#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:17:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178601 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/12/4071287.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_4071287
loop_
_publ_author_name
'Martínez, Gema'
'Pedrosa, Sergio'
'Tabernero, Vanessa'
'Mosquera, Marta E. G.'
'Cuenca, Tomás'
_publ_section_title
;
 Controlled Synthesis of Novel Aryloxide Polynuclear Aluminum Species.
 Study of Their Catalytic Properties in Polymerization Processes†
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2300
_journal_paper_doi               10.1021/om800086a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C20 H18 Al2 F12 O2'
_chemical_formula_weight         572.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 92.638(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9720(16)
_cell_length_b                   7.6787(10)
_cell_length_c                   17.488(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.531
_cell_measurement_theta_min      4.143
_cell_volume                     1337.7(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27149
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3035
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0555
_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)+(0.0694P)²+0.9173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                1983
_reflns_number_total             3035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800086a-file003.cif
_cod_data_source_block           1
_cod_original_cell_volume        1337.7(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071287
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_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
Al1 Al 0.63281(8) 0.07529(11) -0.00646(4) 0.0367(3) Uani 1 1 d U
O1 O 0.49830(18) 0.0483(2) 0.06473(9) 0.0370(4) Uani 1 1 d U
C3 C 0.5029(2) 0.0973(3) 0.14143(12) 0.0294(5) Uani 1 1 d U
C8 C 0.4379(2) 0.2484(3) 0.16302(13) 0.0327(5) Uani 1 1 d U
H8 H 0.3917 0.3165 0.1266 0.039 Uiso 1 1 calc R
C5 C 0.5780(3) 0.0472(3) 0.27216(14) 0.0369(6) Uani 1 1 d U
C6 C 0.5134(3) 0.1975(3) 0.29486(13) 0.0361(6) Uani 1 1 d U
H6 H 0.5174 0.2313 0.3460 0.043 Uiso 1 1 calc R
C7 C 0.4428(3) 0.2968(3) 0.24009(14) 0.0348(5) Uani 1 1 d U
C4 C 0.5731(3) -0.0054(3) 0.19565(14) 0.0345(5) Uani 1 1 d U
H4 H 0.6157 -0.1070 0.1811 0.041 Uiso 1 1 calc R
F6 F 0.5928(3) -0.0791(4) 0.39465(13) 0.1241(12) Uani 1 1 d U
F5 F 0.6923(3) -0.2131(3) 0.30788(13) 0.0944(8) Uani 1 1 d U
C11 C 0.6568(4) -0.0569(5) 0.33173(17) 0.0591(8) Uani 1 1 d U
C10 C 0.3705(4) 0.4583(4) 0.26351(18) 0.0547(7) Uani 1 1 d U
C2 C 0.7883(3) -0.0671(5) 0.02237(19) 0.0655(10) Uani 1 1 d U
H2A H 0.8523 0.0014 0.0520 0.098 Uiso 1 1 calc R
H2B H 0.8288 -0.1086 -0.0229 0.098 Uiso 1 1 calc R
H2C H 0.7607 -0.1645 0.0523 0.098 Uiso 1 1 calc R
F4 F 0.7740(3) 0.0230(4) 0.35237(17) 0.1138(10) Uani 1 1 d U
C1 C 0.6428(4) 0.3158(4) -0.04117(19) 0.0639(9) Uani 1 1 d U
H1A H 0.7103 0.3766 -0.0107 0.096 Uiso 1 1 calc R
H1B H 0.5574 0.3713 -0.0360 0.096 Uiso 1 1 calc R
H1C H 0.6656 0.3179 -0.0939 0.096 Uiso 1 1 calc R
F2 F 0.4424(9) 0.6035(13) 0.2489(6) 0.118(3) Uani 0.70 1 d PU
F1 F 0.2565(4) 0.4853(6) 0.2186(2) 0.0863(12) Uani 0.70 1 d PU
F3 F 0.3300(6) 0.4559(8) 0.3334(3) 0.121(2) Uani 0.70 1 d PU
F1' F 0.4131(15) 0.504(2) 0.3345(6) 0.127(3) Uani 0.30 1 d PU
F2' F 0.2431(11) 0.4401(16) 0.2595(8) 0.100(2) Uani 0.30 1 d PU
F3' F 0.3982(19) 0.594(3) 0.2307(11) 0.090(2) Uani 0.30 1 d PU
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'
O O 0.0106 0.0060 '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
O1 Al1 O1 78.68(8) 3_655 .
O1 Al1 C2 112.55(14) 3_655 .
O1 Al1 C2 110.52(12) . .
O1 Al1 C1 110.76(12) 3_655 .
O1 Al1 C1 111.01(14) . .
C2 Al1 C1 124.20(17) . .
O1 Al1 Al1 39.41(6) 3_655 3_655
O1 Al1 Al1 39.28(5) . 3_655
C2 Al1 Al1 118.33(13) . 3_655
C1 Al1 Al1 117.45(13) . 3_655
C3 O1 Al1 130.61(15) . 3_655
C3 O1 Al1 127.91(15) . .
Al1 O1 Al1 101.32(8) 3_655 .
C4 C3 O1 119.7(2) . .
C4 C3 C8 120.8(2) . .
O1 C3 C8 119.5(2) . .
C7 C8 C3 119.2(2) . .
C6 C5 C4 121.2(2) . .
C6 C5 C11 118.5(2) . .
C4 C5 C11 120.3(2) . .
C5 C6 C7 119.1(2) . .
C8 C7 C6 120.9(2) . .
C8 C7 C10 119.2(2) . .
C6 C7 C10 120.0(2) . .
C3 C4 C5 118.8(2) . .
F6 C11 F5 107.1(3) . .
F6 C11 F4 106.5(3) . .
F5 C11 F4 104.7(3) . .
F6 C11 C5 113.1(3) . .
F5 C11 C5 113.7(3) . .
F4 C11 C5 111.1(3) . .
F3' C10 F3 122.4(10) . .
F3' C10 F2' 108.2(11) . .
F3 C10 F2' 72.5(6) . .
F3' C10 F2 23.3(11) . .
F3 C10 F2 112.2(6) . .
F2' C10 F2 127.8(8) . .
F3' C10 F1 78.6(9) . .
F3 C10 F1 104.8(4) . .
F2' C10 F1 35.6(5) . .
F2 C10 F1 101.6(5) . .
F3' C10 F1' 98.1(12) . .
F3 C10 F1' 40.1(8) . .
F2' C10 F1' 110.6(9) . .
F2 C10 F1' 79.1(10) . .
F1 C10 F1' 135.4(6) . .
F3' C10 C7 116.9(10) . .
F3 C10 C7 114.6(3) . .
F2' C10 C7 112.6(6) . .
F2 C10 C7 111.3(6) . .
F1 C10 C7 111.4(3) . .
F1' C10 C7 109.5(6) . .
F3' F2 F1' 107(3) . .
F3' F2 C10 65(2) . .
F1' F2 C10 50.1(6) . .
F3' F1 F2' 106.2(13) . .
F3' F1 C10 46.9(7) . .
F2' F1 C10 66.1(10) . .
F2' F3 C10 52.9(4) . .
F2' F3 F1' 122.1(10) . .
C10 F3 F1' 72.0(8) . .
F2 F1' C10 50.9(6) . .
F2 F1' F3 110.8(11) . .
C10 F1' F3 67.9(9) . .
F3 F2' F1 127.0(14) . .
F3 F2' C10 54.6(6) . .
F1 F2' C10 78.3(9) . .
F2 F3' C10 92(3) . .
F2 F3' F1 145(3) . .
C10 F3' F1 54.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 O1 1.8778(18) 3_655
Al1 O1 1.8829(19) .
Al1 C2 1.945(3) .
Al1 C1 1.948(3) .
Al1 Al1 2.9085(16) 3_655
O1 C3 1.392(3) .
O1 Al1 1.8778(18) 3_655
C3 C4 1.396(3) .
C3 C8 1.390(3) .
C8 C7 1.397(3) .
C5 C6 1.389(4) .
C5 C4 1.396(3) .
C5 C11 1.505(4) .
C6 C7 1.390(3) .
C7 C10 1.501(4) .
F6 C11 1.308(4) .
F5 C11 1.324(4) .
C11 F4 1.354(4) .
C10 F3' 1.228(17) .
C10 F3 1.306(5) .
C10 F2' 1.277(12) .
C10 F2 1.356(8) .
C10 F1 1.368(5) .
C10 F1' 1.341(11) .
F2 F3' 0.54(2) .
F2 F1' 1.716(19) .
F1 F3' 1.647(17) .
F1 F2' 0.812(11) .
F3 F2' 1.527(15) .
F3 F1' 0.908(18) .
