#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:33:56 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180109 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/07/7100777.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_7100777
loop_
_publ_author_name
'Michael Guy Gardiner'
'Jun Wang'
_publ_section_title
;
C-H Activation (g-deprotonation) of a Sm(III)
bis(trimethylsilyl)amide complex via macrocyclic stabilisation of the
sodium counter ion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b417679k
_journal_year                    2005
_chemical_formula_sum            'C42 H66 N3 O2 Si2 Sm'
_chemical_formula_weight         851.51
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 113.1423(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.17170(10)
_cell_length_b                   27.7942(3)
_cell_length_c                   13.62490(10)
_cell_measurement_temperature    123(2)
_cell_volume                     4238.43(7)
_diffrn_ambient_temperature      123(2)
_exptl_crystal_density_diffrn    1.334
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7100777
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.939181(12) 0.111256(5) 0.207926(11) 0.01390(5) Uani 1 1 d . . .
N1 N 0.92084(19) 0.12508(8) 0.00944(17) 0.0158(5) Uani 1 1 d . . .
N2 N 1.09065(18) 0.03903(8) 0.28982(16) 0.0142(5) Uani 1 1 d . . .
O1 O 1.16266(15) 0.13763(6) 0.22979(13) 0.0152(4) Uani 1 1 d . . .
O2 O 0.82716(15) 0.03473(6) 0.08787(13) 0.0163(4) Uani 1 1 d . . .
C1 C 0.8021(2) 0.12561(10) -0.0040(2) 0.0165(6) Uani 1 1 d . . .
C2 C 0.7763(2) 0.16784(10) 0.0362(2) 0.0185(6) Uani 1 1 d . . .
H2 H 0.7035 0.1762 0.0387 0.022 Uiso 1 1 calc R . .
C3 C 0.8812(2) 0.19586(10) 0.0727(2) 0.0193(6) Uani 1 1 d . . .
H3 H 0.8914 0.2262 0.1038 0.023 Uiso 1 1 calc R . .
C4 C 0.9667(2) 0.16887(9) 0.0527(2) 0.0154(6) Uani 1 1 d . . .
C5 C 1.0912(2) 0.18269(9) 0.0620(2) 0.0157(6) Uani 1 1 d . . .
C6 C 1.1218(2) 0.23485(9) 0.1039(2) 0.0208(6) Uani 1 1 d . . .
H6A H 1.0667 0.2566 0.0520 0.025 Uiso 1 1 calc R . .
H6B H 1.1087 0.2379 0.1694 0.025 Uiso 1 1 calc R . .
C7 C 1.2488(2) 0.25090(10) 0.1256(2) 0.0275(7) Uani 1 1 d . . .
H7A H 1.2597 0.2835 0.1508 0.041 Uiso 1 1 calc R . .
H7B H 1.2624 0.2490 0.0609 0.041 Uiso 1 1 calc R . .
H7C H 1.3044 0.2304 0.1786 0.041 Uiso 1 1 calc R . .
C8 C 1.0963(2) 0.17717(10) -0.0497(2) 0.0204(6) Uani 1 1 d . . .
H8A H 1.1755 0.1863 -0.0441 0.024 Uiso 1 1 calc R . .
H8B H 1.0848 0.1435 -0.0701 0.024 Uiso 1 1 calc R . .
C9 C 1.0049(3) 0.20676(11) -0.1379(2) 0.0303(7) Uani 1 1 d . . .
H9A H 1.0141 0.2012 -0.2038 0.046 Uiso 1 1 calc R . .
H9B H 1.0170 0.2403 -0.1200 0.046 Uiso 1 1 calc R . .
H9C H 0.9259 0.1975 -0.1457 0.046 Uiso 1 1 calc R . .
C10 C 1.1798(2) 0.14841(9) 0.1362(2) 0.0146(6) Uani 1 1 d . . .
C11 C 1.2810(2) 0.12757(10) 0.1413(2) 0.0197(6) Uani 1 1 d . . .
H11 H 1.3127 0.1291 0.0895 0.024 Uiso 1 1 calc R . .
C12 C 1.3319(2) 0.10253(9) 0.2411(2) 0.0199(6) Uani 1 1 d . . .
H12 H 1.4023 0.0848 0.2655 0.024 Uiso 1 1 calc R . .
C13 C 1.2595(2) 0.10929(9) 0.2927(2) 0.0163(6) Uani 1 1 d . . .
C14 C 1.2557(2) 0.09331(10) 0.3963(2) 0.0167(6) Uani 1 1 d . . .
C15 C 1.2790(2) 0.13568(10) 0.4754(2) 0.0232(6) Uani 1 1 d . . .
H15A H 1.2102 0.1569 0.4499 0.028 Uiso 1 1 calc R . .
H15B H 1.2859 0.1230 0.5439 0.028 Uiso 1 1 calc R . .
C16 C 1.3903(3) 0.16522(12) 0.4918(2) 0.0359(8) Uani 1 1 d . . .
H16A H 1.3978 0.1907 0.5415 0.054 Uiso 1 1 calc R . .
H16B H 1.3838 0.1786 0.4248 0.054 Uiso 1 1 calc R . .
H16C H 1.4596 0.1449 0.5194 0.054 Uiso 1 1 calc R . .
C17 C 1.3514(2) 0.05321(10) 0.4419(2) 0.0218(6) Uani 1 1 d . . .
H17A H 1.3348 0.0279 0.3889 0.026 Uiso 1 1 calc R . .
H17B H 1.4290 0.0666 0.4531 0.026 Uiso 1 1 calc R . .
C18 C 1.3580(3) 0.03086(12) 0.5466(2) 0.0374(8) Uani 1 1 d . . .
H18A H 1.4192 0.0066 0.5691 0.056 Uiso 1 1 calc R . .
H18B H 1.2825 0.0165 0.5360 0.056 Uiso 1 1 calc R . .
H18C H 1.3766 0.0554 0.6003 0.056 Uiso 1 1 calc R . .
C19 C 1.1336(2) 0.07218(9) 0.3710(2) 0.0148(6) Uani 1 1 d . . .
C20 C 1.0563(2) 0.07692(10) 0.4237(2) 0.0178(6) Uani 1 1 d . . .
H20 H 1.0641 0.0980 0.4790 0.021 Uiso 1 1 calc R . .
C21 C 0.9645(2) 0.04337(9) 0.3759(2) 0.0164(6) Uani 1 1 d . . .
H21 H 0.8993 0.0378 0.3939 0.020 Uiso 1 1 calc R . .
C22 C 0.9892(2) 0.02002(9) 0.2966(2) 0.0145(6) Uani 1 1 d . . .
C23 C 0.9330(2) -0.02357(10) 0.2299(2) 0.0158(6) Uani 1 1 d . . .
C24 C 1.0324(2) -0.06117(10) 0.2476(2) 0.0189(6) Uani 1 1 d . . .
H24A H 0.9972 -0.0894 0.2049 0.023 Uiso 1 1 calc R . .
H24B H 1.0900 -0.0479 0.2221 0.023 Uiso 1 1 calc R . .
C25 C 1.0982(3) -0.07676(11) 0.3634(2) 0.0287(7) Uani 1 1 d . . .
H25A H 1.1579 -0.1002 0.3677 0.043 Uiso 1 1 calc R . .
H25B H 1.0424 -0.0906 0.3892 0.043 Uiso 1 1 calc R . .
H25C H 1.1357 -0.0493 0.4062 0.043 Uiso 1 1 calc R . .
C26 C 0.8316(2) -0.04410(10) 0.2606(2) 0.0203(6) Uani 1 1 d . . .
H26A H 0.8617 -0.0468 0.3377 0.024 Uiso 1 1 calc R . .
H26B H 0.7662 -0.0212 0.2387 0.024 Uiso 1 1 calc R . .
C27 C 0.7824(3) -0.09299(10) 0.2121(2) 0.0296(7) Uani 1 1 d . . .
H27A H 0.7208 -0.1027 0.2353 0.044 Uiso 1 1 calc R . .
H27B H 0.8456 -0.1163 0.2349 0.044 Uiso 1 1 calc R . .
H27C H 0.7498 -0.0906 0.1357 0.044 Uiso 1 1 calc R . .
C28 C 0.8848(2) -0.01033(9) 0.1138(2) 0.0166(6) Uani 1 1 d . . .
C29 C 0.8817(2) -0.03115(10) 0.0241(2) 0.0196(6) Uani 1 1 d . . .
H29 H 0.9152 -0.0607 0.0194 0.023 Uiso 1 1 calc R . .
C30 C 0.8180(2) 0.00010(10) -0.0628(2) 0.0210(6) Uani 1 1 d . . .
H30 H 0.8020 -0.0056 -0.1344 0.025 Uiso 1 1 calc R . .
C31 C 0.7853(2) 0.03905(10) -0.0231(2) 0.0164(6) Uani 1 1 d . . .
C32 C 0.7207(2) 0.08517(10) -0.0658(2) 0.0173(6) Uani 1 1 d . . .
C33 C 0.6006(2) 0.08586(11) -0.0530(2) 0.0238(7) Uani 1 1 d . . .
H33A H 0.6164 0.0858 0.0226 0.029 Uiso 1 1 calc R . .
H33B H 0.5594 0.1156 -0.0829 0.029 Uiso 1 1 calc R . .
C34 C 0.5187(3) 0.04403(12) -0.1057(3) 0.0373(8) Uani 1 1 d . . .
H34A H 0.4464 0.0468 -0.0936 0.056 Uiso 1 1 calc R . .
H34B H 0.5579 0.0143 -0.0758 0.056 Uiso 1 1 calc R . .
H34C H 0.5000 0.0444 -0.1810 0.056 Uiso 1 1 calc R . .
C35 C 0.7025(2) 0.09011(11) -0.1850(2) 0.0231(6) Uani 1 1 d . . .
H35A H 0.7802 0.0900 -0.1893 0.028 Uiso 1 1 calc R . .
H35B H 0.6589 0.0622 -0.2237 0.028 Uiso 1 1 calc R . .
C36 C 0.6357(3) 0.13519(12) -0.2400(2) 0.0357(8) Uani 1 1 d . . .
H36A H 0.6292 0.1358 -0.3125 0.054 Uiso 1 1 calc R . .
H36B H 0.6784 0.1631 -0.2031 0.054 Uiso 1 1 calc R . .
H36C H 0.5572 0.1351 -0.2391 0.054 Uiso 1 1 calc R . .
N3 N 0.84240(19) 0.15566(8) 0.29364(17) 0.0175(5) Uani 1 1 d . . .
Si1 Si 0.69960(7) 0.14158(3) 0.27926(6) 0.01936(17) Uani 1 1 d . . .
C37 C 0.6631(2) 0.07656(10) 0.2402(2) 0.0251(7) Uani 1 1 d . . .
H37A H 0.6753 0.0701 0.1760 0.038 Uiso 1 1 calc R . .
H37B H 0.5812 0.0704 0.2282 0.038 Uiso 1 1 calc R . .
H37C H 0.7142 0.0562 0.2965 0.038 Uiso 1 1 calc R . .
C38 C 0.5814(2) 0.17875(10) 0.1761(2) 0.0273(7) Uani 1 1 d . . .
H38A H 0.5912 0.1769 0.1097 0.041 Uiso 1 1 calc R . .
H38B H 0.5887 0.2116 0.1994 0.041 Uiso 1 1 calc R . .
H38C H 0.5039 0.1668 0.1666 0.041 Uiso 1 1 calc R . .
C39 C 0.6709(3) 0.14815(11) 0.4044(2) 0.0278(7) Uani 1 1 d . . .
H39A H 0.7288 0.1298 0.4607 0.042 Uiso 1 1 calc R . .
H39B H 0.5921 0.1366 0.3918 0.042 Uiso 1 1 calc R . .
H39C H 0.6770 0.1814 0.4247 0.042 Uiso 1 1 calc R . .
Si2 Si 0.90920(7) 0.20544(3) 0.36831(6) 0.02064(18) Uani 1 1 d . . .
C40 C 1.0416(3) 0.22754(11) 0.3412(2) 0.0284(7) Uani 1 1 d . . .
H40A H 1.0172 0.2335 0.2662 0.043 Uiso 1 1 calc R . .
H40B H 1.1033 0.2035 0.3635 0.043 Uiso 1 1 calc R . .
H40C H 1.0715 0.2567 0.3802 0.043 Uiso 1 1 calc R . .
C41 C 0.9678(3) 0.19537(11) 0.5166(2) 0.0282(7) Uani 1 1 d . . .
H41A H 1.0201 0.1680 0.5352 0.042 Uiso 1 1 calc R . .
H41B H 0.9022 0.1897 0.5374 0.042 Uiso 1 1 calc R . .
H41C H 1.0112 0.2233 0.5530 0.042 Uiso 1 1 calc R . .
C42 C 0.8086(3) 0.25959(10) 0.3378(3) 0.0317(8) Uani 1 1 d . . .
H42A H 0.7770 0.2658 0.2624 0.048 Uiso 1 1 calc R . .
H42B H 0.8534 0.2870 0.3755 0.048 Uiso 1 1 calc R . .
H42C H 0.7441 0.2536 0.3599 0.048 Uiso 1 1 calc R . .
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 N3 2.314(2) . ?
Sm1 N1 2.653(2) . ?
Sm1 N2 2.656(2) . ?
Sm1 O2 2.7029(17) . ?
Sm1 O1 2.7181(16) . ?
Sm1 C1 2.737(3) . ?
Sm1 C19 2.754(2) . ?
Sm1 C22 2.772(3) . ?
Sm1 C4 2.776(2) . ?
Sm1 C2 2.869(3) . ?
Sm1 C20 2.879(3) . ?
Sm1 C21 2.887(2) . ?
N1 C4 1.372(3) . ?
N1 C1 1.384(3) . ?
N2 C19 1.375(3) . ?
N2 C22 1.379(3) . ?
O1 C13 1.396(3) . ?
O1 C10 1.403(3) . ?
O2 C31 1.397(3) . ?
O2 C28 1.411(3) . ?
C1 C2 1.382(4) . ?
C1 C32 1.516(4) . ?
C2 C3 1.409(4) . ?
C3 C4 1.393(3) . ?
C4 C5 1.520(3) . ?
C5 C10 1.495(4) . ?
C5 C6 1.549(3) . ?
C5 C8 1.555(3) . ?
C6 C7 1.522(4) . ?
C8 C9 1.519(4) . ?
C10 C11 1.338(4) . ?
C11 C12 1.433(4) . ?
C12 C13 1.339(3) . ?
C13 C14 1.498(4) . ?
C14 C19 1.507(3) . ?
C14 C15 1.545(4) . ?
C14 C17 1.554(4) . ?
C15 C16 1.524(4) . ?
C17 C18 1.529(4) . ?
C19 C20 1.395(3) . ?
C20 C21 1.404(4) . ?
C21 C22 1.391(3) . ?
C22 C23 1.508(4) . ?
C23 C28 1.500(3) . ?
C23 C24 1.544(3) . ?
C23 C26 1.559(3) . ?
C24 C25 1.525(4) . ?
C26 C27 1.526(4) . ?
C28 C29 1.339(3) . ?
C29 C30 1.427(4) . ?
C30 C31 1.339(4) . ?
C31 C32 1.497(4) . ?
C32 C33 1.540(3) . ?
C32 C35 1.557(3) . ?
C33 C34 1.516(4) . ?
C35 C36 1.521(4) . ?
N3 Si1 1.716(2) . ?
N3 Si2 1.721(2) . ?
Si1 C38 1.877(3) . ?
Si1 C39 1.880(3) . ?
Si1 C37 1.887(3) . ?
Si2 C42 1.881(3) . ?
Si2 C41 1.881(3) . ?
Si2 C40 1.892(3) . ?
