940 0.057 Uiso calc R 1 H
C9 1.0078(3) 0.1517(2) 0.1620(4) 0.0713(12) Uani d . 1 C
H9 1.0585 0.1618 0.2210 0.086 Uiso calc R 1 H
C10 1.0322(4) 0.1057(2) 0.0895(5) 0.0806(15) Uani d . 1 C
H10 1.0999 0.0842 0.0996 0.097 Uiso calc R 1 H
C11 0.9596(4) 0.0913(2) 0.0043(4) 0.0784(14) Uani d . 1 C
H11 0.9781 0.0608 -0.0449 0.094 Uiso calc R 1 H
C12 0.8602(3) 0.12035(17) -0.0110(3) 0.0590(10) Uani d . 1 C
H12 0.8098 0.1096 -0.0700 0.071 Uiso calc R 1 H
C13 0.6535(2) 0.19737(15) 0.1443(2) 0.0317(6) Uani d . 1 C
H13 0.605(2) 0.2308(17) 0.145(2) 0.036(8) Uiso d . 1 H
C14 0.6001(2) 0.15336(19) 0.3241(2) 0.0436(7) Uani d . 1 C
C15 0.6247(3) 0.2223(2) 0.3621(3) 0.0656(11) Uani d . 1 C
H15 0.6647 0.2539 0.3302 0.079 Uiso calc R 1 H
C16 0.5913(5) 0.2448(3) 0.4463(3) 0.0986(18) Uani d . 1 C
H16 0.6087 0.2917 0.4724 0.118 Uiso calc R 1 H
C17 0.5330(5) 0.1995(3) 0.4921(3) 0.0986(18) Uani d . 1 C
H17 0.5097 0.2153 0.5497 0.118 Uiso calc R 1 H
C18 0.5082(3) 0.1319(3) 0.4556(3) 0.0830(15) Uani d . 1 C
H18 0.4668 0.1013 0.4875 0.100 Uiso calc R 1 H
C19 0.5435(3) 0.1067(2) 0.3707(2) 0.0601(10) Uani d . 1 C
H19 0.5285 0.0590 0.3467 0.072 Uiso calc R 1 H
C20 0.7668(2) 0.07750(14) 0.2565(2) 0.0338(6) Uani d . 1 C
C21 0.8358(2) 0.09901(15) 0.3430(2) 0.0406(7) Uani d . 1 C
H21 0.8180 0.1382 0.3807 0.049 Uiso calc R 1 H
C22 0.9305(3) 0.06327(18) 0.3744(3) 0.0536(8) Uani d . 1 C
H22 0.9777 0.0777 0.4337 0.064 Uiso calc R 1 H
C23 0.9557(3) 0.00615(19) 0.3182(3) 0.0607(10) Uani d . 1 C
H23 1.0209 -0.0182 0.3390 0.073 Uiso calc R 1 H
C24 0.8872(3) -0.01546(18) 0.2329(3) 0.0586(9) Uani d . 1 C
H24 0.9053 -0.0545 0.1951 0.070 Uiso calc R 1 H
C25 0.7923(3) 0.01930(17) 0.2019(2) 0.0466(7) Uani d . 1 C
H25 0.7445 0.0037 0.1436 0.056 Uiso calc R 1 H
C26 0.3262(2) 0.05986(19) 0.0857(3) 0.0507(8) Uani d . 1 C
H26A 0.3167 0.0430 0.1509 0.076 Uiso calc R 1 H
H26B 0.2743 0.0365 0.0331 0.076 Uiso calc R 1 H
H26C 0.3164 0.1122 0.0813 0.076 Uiso calc R 1 H
C27 0.5275(3) 0.1071(2) -0.2506(2) 0.0664(11) Uani d . 1 C
H27A 0.5825 0.0705 -0.2470 0.100 Uiso calc R 1 H
H27B 0.5450 0.1492 -0.2870 0.100 Uiso calc R 1 H
H27C 0.4600 0.0872 -0.2852 0.100 Uiso calc R 1 H
C28 0.4081(4) 0.2038(3) -0.0984(4) 0.0979(17) Uani d . 1 C
H28A 0.3400 0.1871 -0.1365 0.147 Uiso calc R 1 H
H28B 0.4237 0.2515 -0.1224 0.147 Uiso calc R 1 H
H28C 0.4055 0.2069 -0.0277 0.147 Uiso calc R 1 H
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'
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Al1 O1 . . 103.94(10)
O3 Al1 C28 . . 108.93(17)
O1 Al1 C28 . . 109.5(2)
O3 Al1 C27 . . 108.32(14)
O1 Al1 C27 . . 106.28(13)
C28 Al1 C27 . . 118.8(2)
O2 Al2 O3 . 3_655 107.19(10)
O2 Al2 O3 . . 108.80(9)
O3 Al2 O3 3_655 . 86.69(9)
O2 Al2 C26 . . 113.48(13)
O3 Al2 C26 3_655 . 117.44(12)
O3 Al2 C26 . . 119.97(13)
O2 Al2 Al2 . 3_655 115.13(9)
O3 Al2 Al2 3_655 3_655 43.43(6)
O3 Al2 Al2 . 3_655 43.26(6)
C26 Al2 Al2 . 3_655 131.32(11)
P1 O1 Al1 . . 141.21(14)
P2 O2 Al2 . . 147.82(14)
Al1 O3 Al2 . 3_655 130.57(11)
Al1 O3 Al2 . . 136.12(12)
Al2 O3 Al2 3_655 . 93.31(9)
O1 P1 C13 . . 119.33(12)
O1 P1 C1 . . 105.99(12)
C13 P1 C1 . . 107.59(13)
O1 P1 C7 . . 105.25(14)
C13 P1 C7 . . 110.56(13)
C1 P1 C7 . . 107.54(12)
O2 P2 C13 . . 117.92(12)
O2 P2 C14 . . 105.54(13)
C13 P2 C14 . . 107.71(15)
O2 P2 C20 . . 104.42(13)
C13 P2 C20 . . 113.39(13)
C14 P2 C20 . . 107.16(13)
C6 C1 C2 . . 118.8(3)
C6 C1 P1 . . 121.8(2)
C2 C1 P1 . . 119.5(2)
C3 C2 C1 . . 120.1(3)
C3 C2 H2 . . 119.9
C1 C2 H2 . . 119.9
C4 C3 C2 . . 120.5(3)
C4 C3 H3 . . 119.8
C2 C3 H3 . . 119.8
C5 C4 C3 . . 120.1(3)
C5 C4 H4 . . 120.0
C3 C4 H4 . . 120.0
C4 C5 C6 . . 120.4(3)
C4 C5 H5 . . 119.8
C6 C5 H5 . . 119.8
C1 C6 C5 . . 120.1(3)
C1 C6 H6 . . 119.9
C5 C6 H6 . . 119.9
C8 C7 C12 . . 120.4(3)
C8 C7 P1 . . 120.5(2)
C12 C7 P1 . . 119.1(3)
C7 C8 C9 . . 120.1(4)
C7 C8 H8 . . 119.9
C9 C8 H8 . . 119.9
C8 C9 C10 . . 118.8(4)
C8 C9 H9 . . 120.6
C10 C9 H9 . . 120.6
C11 C10 C9 . . 120.7(4)
C11 C10 H10 . . 119.7
C9 C10 H10 . . 119.7
C10 C11 C12 . . 120.8(4)
C10 C11 H11 . . 119.6
C12 C11 H11 . . 119.6
C11 C12 C7 . . 119.1(4)
C11 C12 H12 . . 120.4
C7 C12 H12 . . 120.4
P2 C13 P1 . . 129.37(17)
P2 C13 H13 . . 115.1(19)
P1 C13 H13 . . 110.6(19)
C19 C14 C15 . . 120.4(3)
C19 C14 P2 . . 119.2(3)
C15 C14 P2 . . 120.4(3)
C16 C15 C14 . . 120.2(4)
C16 C15 H15 . . 119.9
C14 C15 H15 . . 119.9
C17 C16 C15 . . 120.0(5)
C17 C16 H16 . . 120.0
C15 C16 H16 . . 120.0
C18 C17 C16 . . 120.4(4)
C18 C17 H17 . . 119.8
C16 C17 H17 . . 119.8
C17 C18 C19 . . 120.8(4)
C17 C18 H18 . . 119.6
C19 C18 H18 . . 119.6
C14 C19 C18 . . 118.1(4)
C14 C19 H19 . . 121.0
C18 C19 H19 . . 121.0
C21 C20 C25 . . 120.0(3)
C21 C20 P2 . . 120.5(2)
C25 C20 P2 . . 119.6(2)
C22 C21 C20 . . 120.0(3)
C22 C21 H21 . . 120.0
C20 C21 H21 . . 120.0
C21 C22 C23 . . 119.4(3)
C21 C22 H22 . . 120.3
C23 C22 H22 . . 120.3
C24 C23 C22 . . 120.6(3)
C24 C23 H23 . . 119.7
C22 C23 H23 . . 119.7
C23 C24 C25 . . 120.3(3)
C23 C24 H24 . . 119.8
C25 C24 H24 . . 119.8
C24 C25 C20 . . 119.7(3)
C24 C25 H25 . . 120.2
C20 C25 H25 . . 120.2
Al2 C26 H26A . . 109.5
Al2 C26 H26B . . 109.5
H26A C26 H26B . . 109.5
Al2 C26 H26C . . 109.5
H26A C26 H26C . . 109.5
H26B C26 H26C . . 109.5
Al1 C27 H27A . . 109.5
Al1 C27 H27B . . 109.5
H27A C27 H27B . . 109.5
Al1 C27 H27C . . 109.5
H27A C27 H27C . . 109.5
H27B C27 H27C . . 109.5
Al1 C28 H28A . . 109.5
Al1 C28 H28B . . 109.5
H28A C28 H28B . . 109.5
Al1 C28 H28C . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Al1 O3 . 1.7837(19)
Al1 O1 . 1.809(2)
Al1 C28 . 1.955(5)
Al1 C27 . 1.962(4)
Al2 O2 . 1.750(2)
Al2 O3 3_655 1.790(2)
Al2 O3 . 1.7955(19)
Al2 C26 . 1.948(3)
Al2 Al2 3_655 2.6075(16)
O1 P1 . 1.533(2)
O2 P2 . 1.5390(19)
O3 Al2 3_655 1.790(2)
P1 C13 . 1.701(3)
P1 C1 . 1.800(3)
P1 C7 . 1.800(3)
P2 C13 . 1.695(3)
P2 C14 . 1.799(3)
P2 C20 . 1.802(3)
C1 C6 . 1.385(4)
C1 C2 . 1.389(4)
C2 C3 . 1.383(5)
C2 H2 . 0.9500
C3 C4 . 1.368(5)
C3 H3 . 0.9500
C4 C5 . 1.361(5)
C4 H4 . 0.9500
C5 C6 . 1.390(4)
C5 H5 . 0.9500
C6 H6 . 0.9500
C7 C8 . 1.376(5)
C7 C12 . 1.401(4)
C8 C9 . 1.395(5)
C8 H8 . 0.9500
C9 C10 . 1.398(7)
C9 H9 . 0.9500
C10 C11 . 1.366(7)
C10 H10 . 0.9500
C11 C12 . 1.377(6)
C11 H11 . 0.9500
C12 H12 . 0.9500
C13 H13 . 0.88(3)
C14 C19 . 1.378(5)
C14 C15 . 1.394(5)
C15 C16 . 1.383(5)
C15 H15 . 0.9500
C16 C17 . 1.370(8)
C16 H16 . 0.9500
C17 C18 . 1.365(7)
C17 H17 . 0.9500
C18 C19 . 1.420(5)
C18 H18 . 0.9500
C19 H19 . 0.9500
C20 C21 . 1.388(4)
C20 C25 . 1.394(4)
C21 C22 . 1.386(4)
C21 H21 . 0.9500
C22 C23 . 1.390(5)
C22 H22 . 0.9500
C23 C24 . 1.374(5)
C23 H23 . 0.9500
C24 C25 . 1.379(5)
C24 H24 . 0.9500
C25 H25 . 0.9500
C26 H26A . 0.9800
C26 H26B . 0.9800
C26 H26C . 0.9800
C27 H27A . 0.9800
C27 H27B . 0.9800
C27 H27C . 0.9800
C28 H28A . 0.9800
C28 H28B . 0.9800
C28 H28C . 0.9800
