#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318886.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_4318886
loop_
_publ_author_name
'Garth R. Giesbrecht'
'John C. Gordon'
'David L. Clark'
'Brian L. Scott'
'John G. Watkin'
'Kenneth J. Young'
_publ_section_title
;
 Salt-Free Synthesis of Samarium-Aluminum Mixed-Metal Alkoxides: X-ray
 Crystal Structures of
 {[(i-Pr-O)(i-Bu)Al(μ-O-i-Pr)2Sm(O-i-Pr)(HO-i-Pr)](μ-O-i-Pr)}2,
 [(THF)2Sm(O-t-Bu)2(μ-O-t-Bu)2Al(i-Bu)2], Sm(OAr)3(THF)3 (Ar =
 2,4,6-Me3C6H2), [Nd(μ-OAr)(OAr)2(py)2]2 (Ar = 2,4,6-Me3C6H2), and
 (ArO)3Sm[(μ-O-t-Bu)2Al2(O-t-Bu)4] (Ar = 2,6-i-Pr2C6H3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6372
_journal_page_last               6379
_journal_paper_doi               10.1021/ic0203116
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H70 Al O6 Sm'
_chemical_formula_weight         728.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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            4
_cell_length_a                   11.304(2)
_cell_length_b                   22.429(4)
_cell_length_c                   15.768(2)
_cell_measurement_temperature    203(2)
_cell_volume                     3997.8(11)
_computing_cell_refinement       'XSCANS 2.10b (Siemens)'
_computing_data_collection       'XSCANS 2.10b (Siemens)'
_computing_data_reduction        'XSCANS 2.10b (Siemens)'
_computing_molecular_graphics    'SHELXTL PC 4.2/360 (Siemens)'
_computing_publication_material  'SHELXTL PC 4.2/360 (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'w 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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2401
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.524
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.706
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0582
_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)+(0.1078P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1746
_reflns_number_gt                1694
_reflns_number_total             1925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203116_2.cif
_cod_data_source_block           xr117c
_cod_database_code               4318886
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, -z-1/2'
'x, -y, -z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, -z'
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
Sm1 Sm 0.0000 0.34986(2) 0.2500 0.0503(3) Uani 1 4 d S . .
Al1 Al 0.0000 0.20004(17) 0.2500 0.0612(11) Uani 1 4 d S . .
O1 O 0.1131(5) 0.2547(3) 0.2500 0.0504(13) Uani 1 2 d S . .
O2 O 0.1443(7) 0.4095(3) 0.2500 0.099(3) Uani 1 2 d S . .
O3 O 0.0000 0.3487(4) 0.4066(7) 0.133(6) Uani 1 2 d SD . .
C1 C 0.2382(9) 0.2490(4) 0.2500 0.063(3) Uani 1 2 d S . .
C2 C 0.2745(10) 0.1822(5) 0.2500 0.076(3) Uani 1 2 d S . .
C3 C 0.2860(8) 0.2778(4) 0.3309(7) 0.095(3) Uani 1 1 d . . .
C4 C 0.2220(14) 0.4572(6) 0.2762(13) 0.104(12) Uani 0.50 1 d PD . .
C5 C 0.3445(15) 0.4458(8) 0.2500 0.168(10) Uani 1 2 d SD . .
C6 C 0.168(2) 0.5130(7) 0.2500 0.198(12) Uani 1 2 d SD . .
C7 C 0.236(3) 0.4679(13) 0.3669(11) 0.44(7) Uani 0.50 1 d PD . .
C8 C 0.052(2) 0.3208(13) 0.4751(14) 0.134(11) Uani 0.50 1 d PD . .
C9 C 0.0000 0.3423(18) 0.5465(17) 0.24(2) Uani 1 2 d S . .
C10 C -0.057(3) 0.3990(13) 0.5328(15) 0.149(14) Uani 0.50 1 d P . .
C11 C -0.088(4) 0.390(3) 0.446(2) 0.35(4) Uani 0.50 1 d PD . .
C12 C 0.0000 0.1817(6) 0.3664(9) 0.042(3) Uani 0.50 2 d SPD . .
C12' C 0.0000 0.1313(8) 0.3175(11) 0.051(4) Uani 0.50 2 d SP . .
C13 C 0.0000 0.1345(8) 0.4226(9) 0.112(5) Uani 1 2 d SD . .
C14 C 0.0000 0.0785(12) 0.432(3) 0.34(3) Uani 1 2 d S . .
C15 C 0.100(3) 0.1559(15) 0.470(3) 0.20(2) Uani 0.50 1 d PD . .
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'
Sm Sm -0.1638 3.4418 '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
O2 Sm1 O2 101.3(5) . 11_556 ?
O2 Sm1 O3 90.38(14) . 10_556 ?
O2 Sm1 O3 90.38(14) 11_556 10_556 ?
O2 Sm1 O3 90.38(14) . . ?
O2 Sm1 O3 90.38(14) 11_556 . ?
O3 Sm1 O3 178.8(4) 10_556 . ?
O2 Sm1 O1 160.3(3) . 11_556 ?
O2 Sm1 O1 98.4(3) 11_556 11_556 ?
O3 Sm1 O1 89.49(19) 10_556 11_556 ?
O3 Sm1 O1 89.49(19) . 11_556 ?
O2 Sm1 O1 98.4(3) . . ?
O2 Sm1 O1 160.3(3) 11_556 . ?
O3 Sm1 O1 89.49(19) 10_556 . ?
O3 Sm1 O1 89.49(19) . . ?
O1 Sm1 O1 61.9(3) 11_556 . ?
O2 Sm1 Al1 129.3(2) . . ?
O2 Sm1 Al1 129.3(2) 11_556 . ?
O3 Sm1 Al1 89.4(2) 10_556 . ?
O3 Sm1 Al1 89.4(2) . . ?
O1 Sm1 Al1 30.93(13) 11_556 . ?
O1 Sm1 Al1 30.93(13) . . ?
O1 Al1 O1 92.4(4) . 11_556 ?
O1 Al1 C12' 124.7(3) . 10_556 ?
O1 Al1 C12' 124.7(3) 11_556 10_556 ?
O1 Al1 C12' 124.7(3) . . ?
O1 Al1 C12' 124.7(3) 11_556 . ?
C12' Al1 C12' 69.3(11) 10_556 . ?
O1 Al1 C12 98.7(3) . 10_556 ?
O1 Al1 C12 98.7(3) 11_556 10_556 ?
C12' Al1 C12 42.7(8) 10_556 10_556 ?
C12' Al1 C12 112.0(7) . 10_556 ?
O1 Al1 C12 98.7(3) . . ?
O1 Al1 C12 98.7(3) 11_556 . ?
C12' Al1 C12 112.0(7) 10_556 . ?
C12' Al1 C12 42.7(8) . . ?
C12 Al1 C12 154.7(9) 10_556 . ?
O1 Al1 Sm1 46.2(2) . . ?
O1 Al1 Sm1 46.2(2) 11_556 . ?
C12' Al1 Sm1 145.4(6) 10_556 . ?
C12' Al1 Sm1 145.4(6) . . ?
C12 Al1 Sm1 102.7(5) 10_556 . ?
C12 Al1 Sm1 102.7(5) . . ?
C1 O1 Al1 131.1(6) . . ?
C1 O1 Sm1 126.0(5) . . ?
Al1 O1 Sm1 102.9(3) . . ?
C4 O2 C4 33.3(17) . 10_556 ?
C4 O2 Sm1 160.0(8) . . ?
C4 O2 Sm1 160.0(8) 10_556 . ?
C8 O3 C8 50(2) 4 . ?
C8 O3 C11 103.8(19) 4 4 ?
C8 O3 C11 71(3) . 4 ?
C8 O3 C11 71(3) 4 . ?
C8 O3 C11 103.8(19) . . ?
C11 O3 C11 83(4) 4 . ?
C8 O3 Sm1 141.9(11) 4 . ?
C8 O3 Sm1 141.9(11) . . ?
C11 O3 Sm1 114.2(15) 4 . ?
C11 O3 Sm1 114.2(15) . . ?
O1 C1 C3 108.3(6) . . ?
O1 C1 C3 108.3(6) . 10_556 ?
C3 C1 C3 113.2(11) . 10_556 ?
O1 C1 C2 110.4(8) . . ?
C3 C1 C2 108.3(6) . . ?
C3 C1 C2 108.3(6) 10_556 . ?
C4 C4 C7 7.2(10) 10_556 10_556 ?
C4 C4 O2 73.4(8) 10_556 . ?
C7 C4 O2 80.6(12) 10_556 . ?
C4 C4 C6 73.5(9) 10_556 . ?
C7 C4 C6 69.9(11) 10_556 . ?
O2 C4 C6 107.7(13) . . ?
C4 C4 C5 73.6(9) 10_556 . ?
C7 C4 C5 70.9(12) 10_556 . ?
O2 C4 C5 111.3(12) . . ?
C6 C4 C5 117.6(17) . . ?
C4 C4 C7 168.6(15) 10_556 . ?
C7 C4 C7 161(2) 10_556 . ?
O2 C4 C7 118(2) . . ?
C6 C4 C7 100.5(13) . . ?
C5 C4 C7 101.7(15) . . ?
C4 C5 C4 32.8(17) . 10_556 ?
C4 C6 C4 33.1(18) 10_556 . ?
C4 C7 C4 4.1(6) 10_556 . ?
C8 C8 C9 64.5(14) 4 . ?
C8 C8 O3 64.9(12) 4 . ?
C9 C8 O3 107.7(19) . . ?
C8 C8 C11 104(2) 4 4 ?
C9 C8 C11 90(3) . 4 ?
O3 C8 C11 58.0(16) . 4 ?
C8 C8 C10 91.8(13) 4 4 ?
C9 C8 C10 46.9(18) . 4 ?
O3 C8 C10 88.3(16) . 4 ?
C11 C8 C10 44.9(16) 4 4 ?
C8 C9 C8 51(3) 4 . ?
C8 C9 C10 90(2) 4 . ?
C8 C9 C10 113(2) . . ?
C8 C9 C10 113(2) 4 4 ?
C8 C9 C10 90(2) . 4 ?
C10 C9 C10 53(3) . 4 ?
C10 C10 C11 104(2) 4 . ?
C10 C10 C9 63.3(16) 4 . ?
C11 C10 C9 98(2) . . ?
C10 C10 C8 88.2(13) 4 4 ?
C11 C10 C8 56(2) . 4 ?
C9 C10 C8 43.4(13) . 4 ?
C10 C11 O3 109(2) . . ?
C10 C11 C8 79(3) . 4 ?
O3 C11 C8 51.1(15) . 4 ?
C10 C11 C11 76(2) . 4 ?
O3 C11 C11 48(2) . 4 ?
C8 C11 C11 76(2) 4 4 ?
C12' C12 C13 74.3(12) . . ?
C12' C12 Al1 68.3(10) . . ?
C13 C12 Al1 142.6(12) . . ?
C12 C12' C13 53.2(9) . . ?
C12 C12' Al1 69.0(10) . . ?
C13 C12' Al1 122.2(13) . . ?
C14 C13 C12 147(3) . . ?
C14 C13 C15 106(2) . . ?
C12 C13 C15 94(2) . . ?
C14 C13 C15 106(2) . 4 ?
C12 C13 C15 94(2) . 4 ?
C15 C13 C15 104(4) . 4 ?
C14 C13 C12' 94(3) . . ?
C12 C13 C12' 52.5(11) . . ?
C15 C13 C12' 122(2) . . ?
C15 C13 C12' 122(2) 4 . ?
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
Sm1 O2 2.109(7) . ?
Sm1 O2 2.109(7) 11_556 ?
Sm1 O3 2.470(10) 10_556 ?
Sm1 O3 2.470(10) . ?
Sm1 O1 2.488(6) 11_556 ?
Sm1 O1 2.488(6) . ?
Sm1 Al1 3.360(4) . ?
Al1 O1 1.771(6) . ?
Al1 O1 1.771(6) 11_556 ?
Al1 C12' 1.873(18) 10_556 ?
Al1 C12' 1.873(18) . ?
Al1 C12 1.882(14) 10_556 ?
Al1 C12 1.882(14) . ?
O1 C1 1.420(12) . ?
O2 C4 1.445(16) . ?
O2 C4 1.445(16) 10_556 ?
O3 C8 1.379(16) 4 ?
O3 C8 1.379(16) . ?
O3 C11 1.502(18) 4 ?
O3 C11 1.502(18) . ?
C1 C3 1.529(11) . ?
C1 C3 1.529(11) 10_556 ?
C1 C2 1.555(14) . ?
C4 C4 0.83(4) 10_556 ?
C4 C7 2.27(3) 10_556 ?
C4 C6 1.452(16) . ?
C4 C5 1.467(17) . ?
C4 C7 1.458(18) . ?
C5 C4 1.467(16) 10_556 ?
C6 C4 1.452(16) 10_556 ?
C7 C4 2.27(3) 10_556 ?
C8 C8 1.17(5) 4 ?
C8 C9 1.36(3) . ?
C8 C11 1.68(6) 4 ?
C8 C10 1.98(4) 4 ?
C9 C8 1.36(3) 4 ?
C9 C10 1.44(4) . ?
C9 C10 1.44(4) 4 ?
C10 C10 1.30(7) 4 ?
C10 C11 1.42(4) . ?
C10 C8 1.98(4) 4 ?
C11 C8 1.68(6) 4 ?
C11 C11 2.00(9) 4 ?
C12 C12' 1.37(2) . ?
C12 C13 1.380(16) . ?
C12' C13 1.66(2) . ?
C13 C14 1.26(3) . ?
C13 C15 1.432(13) . ?
C13 C15 1.432(13) 4 ?
