#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:16:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178892 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/21/4112128.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_4112128
loop_
_publ_author_name
'William J. Evans'
'David S. Lee'
'Joseph W. Ziller'
_publ_section_title
;
 Reduction of Dinitrogen to Planar Bimetallic M2(μ-η2:η2-N2) Complexes
 of Y, Ho, Tm, and Lu Using the K/Ln[N(SiMe3)2]3 Reduction System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              454
_journal_page_last               455
_journal_paper_doi               10.1021/ja036923m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C32 H88 Lu2 N6 O2 Si8'
_chemical_formula_weight         1163.74
_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                 112.7590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7686(4)
_cell_length_b                   23.4769(9)
_cell_length_c                   11.4898(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2678.61(17)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27999
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_T_max  0.4828
_exptl_absorpt_correction_T_min  0.3442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0130P)²+4.1455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                6042
_reflns_number_total             6496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036923msi20030626_074320_1.cif
_cod_data_source_block           dl6(213481)
_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               4112128
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
Lu1 Lu 0.449173(9) 0.086714(4) 0.527686(9) 0.01498(4) Uani 1 1 d .
Si1 Si 0.51009(7) 0.17376(3) 0.32060(6) 0.01923(13) Uani 1 1 d .
Si2 Si 0.24324(8) 0.11360(3) 0.22675(7) 0.02630(16) Uani 1 1 d .
Si3 Si 0.26012(7) 0.16961(3) 0.63188(7) 0.02334(14) Uani 1 1 d .
Si4 Si 0.25610(7) 0.04656(3) 0.69478(6) 0.01929(13) Uani 1 1 d .
O1 O 0.63599(17) 0.10778(8) 0.70899(17) 0.0251(4) Uani 1 1 d .
N1 N 0.3958(2) 0.12897(8) 0.34448(18) 0.0175(4) Uani 1 1 d .
N2 N 0.3071(2) 0.10054(8) 0.62188(18) 0.0171(4) Uani 1 1 d .
N3 N 0.4367(2) -0.00562(9) 0.4747(2) 0.0260(5) Uani 1 1 d .
C1 C 0.5568(3) 0.15221(13) 0.1854(3) 0.0340(6) Uani 1 1 d .
H1A H 0.5869 0.1125 0.1962 0.051 Uiso 1 1 calc R
H1B H 0.6297 0.1767 0.1835 0.051 Uiso 1 1 calc R
H1C H 0.4782 0.1562 0.1060 0.051 Uiso 1 1 calc R
C2 C 0.4539(3) 0.25015(11) 0.2934(3) 0.0296(6) Uani 1 1 d .
H2A H 0.4285 0.2631 0.3622 0.044 Uiso 1 1 calc R
H2B H 0.3763 0.2534 0.2130 0.044 Uiso 1 1 calc R
H2C H 0.5277 0.2738 0.2907 0.044 Uiso 1 1 calc R
C3 C 0.6698(3) 0.17311(12) 0.4663(3) 0.0277(6) Uani 1 1 d .
H3A H 0.6499 0.1842 0.5395 0.042 Uiso 1 1 calc R
H3B H 0.7343 0.2000 0.4558 0.042 Uiso 1 1 calc R
H3C H 0.7085 0.1347 0.4795 0.042 Uiso 1 1 calc R
C4 C 0.1491(5) 0.1782(2) 0.1456(6) 0.126(3) Uani 1 1 d .
H4A H 0.2042 0.2001 0.1108 0.188 Uiso 1 1 calc R
H4B H 0.1283 0.2017 0.2061 0.188 Uiso 1 1 calc R
H4C H 0.0651 0.1667 0.0770 0.188 Uiso 1 1 calc R
C5 C 0.2606(5) 0.0664(3) 0.1039(4) 0.094(2) Uani 1 1 d .
H5A H 0.3101 0.0319 0.1437 0.141 Uiso 1 1 calc R
H5B H 0.3098 0.0866 0.0603 0.141 Uiso 1 1 calc R
H5C H 0.1710 0.0559 0.0428 0.141 Uiso 1 1 calc R
C6 C 0.1307(3) 0.07493(14) 0.2891(3) 0.0347(7) Uani 1 1 d .
H6A H 0.1759 0.0403 0.3328 0.052 Uiso 1 1 calc R
H6B H 0.0469 0.0646 0.2189 0.052 Uiso 1 1 calc R
H6C H 0.1103 0.0995 0.3483 0.052 Uiso 1 1 calc R
C7 C 0.0774(3) 0.18498(15) 0.5370(3) 0.0449(8) Uani 1 1 d .
H7A H 0.0215 0.1605 0.5661 0.067 Uiso 1 1 calc R
H7B H 0.0570 0.1775 0.4476 0.067 Uiso 1 1 calc R
H7C H 0.0585 0.2250 0.5479 0.067 Uiso 1 1 calc R
C8 C 0.3553(4) 0.21884(12) 0.5679(4) 0.0516(10) Uani 1 1 d .
H8A H 0.4523 0.2130 0.6137 0.077 Uiso 1 1 calc R
H8B H 0.3325 0.2584 0.5786 0.077 Uiso 1 1 calc R
H8C H 0.3311 0.2109 0.4781 0.077 Uiso 1 1 calc R
C9 C 0.3005(3) 0.19486(12) 0.7985(3) 0.0317(6) Uani 1 1 d .
H9A H 0.2532 0.1709 0.8381 0.048 Uiso 1 1 calc R
H9B H 0.2714 0.2345 0.7969 0.048 Uiso 1 1 calc R
H9C H 0.3978 0.1923 0.8470 0.048 Uiso 1 1 calc R
C10 C 0.3952(3) 0.02671(16) 0.8466(3) 0.0504(9) Uani 1 1 d .
H10A H 0.4234 0.0604 0.9010 0.076 Uiso 1 1 calc R
H10B H 0.4718 0.0121 0.8295 0.076 Uiso 1 1 calc R
H10C H 0.3636 -0.0028 0.8890 0.076 Uiso 1 1 calc R
C11 C 0.1056(3) 0.06414(15) 0.7320(4) 0.0432(8) Uani 1 1 d .
H11A H 0.1238 0.0987 0.7837 0.065 Uiso 1 1 calc R
H11B H 0.0871 0.0325 0.7785 0.065 Uiso 1 1 calc R
H11C H 0.0273 0.0704 0.6533 0.065 Uiso 1 1 calc R
C12 C 0.2080(4) -0.01934(13) 0.5966(3) 0.0477(9) Uani 1 1 d .
H12A H 0.1348 -0.0106 0.5157 0.072 Uiso 1 1 calc R
H12B H 0.1778 -0.0484 0.6410 0.072 Uiso 1 1 calc R
H12C H 0.2860 -0.0336 0.5815 0.072 Uiso 1 1 calc R
C13 C 0.6380(3) 0.13942(13) 0.8188(3) 0.0338(6) Uani 1 1 d .
H13A H 0.5500 0.1368 0.8269 0.041 Uiso 1 1 calc R
H13B H 0.6593 0.1801 0.8126 0.041 Uiso 1 1 calc R
C14 C 0.7474(3) 0.11124(16) 0.9296(3) 0.0411(7) Uani 1 1 d .
H14A H 0.7896 0.1388 0.9989 0.049 Uiso 1 1 calc R
H14B H 0.7107 0.0790 0.9619 0.049 Uiso 1 1 calc R
C15 C 0.8475(4) 0.09066(17) 0.8765(3) 0.0490(9) Uani 1 1 d .
H15A H 0.9252 0.1170 0.9000 0.059 Uiso 1 1 calc R
H15B H 0.8809 0.0522 0.9092 0.059 Uiso 1 1 calc R
C16 C 0.7749(3) 0.08915(18) 0.7390(3) 0.0469(9) Uani 1 1 d .
H16A H 0.8192 0.1147 0.6982 0.056 Uiso 1 1 calc R
H16B H 0.7756 0.0500 0.7073 0.056 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'
Lu Lu -0.4720 5.8584 '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 Lu1 N2 115.40(7) . .
N1 Lu1 N3 102.17(8) . .
N2 Lu1 N3 107.13(8) . .
N1 Lu1 N3 108.04(8) . 3_656
N2 Lu1 N3 127.46(8) . 3_656
N3 Lu1 N3 33.08(10) . 3_656
N1 Lu1 O1 125.40(7) . .
N2 Lu1 O1 93.04(7) . .
N3 Lu1 O1 112.94(7) . .
N3 Lu1 O1 84.51(7) 3_656 .
N1 Si1 C1 113.85(12) . .
N1 Si1 C3 108.53(11) . .
C1 Si1 C3 106.78(14) . .
N1 Si1 C2 113.95(11) . .
C1 Si1 C2 106.94(13) . .
C3 Si1 C2 106.30(13) . .
N1 Si1 Lu1 34.31(7) . .
C1 Si1 Lu1 127.23(10) . .
C3 Si1 Lu1 74.26(9) . .
C2 Si1 Lu1 123.72(9) . .
N1 Si2 C5 112.17(17) . .
N1 Si2 C4 113.20(16) . .
C5 Si2 C4 107.4(3) . .
N1 Si2 C6 111.48(12) . .
C5 Si2 C6 105.81(18) . .
C4 Si2 C6 106.3(2) . .
N1 Si2 Lu1 34.91(6) . .
C5 Si2 Lu1 116.6(2) . .
C4 Si2 Lu1 133.0(2) . .
C6 Si2 Lu1 77.41(10) . .
N2 Si3 C8 109.68(12) . .
N2 Si3 C7 114.35(13) . .
C8 Si3 C7 105.26(18) . .
N2 Si3 C9 114.00(12) . .
C8 Si3 C9 104.94(16) . .
C7 Si3 C9 107.86(13) . .
N2 Si3 Lu1 36.14(7) . .
C8 Si3 Lu1 73.63(10) . .
C7 Si3 Lu1 123.25(10) . .
C9 Si3 Lu1 127.66(9) . .
N2 Si4 C10 110.29(13) . .
N2 Si4 C12 112.48(12) . .
C10 Si4 C12 107.03(18) . .
N2 Si4 C11 114.54(13) . .
C10 Si4 C11 107.08(17) . .
C12 Si4 C11 104.95(16) . .
C13 O1 C16 106.0(2) . .
C13 O1 Lu1 127.09(15) . .
C16 O1 Lu1 126.79(17) . .
Si2 N1 Si1 121.96(12) . .
Si2 N1 Lu1 118.52(10) . .
Si1 N1 Lu1 119.46(10) . .
Si3 N2 Si4 120.36(11) . .
Si3 N2 Lu1 116.66(10) . .
Si4 N2 Lu1 122.74(10) . .
N3 N3 Lu1 74.76(19) 3_656 .
N3 N3 Lu1 72.16(18) 3_656 3_656
Lu1 N3 Lu1 146.92(10) . 3_656
O1 C13 C14 104.6(2) . .
C15 C14 C13 104.2(3) . .
C16 C15 C14 106.1(3) . .
O1 C16 C15 108.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 N1 2.1930(19) .
Lu1 N2 2.2136(19) .
Lu1 N3 2.241(2) .
Lu1 N3 2.272(2) 3_656
Lu1 O1 2.3214(18) .
Si1 N1 1.720(2) .
Si1 C1 1.877(3) .
Si1 C3 1.880(3) .
Si1 C2 1.880(3) .
Si2 N1 1.714(2) .
Si2 C5 1.860(4) .
Si2 C4 1.862(4) .
Si2 C6 1.864(3) .
Si3 N2 1.716(2) .
Si3 C8 1.874(3) .
Si3 C7 1.879(3) .
Si3 C9 1.887(3) .
Si4 N2 1.722(2) .
Si4 C10 1.866(3) .
Si4 C12 1.866(3) .
Si4 C11 1.875(3) .
O1 C13 1.457(3) .
O1 C16 1.466(3) .
N3 N3 1.285(4) 3_656
N3 Lu1 2.272(2) 3_656
C13 C14 1.512(4) .
C14 C15 1.509(5) .
C15 C16 1.467(4) .
