#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:33:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178904 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/33/4113374.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_4113374
loop_
_publ_author_name
'William J. Evans'
'Gaël Zucchi'
'Joseph W. Ziller'
_publ_section_title
;
 Dinitrogen Reduction by Tm(II), Dy(II), and Nd(II) with Simple Amide and
 Aryloxide Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10
_journal_page_last               11
_journal_paper_doi               10.1021/ja0211712
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C32 H90 N6 O2 Si8 Tm2'
_chemical_formula_weight         1153.68
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.6710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7744(4)
_cell_length_b                   23.4795(10)
_cell_length_c                   11.5031(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2685.18(19)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28363
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    3.492
_exptl_absorpt_correction_T_max  0.5005
_exptl_absorpt_correction_T_min  0.3582
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.00031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0201P)²+5.0639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                5996
_reflns_number_total             6515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0211712_1.cif
_cod_data_source_block           gz16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4113374
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
Tm1 Tm 0.448580(11) 0.087756(4) 0.529706(10) 0.01662(4) Uani 1 1 d .
Si1 Si 0.50921(8) 0.17385(3) 0.32229(7) 0.02064(15) Uani 1 1 d .
Si2 Si 0.24176(8) 0.11406(3) 0.22686(8) 0.02763(17) Uani 1 1 d .
Si3 Si 0.25977(9) 0.17034(3) 0.63582(8) 0.02508(16) Uani 1 1 d .
Si4 Si 0.25505(8) 0.04668(3) 0.69612(7) 0.02099(15) Uani 1 1 d .
O1 O 0.6370(2) 0.10733(9) 0.71514(19) 0.0264(4) Uani 1 1 d .
N1 N 0.3937(2) 0.12954(9) 0.3443(2) 0.0190(4) Uani 1 1 d .
N2 N 0.3059(2) 0.10133(9) 0.6249(2) 0.0185(4) Uani 1 1 d .
N3 N 0.4383(2) -0.00488(9) 0.4700(2) 0.0207(4) Uani 1 1 d .
C1 C 0.5577(4) 0.15205(14) 0.1882(3) 0.0351(7) Uani 1 1 d .
H1A H 0.5686 0.1861 0.1438 0.053 Uiso 1 1 calc R
H1B H 0.4871 0.1278 0.1298 0.053 Uiso 1 1 calc R
H1C H 0.6426 0.1309 0.2212 0.053 Uiso 1 1 calc R
C2 C 0.4541(3) 0.25031(12) 0.2953(3) 0.0303(6) Uani 1 1 d .
H2A H 0.4826 0.2669 0.2314 0.045 Uiso 1 1 calc R
H2B H 0.4951 0.2716 0.3743 0.045 Uiso 1 1 calc R
H2C H 0.3559 0.2523 0.2663 0.045 Uiso 1 1 calc R
C3 C 0.6672(3) 0.17198(13) 0.4691(3) 0.0289(6) Uani 1 1 d .
H3A H 0.7359 0.1960 0.4575 0.043 Uiso 1 1 calc R
H3B H 0.7002 0.1327 0.4860 0.043 Uiso 1 1 calc R
H3C H 0.6479 0.1862 0.5405 0.043 Uiso 1 1 calc R
C4 C 0.1486(5) 0.1787(2) 0.1457(7) 0.122(3) Uani 1 1 d .
H4A H 0.1375 0.2046 0.2079 0.183 Uiso 1 1 calc R
H4B H 0.0599 0.1676 0.0841 0.183 Uiso 1 1 calc R
H4C H 0.1992 0.1979 0.1024 0.183 Uiso 1 1 calc R
C5 C 0.2600(5) 0.0664(3) 0.1052(4) 0.089(2) Uani 1 1 d .
H5A H 0.3096 0.0321 0.1457 0.133 Uiso 1 1 calc R
H5B H 0.3093 0.0863 0.0615 0.133 Uiso 1 1 calc R
H5C H 0.1707 0.0556 0.0443 0.133 Uiso 1 1 calc R
C6 C 0.1291(3) 0.07572(15) 0.2894(3) 0.0369(7) Uani 1 1 d .
H6A H 0.1151 0.0992 0.3538 0.055 Uiso 1 1 calc R
H6B H 0.1706 0.0395 0.3268 0.055 Uiso 1 1 calc R
H6C H 0.0423 0.0684 0.2205 0.055 Uiso 1 1 calc R
C7 C 0.0784(4) 0.18630(16) 0.5417(3) 0.0474(10) Uani 1 1 d .
H7A H 0.0435 0.2111 0.5906 0.071 Uiso 1 1 calc R
H7B H 0.0270 0.1507 0.5220 0.071 Uiso 1 1 calc R
H7C H 0.0696 0.2055 0.4632 0.071 Uiso 1 1 calc R
C8 C 0.3567(5) 0.21891(14) 0.5722(4) 0.0552(12) Uani 1 1 d .
H8A H 0.3347 0.2586 0.5825 0.083 Uiso 1 1 calc R
H8B H 0.3328 0.2109 0.4825 0.083 Uiso 1 1 calc R
H8C H 0.4533 0.2127 0.6182 0.083 Uiso 1 1 calc R
C9 C 0.3000(3) 0.19525(14) 0.8017(3) 0.0324(7) Uani 1 1 d .
H9A H 0.2260 0.2188 0.8042 0.049 Uiso 1 1 calc R
H9B H 0.3831 0.2177 0.8304 0.049 Uiso 1 1 calc R
H9C H 0.3119 0.1622 0.8570 0.049 Uiso 1 1 calc R
C10 C 0.3936(4) 0.02678(18) 0.8480(4) 0.0504(10) Uani 1 1 d .
H10A H 0.4748 0.0177 0.8326 0.076 Uiso 1 1 calc R
H10B H 0.3666 -0.0065 0.8839 0.076 Uiso 1 1 calc R
H10C H 0.4123 0.0587 0.9071 0.076 Uiso 1 1 calc R
C11 C 0.1033(4) 0.06351(16) 0.7320(4) 0.0410(8) Uani 1 1 d .
H11A H 0.1208 0.0976 0.7850 0.062 Uiso 1 1 calc R
H11B H 0.0837 0.0313 0.7765 0.062 Uiso 1 1 calc R
H11C H 0.0259 0.0704 0.6531 0.062 Uiso 1 1 calc R
C12 C 0.2092(4) -0.01852(14) 0.5966(3) 0.0414(8) Uani 1 1 d .
H12A H 0.2845 -0.0296 0.5736 0.062 Uiso 1 1 calc R
H12B H 0.1298 -0.0108 0.5200 0.062 Uiso 1 1 calc R
H12C H 0.1893 -0.0495 0.6437 0.062 Uiso 1 1 calc R
C13 C 0.6393(3) 0.13848(14) 0.8251(3) 0.0349(7) Uani 1 1 d .
H13A H 0.5514 0.1358 0.8333 0.042 Uiso 1 1 calc R
H13B H 0.6608 0.1791 0.8196 0.042 Uiso 1 1 calc R
C14 C 0.7481(4) 0.11006(17) 0.9350(3) 0.0425(8) Uani 1 1 d .
H14A H 0.7119 0.0770 0.9654 0.051 Uiso 1 1 calc R
H14B H 0.7889 0.1372 1.0054 0.051 Uiso 1 1 calc R
C15 C 0.8495(4) 0.09115(19) 0.8817(4) 0.0504(10) Uani 1 1 d .
H15A H 0.9243 0.1189 0.9032 0.060 Uiso 1 1 calc R
H15B H 0.8870 0.0534 0.9157 0.060 Uiso 1 1 calc R
C16 C 0.7754(4) 0.0882(2) 0.7441(3) 0.0489(10) Uani 1 1 d .
H16A H 0.8190 0.1129 0.7012 0.059 Uiso 1 1 calc R
H16B H 0.7752 0.0486 0.7144 0.059 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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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
N1 Tm1 N2 115.59(8) . .
N1 Tm1 N3 99.77(8) . .
N2 Tm1 N3 108.85(8) . .
N1 Tm1 N3 108.78(8) . 3_656
N2 Tm1 N3 125.97(8) . 3_656
N3 Tm1 N3 32.06(11) . 3_656
N1 Tm1 O1 127.16(8) . .
N2 Tm1 O1 92.53(7) . .
N3 Tm1 O1 112.68(8) . .
N3 Tm1 O1 83.82(7) 3_656 .
N1 Si1 C2 113.77(13) . .
N1 Si1 C1 113.77(13) . .
C2 Si1 C1 107.15(15) . .
N1 Si1 C3 108.09(12) . .
C2 Si1 C3 106.83(14) . .
C1 Si1 C3 106.80(15) . .
N1 Si1 Tm1 35.24(7) . .
C2 Si1 Tm1 123.62(10) . .
C1 Si1 Tm1 127.38(11) . .
C3 Si1 Tm1 72.90(10) . .
N1 Si2 C4 112.94(17) . .
N1 Si2 C5 112.03(19) . .
C4 Si2 C5 107.8(3) . .
N1 Si2 C6 111.38(13) . .
C4 Si2 C6 106.4(3) . .
C5 Si2 C6 105.8(2) . .
N2 Si3 C7 114.51(15) . .
N2 Si3 C8 108.99(14) . .
C7 Si3 C8 105.5(2) . .
N2 Si3 C9 114.12(13) . .
C7 Si3 C9 107.81(15) . .
C8 Si3 C9 105.18(17) . .
N2 Si3 Tm1 36.38(8) . .
C7 Si3 Tm1 123.28(11) . .
C8 Si3 Tm1 72.71(11) . .
C9 Si3 Tm1 127.80(10) . .
N2 Si4 C12 112.22(13) . .
N2 Si4 C10 110.19(15) . .
C12 Si4 C10 107.25(19) . .
N2 Si4 C11 114.32(14) . .
C12 Si4 C11 105.16(17) . .
C10 Si4 C11 107.31(19) . .
C13 O1 C16 106.3(2) . .
C13 O1 Tm1 127.35(17) . .
C16 O1 Tm1 126.27(19) . .
Si2 N1 Si1 122.68(13) . .
Si2 N1 Tm1 119.08(11) . .
Si1 N1 Tm1 118.17(11) . .
Si3 N2 Si4 121.04(13) . .
Si3 N2 Tm1 116.48(11) . .
Si4 N2 Tm1 122.26(11) . .
N3 N3 Tm1 75.1(2) 3_656 .
N3 N3 Tm1 72.87(19) 3_656 3_656
Tm1 N3 Tm1 147.94(11) . 3_656
O1 C13 C14 104.7(2) . .
C13 C14 C15 103.9(3) . .
C16 C15 C14 105.8(3) . .
O1 C16 C15 108.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 N1 2.211(2) .
Tm1 N2 2.228(2) .
Tm1 N3 2.271(2) .
Tm1 N3 2.296(2) 3_656
Tm1 O1 2.355(2) .
Si1 N1 1.715(2) .
Si1 C2 1.879(3) .
Si1 C1 1.880(3) .
Si1 C3 1.881(3) .
Si2 N1 1.712(2) .
Si2 C4 1.860(4) .
Si2 C5 1.861(5) .
Si2 C6 1.864(3) .
Si3 N2 1.714(2) .
Si3 C7 1.871(4) .
Si3 C8 1.876(4) .
Si3 C9 1.880(3) .
Si4 N2 1.721(2) .
Si4 C12 1.861(3) .
Si4 C10 1.868(4) .
Si4 C11 1.876(3) .
O1 C13 1.453(4) .
O1 C16 1.468(4) .
N3 N3 1.261(4) 3_656
N3 Tm1 2.296(2) 3_656
C13 C14 1.508(5) .
C14 C15 1.511(5) .
C15 C16 1.474(5) .
