#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007260.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_2007260
loop_
_publ_author_name
'Kritikos, M.'
'Wijk, M.'
'Westin, G.'
_publ_section_title
;
[Er~2~Al~2~(O^i^Pr)~12~(HO^i^Pr)~2~], a Novel
Heterobimetallic Alkoxide
;
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 576
_journal_page_last 578
_journal_volume 54
_journal_year 1998
_chemical_formula_moiety 'C42 H100 Al2 Er2 O14'
_chemical_formula_sum 'C42 H100 Al2 Er2 O14'
_chemical_formula_weight 1217.70
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 82.4570(10)
_cell_angle_beta 66.7620(10)
_cell_angle_gamma 70.9850(10)
_cell_formula_units_Z 1
_cell_length_a 10.797(3)
_cell_length_b 11.933(3)
_cell_length_c 12.939(3)
_cell_measurement_reflns_used 24
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 18.2
_cell_measurement_theta_min 15.2
_cell_volume 1448.2(6)
_computing_cell_refinement DIF4
_computing_data_collection 'DIF4 (Stoe, 1990)'
_computing_data_reduction 'X-RED (Stoe, 1996a)'
_computing_molecular_graphics 'XP (Siemens, 1990)'
_computing_publication_material SHELXL93
_computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature 150(2)
_diffrn_measurement_device_type 'Stoe 4-circle'
_diffrn_measurement_method \w--2\q
_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 0.0132
_diffrn_reflns_av_sigmaI/netI 0.0115
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 7157
_diffrn_reflns_theta_max 26.99
_diffrn_reflns_theta_min 1.71
_diffrn_standards_decay_% 3.1
_diffrn_standards_interval_time 240
_diffrn_standards_number 4
_exptl_absorpt_coefficient_mu 2.959
_exptl_absorpt_correction_T_max 0.6782
_exptl_absorpt_correction_T_min 0.5143
_exptl_absorpt_correction_type 'integration (X-SHAPE; Stoe, 1996b)'
_exptl_crystal_colour 'Pale pink'
_exptl_crystal_density_diffrn 1.396
_exptl_crystal_density_meas 'Not measured'
_exptl_crystal_density_method 'Not measured'
_exptl_crystal_description Irregular
_exptl_crystal_F_000 626
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.25
_refine_diff_density_max 1.591
_refine_diff_density_min -1.335
_refine_ls_extinction_coef 0.0022(3)
_refine_ls_extinction_method SHELXL93_(Sheldrick,_1993)
_refine_ls_goodness_of_fit_all 1.088
_refine_ls_goodness_of_fit_obs 1.095
_refine_ls_hydrogen_treatment H_atoms:_see_text_below
_refine_ls_matrix_type full
_refine_ls_number_parameters 288
_refine_ls_number_reflns 6309
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.088
_refine_ls_restrained_S_obs 1.095
_refine_ls_R_factor_all 0.0250
_refine_ls_R_factor_gt 0.0237
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0366P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.0626
_refine_ls_wR_factor_ref 0.0618
_reflns_number_gt 6084
_reflns_number_total 6309
_reflns_observed_criterion >2sigma(I)
_[local]_cod_data_source_file os1001.cif
_[local]_cod_data_source_block Er2Al2
_cod_database_code 2007260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Er 0.02069(7) 0.02341(7) 0.02076(7) -0.00367(5) -0.00900(5) -0.00113(4)
Al 0.0246(4) 0.0265(4) 0.0242(4) -0.0064(3) -0.0096(3) -0.0035(3)
O1 0.0238(9) 0.0267(9) 0.0261(9) -0.0121(7) -0.0085(7) 0.0015(7)
O2 0.0271(9) 0.0257(9) 0.0228(9) -0.0037(7) -0.0118(7) -0.0003(7)
O3 0.0309(10) 0.0233(9) 0.0282(9) -0.0040(8) -0.0131(8) 0.0008(7)
O4 0.0234(9) 0.0450(12) 0.0317(10) -0.0104(9) -0.0095(8) -0.0071(9)
O5 0.0279(10) 0.0419(12) 0.0263(10) -0.0096(9) -0.0051(8) -0.0090(8)
O6 0.0351(11) 0.0434(12) 0.0385(11) -0.0135(9) -0.0150(9) -0.0093(9)
O7 0.0386(11) 0.0401(12) 0.0336(11) -0.0019(9) -0.0223(9) 0.0018(9)
C1 0.040(2) 0.0290(14) 0.0294(14) -0.0029(12) -0.0180(12) 0.0006(11)
C2 0.047(2) 0.048(2) 0.063(2) -0.032(2) -0.019(2) 0.008(2)
C3 0.059(2) 0.028(2) 0.055(2) -0.0020(15) -0.031(2) 0.0032(14)
C4 0.0264(14) 0.053(2) 0.046(2) -0.0124(13) -0.0152(13) -0.0120(15)
C5 0.040(2) 0.073(3) 0.036(2) -0.011(2) -0.0038(14) -0.022(2)
C6 0.035(2) 0.041(2) 0.055(2) -0.0130(13) -0.0178(15) -0.0065(15)
C7 0.084(3) 0.054(2) 0.063(3) -0.009(2) -0.056(2) 0.011(2)
C1A 0.076(3) 0.105(4) 0.072(3) -0.065(3) -0.033(2) 0.000(3)
C1B 0.143(6) 0.083(4) 0.115(5) -0.087(4) -0.064(4) 0.053(4)
C2A 0.077(3) 0.043(2) 0.062(2) -0.007(2) -0.054(2) 0.006(2)
C2B 0.063(3) 0.047(2) 0.073(3) -0.018(2) -0.019(2) 0.027(2)
C3A 0.077(3) 0.037(2) 0.064(3) 0.010(2) -0.018(2) -0.002(2)
C3B 0.158(6) 0.045(3) 0.055(3) -0.006(3) -0.009(3) 0.019(2)
C4A 0.035(2) 0.064(2) 0.058(2) -0.001(2) -0.021(2) -0.010(2)
C4B 0.042(2) 0.076(3) 0.090(3) -0.037(2) -0.011(2) -0.002(3)
C5A 0.038(2) 0.222(9) 0.093(4) 0.010(4) -0.005(3) -0.096(5)
C5B 0.178(8) 0.121(6) 0.029(2) 0.043(5) -0.004(3) -0.002(3)
C6A 0.053(2) 0.064(3) 0.084(3) -0.030(2) -0.016(2) 0.011(2)
C6B 0.092(4) 0.085(3) 0.083(3) -0.041(3) -0.062(3) 0.011(3)
C7A 0.065(3) 0.080(3) 0.062(3) -0.016(2) -0.045(2) 0.002(2)
C7B 0.103(4) 0.085(4) 0.079(3) -0.032(3) -0.058(3) 0.037(3)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Er 0.147833(11) 0.372695(9) 0.438328(8) 0.02189(5) Uani d . 1 Er
Al 0.21054(8) 0.24321(7) 0.21332(7) 0.0250(2) Uani d . 1 Al
O1 0.0861(2) 0.5687(2) 0.4623(2) 0.0248(4) Uani d . 1 O
O2 0.1145(2) 0.3884(2) 0.2678(2) 0.0255(4) Uani d . 1 O
O3 0.2034(2) 0.1921(2) 0.3510(2) 0.0280(4) Uani d . 1 O
O4 0.3778(2) 0.3653(2) 0.2990(2) 0.0329(4) Uani d . 1 O
O5 0.3832(2) 0.2437(2) 0.1336(2) 0.0330(4) Uani d . 1 O
O6 0.1491(2) 0.1768(2) 0.1438(2) 0.0373(5) Uani d . 1 O
O7 0.2339(2) 0.2978(2) 0.5552(2) 0.0374(5) Uani d . 1 O
C1 0.0638(3) 0.4965(3) 0.2137(3) 0.0332(6) Uani d . 1 C
H1 -0.0006(3) 0.5573(3) 0.2734(3) 0.040(10) Uiso calc R 1 H
C2 0.1847(4) 0.6345(4) 0.4291(4) 0.0494(9) Uani d . 1 C
H2 0.2735(4) 0.5821(4) 0.3745(4) 0.059 Uiso calc R 1 H
C3 0.2879(4) 0.0797(3) 0.3770(3) 0.0475(8) Uani d . 1 C
H3 0.3640(4) 0.0949(3) 0.3936(3) 0.057 Uiso calc R 1 H
C4 0.5080(3) 0.3576(3) 0.3101(3) 0.0400(7) Uani d . 1 C
H4 0.4835(3) 0.3992(3) 0.3811(3) 0.048 Uiso calc R 1 H
C5 0.4728(4) 0.1880(4) 0.0272(3) 0.0525(9) Uani d . 1 C
H5 0.4409(4) 0.1193(4) 0.0234(3) 0.063 Uiso calc R 1 H
C6 0.0193(4) 0.1630(3) 0.1570(3) 0.0421(7) Uani d . 1 C
H6 -0.0585(4) 0.2321(3) 0.2005(3) 0.050 Uiso calc R 1 H
C7 0.3083(5) 0.2404(4) 0.6236(4) 0.0617(11) Uani d . 1 C
H7 0.3860(5) 0.1729(4) 0.5774(4) 0.074 Uiso calc R 1 H
C1A 0.2220(5) 0.6495(5) 0.5236(4) 0.0726(14) Uani d . 1 C
H1A1 0.256(4) 0.5717(6) 0.556(2) 0.109 Uiso calc R 1 H
H1A2 0.297(3) 0.688(3) 0.4963(8) 0.109 Uiso calc R 1 H
H1A3 0.1385(12) 0.699(3) 0.5818(16) 0.109 Uiso calc R 1 H
C1B 0.1453(8) 0.7405(5) 0.3649(6) 0.100(2) Uani d . 1 C
H1B1 0.225(2) 0.773(3) 0.330(4) 0.150 Uiso calc R 1 H
H1B2 0.121(6) 0.7200(11) 0.306(3) 0.150 Uiso calc R 1 H
H1B3 0.064(4) 0.7996(19) 0.4152(10) 0.150 Uiso calc R 1 H
C2A -0.0203(5) 0.4790(3) 0.1515(4) 0.0549(10) Uani d . 1 C
H2A1 -0.064(3) 0.5554(6) 0.123(3) 0.082 Uiso calc R 1 H
H2A2 -0.095(2) 0.446(3) 0.2028(8) 0.082 Uiso calc R 1 H
H2A3 0.0423(8) 0.425(2) 0.0886(17) 0.082 Uiso calc R 1 H
C2B 0.1841(5) 0.5419(4) 0.1370(4) 0.0652(12) Uani d . 1 C
H2B1 0.1463(5) 0.6207(15) 0.109(3) 0.098 Uiso calc R 1 H
H2B2 0.244(2) 0.4876(18) 0.0734(17) 0.098 Uiso calc R 1 H
H2B3 0.241(2) 0.547(3) 0.1786(9) 0.098 Uiso calc R 1 H
C3A 0.3585(6) -0.0049(4) 0.2809(4) 0.0691(13) Uani d . 1 C
H3A1 0.416(3) -0.0794(13) 0.3024(12) 0.104 Uiso calc R 1 H
H3A2 0.420(3) 0.0295(15) 0.2158(11) 0.104 Uiso calc R 1 H
H3A3 0.2867(6) -0.020(3) 0.261(2) 0.104 Uiso calc R 1 H
C3B 0.2030(8) 0.0288(5) 0.4782(4) 0.105(3) Uani d . 1 C
H3B1 0.2625(16) -0.047(3) 0.496(3) 0.157 Uiso calc R 1 H
H3B2 0.126(4) 0.015(5) 0.4654(17) 0.157 Uiso calc R 1 H
H3B3 0.164(5) 0.084(2) 0.5411(12) 0.157 Uiso calc R 1 H
C4A 0.5900(4) 0.2302(4) 0.3202(4) 0.0537(9) Uani d . 1 C
H4A1 0.6727(19) 0.2273(4) 0.336(3) 0.081 Uiso calc R 1 H
H4A2 0.621(3) 0.1888(8) 0.2496(10) 0.081 Uiso calc R 1 H
H4A3 0.5295(11) 0.1917(9) 0.3817(18) 0.081 Uiso calc R 1 H
C4B 0.5917(4) 0.4214(5) 0.2133(5) 0.0685(13) Uani d . 1 C
H4B1 0.676(2) 0.422(3) 0.2242(17) 0.103 Uiso calc R 1 H
H4B2 0.5336(15) 0.5033(11) 0.210(2) 0.103 Uiso calc R 1 H
H4B3 0.620(4) 0.381(2) 0.1428(6) 0.103 Uiso calc R 1 H
C5A 0.6212(5) 0.1386(8) 0.0203(6) 0.127(3) Uani d . 1 C
H5A1 0.6789(17) 0.092(6) -0.049(3) 0.190 Uiso calc R 1 H
H5A2 0.6241(11) 0.088(5) 0.086(3) 0.190 Uiso calc R 1 H
H5A3 0.659(3) 0.2036(8) 0.019(6) 0.190 Uiso calc R 1 H
C5B 0.4555(10) 0.2672(7) -0.0644(4) 0.144(4) Uani d . 1 C
H5B1 0.523(6) 0.229(3) -0.1363(5) 0.216 Uiso calc R 1 H
H5B2 0.473(8) 0.341(3) -0.058(4) 0.216 Uiso calc R 1 H
H5B3 0.359(3) 0.285(6) -0.062(4) 0.216 Uiso calc R 1 H
C6A -0.0002(5) 0.0517(4) 0.2207(5) 0.0679(12) Uani d . 1 C
H6A1 -0.0926(18) 0.0455(18) 0.231(3) 0.102 Uiso calc R 1 H
H6A2 0.005(4) 0.0539(16) 0.2944(14) 0.102 Uiso calc R 1 H
H6A3 0.074(2) -0.0170(5) 0.1784(16) 0.102 Uiso calc R 1 H
C6B 0.0131(6) 0.1633(5) 0.0427(5) 0.0740(14) Uani d . 1 C
H6B1 -0.074(2) 0.147(4) 0.0509(5) 0.111 Uiso calc R 1 H
H6B2 0.095(2) 0.102(3) -0.0041(12) 0.111 Uiso calc R 1 H
H6B3 0.014(4) 0.2409(13) 0.0071(15) 0.111 Uiso calc R 1 H
C7A 0.3813(5) 0.3154(5) 0.6457(4) 0.0639(11) Uani d . 1 C
H7A1 0.436(3) 0.2706(12) 0.691(3) 0.096 Uiso calc R 1 H
H7A2 0.3111(5) 0.3867(17) 0.687(3) 0.096 Uiso calc R 1 H
H7A3 0.445(3) 0.338(3) 0.5741(4) 0.096 Uiso calc R 1 H
C7B 0.2288(7) 0.1862(5) 0.7221(5) 0.084(2) Uani d . 1 C
H7B1 0.2930(8) 0.132(2) 0.7559(16) 0.126 Uiso calc R 1 H
H7B2 0.181(3) 0.142(2) 0.7011(6) 0.126 Uiso calc R 1 H
H7B3 0.159(2) 0.2478(6) 0.7764(12) 0.126 Uiso calc R 1 H
H100 0.390(3) 0.331(3) 0.2411(8) 0.052(12) Uiso d R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Er Er -.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al .0645 .0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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
_geom_angle_publ_flag
O7 Er O1 . . 105.16(8) y
O7 Er O1 . 2_566 104.24(8) ?
O1 Er O1 . 2_566 73.64(7) ?
O7 Er O2 . . 156.93(8) y
O1 Er O2 . . 94.94(7) y
O1 Er O2 2_566 . 92.06(7) y
O7 Er O3 . . 94.82(8) y
O1 Er O3 . . 159.11(7) y
O1 Er O3 2_566 . 107.65(7) y
O2 Er O3 . . 64.30(7) y
O7 Er O4 . . 90.89(9) y
O1 Er O4 . . 93.07(7) y
O1 Er O4 2_566 . 161.92(8) y
O2 Er O4 . . 76.62(7) y
O3 Er O4 . . 80.38(7) y
O7 Er Al . . 124.32(7) y
O1 Er Al . . 126.04(5) y
O1 Er Al 2_566 . 109.42(5) ?
O2 Er Al . . 32.91(5) ?
O3 Er Al . . 33.22(5) ?
O4 Er Al . . 68.20(5) ?
O7 Er Er . 2_566 108.48(6) ?
O1 Er Er . 2_566 36.86(5) ?
O1 Er Er 2_566 2_566 36.78(5) ?
O2 Er Er . 2_566 94.37(5) ?
O3 Er Er . 2_566 140.58(5) ?
O4 Er Er . 2_566 128.88(6) ?
Al Er Er . 2_566 125.09(2) ?
O6 Al O5 . . 111.48(11) y
O6 Al O2 . . 120.38(11) y
O5 Al O2 . . 106.79(10) y
O6 Al O3 . . 119.00(11) y
O5 Al O3 . . 107.40(10) y
O2 Al O3 . . 89.29(9) y
O6 Al Er . . 147.05(9) ?
O5 Al Er . . 101.46(7) ?
O2 Al Er . . 45.93(6) ?
O3 Al Er . . 46.27(7) y
C2 O1 Er . . 123.8(2) y
C2 O1 Er . 2_566 129.5(2) y
Er O1 Er . 2_566 106.36(7) y
C1 O2 Al . . 130.6(2) ?
C1 O2 Er . . 126.1(2) y
Al O2 Er . . 101.16(8) y
C3 O3 Al . . 125.5(2) y
C3 O3 Er . . 124.7(2) y
Al O3 Er . . 100.50(9) y
C4 O4 Er . . 131.2(2) y
C4 O4 O5 . . 119.9(2) ?
Er O4 O5 . . 100.47(8) ?
C5 O5 Al . . 127.1(2) ?
C5 O5 O4 . . 143.1(2) ?
Al O5 O4 . . 89.73(9) ?
C6 O6 Al . . 137.5(2) ?
C7 O7 Er . . 172.8(3) ?
O2 C1 C2A . . 110.5(3) ?
O2 C1 C2B . . 110.8(3) ?
C2A C1 C2B . . 111.5(3) ?
O1 C2 C1B . 2_566 112.5(4) ?
O1 C2 C1A . 2_566 111.5(3) ?
C1B C2 C1A 2_566 2_566 116.9(4) ?
O3 C3 C3B . . 110.4(4) ?
O3 C3 C3A . . 112.6(3) ?
C3B C3 C3A . . 111.4(4) ?
O4 C4 C4B . . 109.6(3) ?
O4 C4 C4A . . 110.8(3) ?
C4B C4 C4A . . 112.7(3) ?
O5 C5 C5B . . 111.0(4) ?
O5 C5 C5A . . 110.4(3) ?
C5B C5 C5A . . 114.2(6) ?
O6 C6 C6A . . 111.0(3) ?
O6 C6 C6B . . 109.0(3) ?
C6A C6 C6B . . 111.3(4) ?
O7 C7 C7B . . 114.1(4) ?
O7 C7 C7A . . 112.0(4) ?
C7B C7 C7A . . 114.4(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Er O7 . 2.040(2) y
Er O1 . 2.241(2) y
Er O1 2_566 2.245(2) ?
Er O2 . 2.346(2) y
Er O3 . 2.355(2) y
Er O4 . 2.406(2) y
Er Al . 3.2041(10) y
Er Er 2_566 3.5918(7) y
Al O6 . 1.697(2) y
Al O5 . 1.740(2) y
Al O2 . 1.774(2) y
Al O3 . 1.785(2) y
O1 C2 . 1.424(4) ?
O1 Er 2_566 2.245(2) ?
O2 C1 . 1.435(3) ?
O3 C3 . 1.439(4) ?
O4 C4 . 1.442(3) ?
O4 O5 . 2.710(3) ?
O5 C5 . 1.430(4) ?
O6 C6 . 1.405(4) ?
O7 C7 . 1.394(4) ?
C1 C2A . 1.503(5) ?
C1 C2B . 1.505(5) ?
C2 C1B 2_566 1.457(7) ?
C2 C1A 2_566 1.478(6) ?
C3 C3B . 1.460(7) ?
C3 C3A . 1.493(6) ?
C4 C4B . 1.507(6) ?
C4 C4A . 1.508(5) ?
C5 C5B . 1.449(7) ?
C5 C5A . 1.486(6) ?
C6 C6A . 1.499(6) ?
C6 C6B . 1.506(6) ?
C7 C7B . 1.435(7) ?
C7 C7A . 1.487(6) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H100 O5 0.84(2) 1.88(3) 2.710(3) 167(3) y