#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318887.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_4318887
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            'C42 H40 O6 Sm'
_chemical_formula_weight         791.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   16.5822(9)
_cell_length_b                   15.5668(9)
_cell_length_c                   29.9017(18)
_cell_measurement_temperature    203(2)
_cell_volume                     7718.6(8)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       'ω and φ 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5577
_diffrn_reflns_theta_full        23.45
_diffrn_reflns_theta_max         23.45
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0353P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                4092
_reflns_number_total             5577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203116_3.cif
_cod_data_source_block           ccd231a
_cod_database_code               4318887
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.009383(14) 0.384465(17) 0.351597(9) 0.04199(11) Uani 1 1 d . . .
O1 O 0.1260(2) 0.4069(2) 0.38107(12) 0.0556(10) Uani 1 1 d . . .
O2 O 0.0291(2) 0.4178(2) 0.28225(12) 0.0537(10) Uani 1 1 d . . .
O3 O -0.0620(2) 0.4913(2) 0.37547(12) 0.0527(10) Uani 1 1 d . . .
O4 O -0.0185(2) 0.2997(2) 0.42364(13) 0.0589(10) Uani 1 1 d . . .
O5 O 0.0547(2) 0.2351(2) 0.32966(12) 0.0522(10) Uani 1 1 d . . .
O6 O -0.1216(2) 0.3128(2) 0.33003(13) 0.0520(10) Uani 1 1 d . . .
C1 C 0.1954(3) 0.4332(4) 0.39904(18) 0.0549(16) Uani 1 1 d . . .
C2 C 0.2635(3) 0.3795(4) 0.3977(2) 0.0621(17) Uani 1 1 d . . .
C3 C 0.3343(4) 0.4081(5) 0.4176(2) 0.0717(19) Uani 1 1 d . . .
H3 H 0.3794 0.3726 0.4166 0.086 Uiso 1 1 calc R . .
C4 C 0.3409(4) 0.4867(5) 0.4387(2) 0.0675(19) Uani 1 1 d . . .
C5 C 0.2743(4) 0.5386(4) 0.43795(18) 0.0685(18) Uani 1 1 d . . .
H5 H 0.2781 0.5930 0.4506 0.082 Uiso 1 1 calc R . .
C6 C 0.2012(3) 0.5140(4) 0.41919(18) 0.0561(16) Uani 1 1 d . . .
C7 C 0.2580(4) 0.2939(4) 0.3754(3) 0.094(2) Uani 1 1 d . . .
H7A H 0.2046 0.2860 0.3637 0.141 Uiso 1 1 calc R . .
H7B H 0.2696 0.2495 0.3967 0.141 Uiso 1 1 calc R . .
H7C H 0.2963 0.2912 0.3514 0.141 Uiso 1 1 calc R . .
C8 C 0.4186(4) 0.5152(5) 0.4605(2) 0.110(3) Uani 1 1 d . . .
H8A H 0.4578 0.4701 0.4584 0.165 Uiso 1 1 calc R . .
H8B H 0.4087 0.5283 0.4914 0.165 Uiso 1 1 calc R . .
H8C H 0.4386 0.5655 0.4456 0.165 Uiso 1 1 calc R . .
C9 C 0.1293(4) 0.5721(4) 0.4194(2) 0.085(2) Uani 1 1 d . . .
H9A H 0.1425 0.6245 0.4347 0.127 Uiso 1 1 calc R . .
H9B H 0.0854 0.5442 0.4344 0.127 Uiso 1 1 calc R . .
H9C H 0.1139 0.5849 0.3892 0.127 Uiso 1 1 calc R . .
C10 C 0.0563(3) 0.4413(3) 0.2421(2) 0.0475(14) Uani 1 1 d . . .
C11 C 0.0120(3) 0.4221(4) 0.2037(2) 0.0520(14) Uani 1 1 d . . .
C12 C 0.0428(4) 0.4466(4) 0.16169(19) 0.0613(17) Uani 1 1 d . . .
H12 H 0.0134 0.4331 0.1361 0.074 Uiso 1 1 calc R . .
C13 C 0.1142(4) 0.4894(4) 0.1571(2) 0.0626(17) Uani 1 1 d . . .
C14 C 0.1561(4) 0.5091(4) 0.1954(2) 0.0618(17) Uani 1 1 d . . .
H14 H 0.2041 0.5396 0.1928 0.074 Uiso 1 1 calc R . .
C15 C 0.1300(3) 0.4855(3) 0.2379(2) 0.0550(15) Uani 1 1 d . . .
C16 C -0.0676(3) 0.3775(4) 0.2078(2) 0.0693(18) Uani 1 1 d . . .
H16A H -0.0899 0.3684 0.1785 0.104 Uiso 1 1 calc R . .
H16B H -0.1039 0.4123 0.2250 0.104 Uiso 1 1 calc R . .
H16C H -0.0602 0.3231 0.2223 0.104 Uiso 1 1 calc R . .
C17 C 0.1457(4) 0.5146(5) 0.1114(2) 0.093(2) Uani 1 1 d . . .
H17A H 0.1084 0.4961 0.0888 0.139 Uiso 1 1 calc R . .
H17B H 0.1971 0.4879 0.1064 0.139 Uiso 1 1 calc R . .
H17C H 0.1517 0.5759 0.1099 0.139 Uiso 1 1 calc R . .
C18 C 0.1777(4) 0.5055(5) 0.2796(2) 0.090(2) Uani 1 1 d . . .
H18A H 0.1494 0.4841 0.3053 0.136 Uiso 1 1 calc R . .
H18B H 0.1844 0.5666 0.2822 0.136 Uiso 1 1 calc R . .
H18C H 0.2297 0.4786 0.2777 0.136 Uiso 1 1 calc R . .
C19 C -0.0943(3) 0.5623(3) 0.39350(19) 0.0451(14) Uani 1 1 d . . .
C20 C -0.0816(4) 0.6430(4) 0.3744(2) 0.0687(18) Uani 1 1 d . . .
C21 C -0.1162(5) 0.7159(4) 0.3943(3) 0.082(2) Uani 1 1 d . . .
H21 H -0.1089 0.7693 0.3810 0.099 Uiso 1 1 calc R . .
C22 C -0.1609(4) 0.7100(5) 0.4334(3) 0.087(2) Uani 1 1 d . . .
C23 C -0.1727(3) 0.6311(4) 0.4510(2) 0.0701(19) Uani 1 1 d . . .
H23 H -0.2041 0.6259 0.4766 0.084 Uiso 1 1 calc R . .
C24 C -0.1401(3) 0.5578(4) 0.4324(2) 0.0526(15) Uani 1 1 d . . .
C25 C -0.0334(5) 0.6481(5) 0.3322(3) 0.111(3) Uani 1 1 d . . .
H25A H -0.0290 0.7070 0.3230 0.167 Uiso 1 1 calc R . .
H25B H -0.0596 0.6154 0.3092 0.167 Uiso 1 1 calc R . .
H25C H 0.0195 0.6251 0.3374 0.167 Uiso 1 1 calc R . .
C26 C -0.1913(4) 0.7924(4) 0.4556(3) 0.139(4) Uani 1 1 d . . .
H26A H -0.2205 0.7782 0.4823 0.208 Uiso 1 1 calc R . .
H26B H -0.2261 0.8225 0.4353 0.208 Uiso 1 1 calc R . .
H26C H -0.1462 0.8283 0.4631 0.208 Uiso 1 1 calc R . .
C27 C -0.1540(4) 0.4716(4) 0.4539(2) 0.0700(18) Uani 1 1 d . . .
H27A H -0.1274 0.4278 0.4368 0.105 Uiso 1 1 calc R . .
H27B H -0.2108 0.4598 0.4549 0.105 Uiso 1 1 calc R . .
H27C H -0.1327 0.4721 0.4838 0.105 Uiso 1 1 calc R . .
C28 C -0.0817(4) 0.2429(4) 0.4326(2) 0.0656(18) Uani 1 1 d . . .
H28A H -0.0712 0.1880 0.4184 0.079 Uiso 1 1 calc R . .
H28B H -0.1317 0.2657 0.4206 0.079 Uiso 1 1 calc R . .
C29 C -0.0893(5) 0.2310(6) 0.4825(3) 0.131(4) Uani 1 1 d . . .
H29A H -0.0928 0.1705 0.4900 0.157 Uiso 1 1 calc R . .
H29B H -0.1370 0.2599 0.4938 0.157 Uiso 1 1 calc R . .
C30 C -0.0138(6) 0.2704(7) 0.5021(2) 0.133(4) Uani 1 1 d . . .
H30A H 0.0220 0.2263 0.5136 0.160 Uiso 1 1 calc R . .
H30B H -0.0269 0.3100 0.5260 0.160 Uiso 1 1 calc R . .
C31 C 0.0249(4) 0.3175(5) 0.4627(2) 0.0733(19) Uani 1 1 d . . .
H31A H 0.0248 0.3789 0.4684 0.088 Uiso 1 1 calc R . .
H31B H 0.0804 0.2990 0.4592 0.088 Uiso 1 1 calc R . .
C32 C 0.0830(4) 0.2179(4) 0.2850(2) 0.082(2) Uani 1 1 d . . .
H32A H 0.1286 0.2545 0.2778 0.099 Uiso 1 1 calc R . .
H32B H 0.0405 0.2285 0.2633 0.099 Uiso 1 1 calc R . .
C33 C 0.1073(4) 0.1260(4) 0.2842(2) 0.0723(18) Uani 1 1 d . . .
H33A H 0.1530 0.1172 0.2645 0.087 Uiso 1 1 calc R . .
H33B H 0.0631 0.0899 0.2744 0.087 Uiso 1 1 calc R . .
C34 C 0.1296(4) 0.1065(4) 0.3316(2) 0.0605(16) Uani 1 1 d . . .
H34A H 0.1221 0.0460 0.3383 0.073 Uiso 1 1 calc R . .
H34B H 0.1851 0.1222 0.3378 0.073 Uiso 1 1 calc R . .
C35 C 0.0724(3) 0.1608(3) 0.3576(2) 0.0548(15) Uani 1 1 d . . .
H35A H 0.0234 0.1292 0.3642 0.066 Uiso 1 1 calc R . .
H35B H 0.0967 0.1788 0.3856 0.066 Uiso 1 1 calc R . .
C36 C -0.1361(4) 0.2304(4) 0.3112(3) 0.093(3) Uani 1 1 d . . .
H36A H -0.1246 0.1858 0.3330 0.111 Uiso 1 1 calc R . .
H36B H -0.1022 0.2214 0.2853 0.111 Uiso 1 1 calc R . .
C37 C -0.2210(4) 0.2281(5) 0.2985(3) 0.141(4) Uani 1 1 d . . .
H37A H -0.2270 0.2006 0.2696 0.169 Uiso 1 1 calc R . .
H37B H -0.2516 0.1957 0.3204 0.169 Uiso 1 1 calc R . .
C38 C -0.2497(4) 0.3140(4) 0.2965(3) 0.090(2) Uani 1 1 d . . .
H38A H -0.3045 0.3178 0.3077 0.108 Uiso 1 1 calc R . .
H38B H -0.2484 0.3355 0.2660 0.108 Uiso 1 1 calc R . .
C39 C -0.1935(3) 0.3633(4) 0.3255(2) 0.079(2) Uani 1 1 d . . .
H39A H -0.1811 0.4184 0.3120 0.094 Uiso 1 1 calc R . .
H39B H -0.2177 0.3733 0.3546 0.094 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'
O O 0.0106 0.0060 '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
O1 Sm1 O2 102.57(14) . . ?
O1 Sm1 O3 103.39(13) . . ?
O2 Sm1 O3 102.39(14) . . ?
O1 Sm1 O6 161.49(13) . . ?
O2 Sm1 O6 89.51(13) . . ?
O3 Sm1 O6 87.34(12) . . ?
O1 Sm1 O5 89.34(13) . . ?
O2 Sm1 O5 85.83(13) . . ?
O3 Sm1 O5 162.73(12) . . ?
O6 Sm1 O5 77.46(11) . . ?
O1 Sm1 O4 84.36(13) . . ?
O2 Sm1 O4 162.75(13) . . ?
O3 Sm1 O4 91.12(13) . . ?
O6 Sm1 O4 80.35(12) . . ?
O5 Sm1 O4 78.40(12) . . ?
C1 O1 Sm1 171.4(4) . . ?
C10 O2 Sm1 168.6(4) . . ?
C19 O3 Sm1 170.0(3) . . ?
C28 O4 C31 110.6(5) . . ?
C28 O4 Sm1 128.3(4) . . ?
C31 O4 Sm1 120.4(3) . . ?
C32 O5 C35 108.6(4) . . ?
C32 O5 Sm1 120.5(3) . . ?
C35 O5 Sm1 129.8(3) . . ?
C36 O6 C39 108.4(4) . . ?
C36 O6 Sm1 130.2(3) . . ?
C39 O6 Sm1 119.8(3) . . ?
O1 C1 C6 120.6(5) . . ?
O1 C1 C2 119.9(6) . . ?
C6 C1 C2 119.5(5) . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 C7 121.9(6) . . ?
C1 C2 C7 119.6(5) . . ?
C4 C3 C2 123.1(6) . . ?
C5 C4 C3 116.9(6) . . ?
C5 C4 C8 121.4(7) . . ?
C3 C4 C8 121.7(7) . . ?
C4 C5 C6 123.2(6) . . ?
C5 C6 C1 118.8(6) . . ?
C5 C6 C9 121.8(6) . . ?
C1 C6 C9 119.4(5) . . ?
O2 C10 C11 120.3(5) . . ?
O2 C10 C15 120.5(5) . . ?
C11 C10 C15 119.2(6) . . ?
C10 C11 C12 119.1(6) . . ?
C10 C11 C16 119.8(5) . . ?
C12 C11 C16 121.1(6) . . ?
C13 C12 C11 122.3(6) . . ?
C12 C13 C14 117.7(6) . . ?
C12 C13 C17 121.0(7) . . ?
C14 C13 C17 121.3(6) . . ?
C13 C14 C15 123.0(6) . . ?
C14 C15 C10 118.7(6) . . ?
C14 C15 C18 122.5(5) . . ?
C10 C15 C18 118.8(5) . . ?
O3 C19 C24 120.8(5) . . ?
O3 C19 C20 121.1(6) . . ?
C24 C19 C20 118.0(6) . . ?
C19 C20 C21 119.4(7) . . ?
C19 C20 C25 118.2(7) . . ?
C21 C20 C25 122.3(7) . . ?
C22 C21 C20 121.6(7) . . ?
C23 C22 C21 117.7(7) . . ?
C23 C22 C26 123.1(9) . . ?
C21 C22 C26 119.1(8) . . ?
C22 C23 C24 122.6(7) . . ?
C23 C24 C19 120.6(6) . . ?
C23 C24 C27 120.3(6) . . ?
C19 C24 C27 119.1(5) . . ?
O4 C28 C29 109.2(6) . . ?
C28 C29 C30 105.3(6) . . ?
C29 C30 C31 104.1(6) . . ?
O4 C31 C30 109.4(6) . . ?
O5 C32 C33 106.2(5) . . ?
C32 C33 C34 104.4(5) . . ?
C35 C34 C33 102.8(5) . . ?
O5 C35 C34 106.3(5) . . ?
O6 C36 C37 106.8(5) . . ?
C38 C37 C36 108.2(6) . . ?
C37 C38 C39 104.5(5) . . ?
O6 C39 C38 107.1(5) . . ?
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 O1 2.154(3) . ?
Sm1 O2 2.163(4) . ?
Sm1 O3 2.162(4) . ?
Sm1 O6 2.526(3) . ?
Sm1 O5 2.531(3) . ?
Sm1 O4 2.568(4) . ?
O1 C1 1.334(6) . ?
O2 C10 1.333(6) . ?
O3 C19 1.341(6) . ?
O4 C28 1.397(6) . ?
O4 C31 1.400(7) . ?
O5 C32 1.442(6) . ?
O5 C35 1.456(6) . ?
O6 C36 1.421(6) . ?
O6 C39 1.435(6) . ?
C1 C6 1.399(8) . ?
C1 C2 1.405(8) . ?
C2 C3 1.389(8) . ?
C2 C7 1.493(8) . ?
C3 C4 1.381(8) . ?
C4 C5 1.370(9) . ?
C4 C8 1.511(8) . ?
C5 C6 1.389(7) . ?
C6 C9 1.496(8) . ?
C10 C11 1.395(7) . ?
C10 C15 1.409(7) . ?
C11 C12 1.408(7) . ?
C11 C16 1.498(7) . ?
C12 C13 1.365(8) . ?
C13 C14 1.373(8) . ?
C13 C17 1.517(8) . ?
C14 C15 1.391(8) . ?
C15 C18 1.508(8) . ?
C19 C24 1.391(7) . ?
C19 C20 1.396(8) . ?
C20 C21 1.404(9) . ?
C20 C25 1.495(9) . ?
C21 C22 1.386(10) . ?
C22 C23 1.352(9) . ?
C22 C26 1.529(9) . ?
C23 C24 1.379(7) . ?
C24 C27 1.507(7) . ?
C28 C29 1.511(10) . ?
C29 C30 1.512(11) . ?
C30 C31 1.528(11) . ?
C32 C33 1.487(8) . ?
C33 C34 1.496(8) . ?
C34 C35 1.489(7) . ?
C36 C37 1.458(8) . ?
C37 C38 1.421(8) . ?
C38 C39 1.486(8) . ?
