#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324448.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_4324448
loop_
_publ_author_name
'Ming Fang'
'Jefferson E. Bates'
'Sara E. Lorenz'
'David S. Lee'
'Daniel B. Rego'
'Joseph W. Ziller'
'Filipp Furche'
'William J. Evans'
_publ_section_title
;
 (N2)3- Radical Chemistry via Trivalent Lanthanide Salt/Alkali Metal
 Reduction of Dinitrogen: New Syntheses and Examples of (N2)2- and (N2)3-
 Complexes and Density Functional Theory Comparisons of Closed Shell Sc3+,
 Y3+, and Lu3+ versus 4f9 Dy3+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1459
_journal_page_last               1469
_journal_paper_doi               10.1021/ic102016k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C56 H136 N6 Na O8 Si8 Y2'
_chemical_formula_weight         1447.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.962(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.860(3)
_cell_length_b                   19.633(5)
_cell_length_c                   16.079(4)
_cell_measurement_temperature    163(2)
_cell_volume                     4057.3(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      163(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29204
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.5684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange/yello
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1558
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0519
_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)+(0.0905P)²+2.7268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                4243
_reflns_number_total             5798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102016k_si_002_2.cif
_cod_data_source_block           dl23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_original_cell_volume        4057.5(16)
_cod_database_code               4324448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Y1 Y 0.04994(4) 0.09645(2) 0.46290(3) 0.02137(18) Uani 1 1 d .
Si1 Si -0.20523(11) 0.15360(7) 0.46376(8) 0.0251(3) Uani 1 1 d .
Si2 Si -0.05071(11) 0.25874(7) 0.41504(9) 0.0276(4) Uani 1 1 d .
Si3 Si 0.32821(11) 0.12170(8) 0.46925(9) 0.0296(4) Uani 1 1 d .
Si4 Si 0.20443(11) 0.15554(8) 0.61746(8) 0.0273(4) Uani 1 1 d .
O1 O 0.0663(3) 0.08057(19) 0.3143(2) 0.0389(10) Uani 1 1 d .
N1 N -0.0807(3) 0.1775(2) 0.4399(2) 0.0216(9) Uani 1 1 d .
N2 N 0.2132(3) 0.1273(2) 0.5176(2) 0.0242(10) Uani 1 1 d .
N3 N -0.0140(3) 0.0138(2) 0.5379(2) 0.0271(10) Uani 1 1 d .
C1 C -0.2215(4) 0.1440(3) 0.5788(3) 0.0435(15) Uani 1 1 d .
H1A H -0.1692 0.1122 0.6015 0.065 Uiso 1 1 calc R
H1B H -0.2912 0.1264 0.5889 0.065 Uiso 1 1 calc R
H1C H -0.2127 0.1885 0.6059 0.065 Uiso 1 1 calc R
C2 C -0.2405(4) 0.0711(3) 0.4125(4) 0.0410(15) Uani 1 1 d .
H2A H -0.1886 0.0365 0.4282 0.062 Uiso 1 1 calc R
H2B H -0.2425 0.0770 0.3519 0.062 Uiso 1 1 calc R
H2C H -0.3091 0.0564 0.4304 0.062 Uiso 1 1 calc R
C3 C -0.3102(4) 0.2156(3) 0.4283(3) 0.0358(13) Uani 1 1 d .
H3A H -0.3061 0.2232 0.3682 0.054 Uiso 1 1 calc R
H3B H -0.3003 0.2589 0.4577 0.054 Uiso 1 1 calc R
H3C H -0.3786 0.1967 0.4405 0.054 Uiso 1 1 calc R
C4 C 0.0923(4) 0.2654(3) 0.3951(4) 0.0375(14) Uani 1 1 d .
H4A H 0.1326 0.2485 0.4437 0.056 Uiso 1 1 calc R
H4B H 0.1104 0.3132 0.3852 0.056 Uiso 1 1 calc R
H4C H 0.1085 0.2382 0.3462 0.056 Uiso 1 1 calc R
C5 C -0.1182(4) 0.2930(3) 0.3176(4) 0.0422(15) Uani 1 1 d .
H5A H -0.1938 0.2909 0.3236 0.063 Uiso 1 1 calc R
H5B H -0.0988 0.2656 0.2697 0.063 Uiso 1 1 calc R
H5C H -0.0972 0.3404 0.3091 0.063 Uiso 1 1 calc R
C6 C -0.0789(4) 0.3224(3) 0.4987(4) 0.0410(14) Uani 1 1 d .
H6A H -0.1531 0.3208 0.5107 0.062 Uiso 1 1 calc R
H6B H -0.0608 0.3682 0.4798 0.062 Uiso 1 1 calc R
H6C H -0.0376 0.3113 0.5493 0.062 Uiso 1 1 calc R
C7 C 0.3212(5) 0.0594(3) 0.3811(4) 0.0544(18) Uani 1 1 d .
H7A H 0.2638 0.0719 0.3424 0.082 Uiso 1 1 calc R
H7B H 0.3094 0.0136 0.4029 0.082 Uiso 1 1 calc R
H7C H 0.3868 0.0603 0.3518 0.082 Uiso 1 1 calc R
C8 C 0.4406(4) 0.0936(3) 0.5388(4) 0.0459(16) Uani 1 1 d .
H8A H 0.4238 0.0499 0.5646 0.069 Uiso 1 1 calc R
H8B H 0.4538 0.1278 0.5822 0.069 Uiso 1 1 calc R
H8C H 0.5027 0.0883 0.5058 0.069 Uiso 1 1 calc R
C9 C 0.3694(4) 0.2052(3) 0.4229(4) 0.0409(15) Uani 1 1 d .
H9A H 0.3136 0.2225 0.3856 0.061 Uiso 1 1 calc R
H9B H 0.4325 0.1983 0.3914 0.061 Uiso 1 1 calc R
H9C H 0.3836 0.2382 0.4675 0.061 Uiso 1 1 calc R
C10 C 0.2751(5) 0.2377(3) 0.6391(4) 0.0467(16) Uani 1 1 d .
H10A H 0.3133 0.2345 0.6928 0.070 Uiso 1 1 calc R
H10B H 0.2248 0.2751 0.6409 0.070 Uiso 1 1 calc R
H10C H 0.3241 0.2463 0.5950 0.070 Uiso 1 1 calc R
C11 C 0.0646(4) 0.1707(3) 0.6404(3) 0.0411(15) Uani 1 1 d .
H11A H 0.0601 0.1937 0.6943 0.062 Uiso 1 1 calc R
H11B H 0.0279 0.1270 0.6422 0.062 Uiso 1 1 calc R
H11C H 0.0326 0.1994 0.5967 0.062 Uiso 1 1 calc R
C12 C 0.2545(5) 0.0946(3) 0.6997(3) 0.0420(15) Uani 1 1 d .
H12A H 0.2985 0.1192 0.7406 0.063 Uiso 1 1 calc R
H12B H 0.2955 0.0588 0.6738 0.063 Uiso 1 1 calc R
H12C H 0.1957 0.0740 0.7277 0.063 Uiso 1 1 calc R
C13 C 0.0838(5) 0.0129(3) 0.2790(3) 0.0477(16) Uani 1 1 d .
H13A H 0.0848 -0.0221 0.3233 0.057 Uiso 1 1 calc R
H13B H 0.1511 0.0116 0.2509 0.057 Uiso 1 1 calc R
C14 C -0.0025(6) 0.0006(4) 0.2190(5) 0.067(2) Uani 1 1 d .
H14A H -0.0537 -0.0310 0.2427 0.081 Uiso 1 1 calc R
H14B H 0.0235 -0.0197 0.1673 0.081 Uiso 1 1 calc R
C15 C -0.0521(5) 0.0692(3) 0.2011(4) 0.0527(17) Uani 1 1 d .
H15A H -0.0521 0.0795 0.1408 0.063 Uiso 1 1 calc R
H15B H -0.1248 0.0701 0.2196 0.063 Uiso 1 1 calc R
C16 C 0.0134(5) 0.1190(3) 0.2492(3) 0.0444(16) Uani 1 1 d .
H16A H 0.0642 0.1408 0.2128 0.053 Uiso 1 1 calc R
H16B H -0.0305 0.1549 0.2732 0.053 Uiso 1 1 calc R
Na1 Na 0.5000 0.5000 0.5000 0.0224(6) Uani 1 2 d S
O2 O 0.3301(3) 0.45931(19) 0.4816(2) 0.0397(10) Uani 1 1 d .
O3 O 0.4607(3) 0.58677(19) 0.4002(2) 0.0411(10) Uani 1 1 d .
O4 O 0.4434(3) 0.57403(19) 0.6045(2) 0.0376(10) Uani 1 1 d .
C17 C 0.2922(5) 0.3970(3) 0.5137(5) 0.0558(18) Uani 1 1 d .
H17A H 0.3395 0.3794 0.5586 0.067 Uiso 1 1 calc R
H17B H 0.2854 0.3623 0.4692 0.067 Uiso 1 1 calc R
C18 C 0.1874(5) 0.4142(3) 0.5470(4) 0.0534(18) Uani 1 1 d .
H18A H 0.1938 0.4306 0.6052 0.064 Uiso 1 1 calc R
H18B H 0.1403 0.3743 0.5444 0.064 Uiso 1 1 calc R
C19 C 0.1493(5) 0.4700(4) 0.4890(6) 0.081(3) Uani 1 1 d .
H19A H 0.0956 0.4524 0.4491 0.097 Uiso 1 1 calc R
H19B H 0.1193 0.5080 0.5208 0.097 Uiso 1 1 calc R
C20 C 0.2431(5) 0.4934(4) 0.4443(4) 0.0513(17) Uani 1 1 d .
H20A H 0.2360 0.4818 0.3845 0.062 Uiso 1 1 calc R
H20B H 0.2514 0.5433 0.4498 0.062 Uiso 1 1 calc R
C21 C 0.4684(7) 0.5789(4) 0.3112(4) 0.077(3) Uani 1 1 d .
H21A H 0.4164 0.5454 0.2898 0.092 Uiso 1 1 calc R
H21B H 0.5386 0.5625 0.2976 0.092 Uiso 1 1 calc R
C22 C 0.4486(7) 0.6456(4) 0.2737(4) 0.076(2) Uani 1 1 d .
H22A H 0.4141 0.6413 0.2180 0.091 Uiso 1 1 calc R
H22B H 0.5139 0.6718 0.2690 0.091 Uiso 1 1 calc R
C23 C 0.3783(7) 0.6780(4) 0.3341(5) 0.085(3) Uani 1 1 d .
H23A H 0.3828 0.7282 0.3316 0.103 Uiso 1 1 calc R
H23B H 0.3052 0.6639 0.3233 0.103 Uiso 1 1 calc R
C24 C 0.4183(5) 0.6521(3) 0.4151(4) 0.0487(17) Uani 1 1 d .
H24A H 0.4725 0.6829 0.4388 0.058 Uiso 1 1 calc R
H24B H 0.3613 0.6488 0.4548 0.058 Uiso 1 1 calc R
C25 C 0.5112(5) 0.6224(3) 0.6434(4) 0.0510(17) Uani 1 1 d .
H25A H 0.5286 0.6588 0.6036 0.061 Uiso 1 1 calc R
H25B H 0.5765 0.6002 0.6633 0.061 Uiso 1 1 calc R
C26 C 0.4544(6) 0.6520(3) 0.7159(4) 0.0562(19) Uani 1 1 d .
H26A H 0.5026 0.6607 0.7641 0.067 Uiso 1 1 calc R
H26B H 0.4184 0.6949 0.7002 0.067 Uiso 1 1 calc R
C27 C 0.3788(7) 0.5975(4) 0.7347(4) 0.068(2) Uani 1 1 d .
H27A H 0.3176 0.6160 0.7627 0.082 Uiso 1 1 calc R
H27B H 0.4114 0.5616 0.7702 0.082 Uiso 1 1 calc R
C28 C 0.3496(5) 0.5708(3) 0.6499(4) 0.0489(16) Uani 1 1 d .
H28A H 0.3242 0.5233 0.6532 0.059 Uiso 1 1 calc R
H28B H 0.2946 0.5993 0.6230 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'
Na Na 0.0362 0.0249 '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'
Y Y -2.7962 3.5667 '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
N3 Y1 N3 36.82(18) . 3_556
N3 Y1 N2 109.51(15) . .
N3 Y1 N2 116.23(15) 3_556 .
N3 Y1 N1 108.03(14) . .
N3 Y1 N1 121.11(14) 3_556 .
N2 Y1 N1 121.17(14) . .
N3 Y1 O1 119.50(14) . .
N3 Y1 O1 83.89(13) 3_556 .
N2 Y1 O1 107.34(13) . .
N1 Y1 O1 91.00(12) . .
N1 Si1 C2 110.6(2) . .
N1 Si1 C1 112.5(2) . .
C2 Si1 C1 108.3(3) . .
N1 Si1 C3 114.6(2) . .
C2 Si1 C3 105.3(3) . .
C1 Si1 C3 105.0(3) . .
N1 Si2 C6 114.0(2) . .
N1 Si2 C4 109.7(2) . .
C6 Si2 C4 106.8(3) . .
N1 Si2 C5 115.4(2) . .
C6 Si2 C5 105.2(3) . .
C4 Si2 C5 105.0(2) . .
N2 Si3 C7 111.6(2) . .
N2 Si3 C8 114.2(2) . .
C7 Si3 C8 105.9(3) . .
N2 Si3 C9 112.7(2) . .
C7 Si3 C9 106.0(3) . .
C8 Si3 C9 105.7(3) . .
N2 Si4 C11 109.4(2) . .
N2 Si4 C10 114.0(2) . .
C11 Si4 C10 106.8(3) . .
N2 Si4 C12 115.0(2) . .
C11 Si4 C12 105.7(3) . .
C10 Si4 C12 105.3(3) . .
N2 Si4 Y1 40.78(13) . .
C11 Si4 Y1 69.55(17) . .
C10 Si4 Y1 135.1(2) . .
C12 Si4 Y1 118.92(19) . .
C16 O1 C13 105.6(4) . .
C16 O1 Y1 126.4(3) . .
C13 O1 Y1 121.2(3) . .
Si2 N1 Si1 122.0(2) . .
Si2 N1 Y1 120.8(2) . .
Si1 N1 Y1 116.6(2) . .
Si3 N2 Si4 122.6(2) . .
Si3 N2 Y1 126.8(2) . .
Si4 N2 Y1 110.62(19) . .
N3 N3 Y1 72.1(3) 3_556 .
N3 N3 Y1 71.0(3) 3_556 3_556
Y1 N3 Y1 143.18(18) . 3_556
O1 C13 C14 106.3(5) . .
C13 C14 C15 106.5(6) . .
C16 C15 C14 104.9(5) . .
O1 C16 C15 106.1(5) . .
O2 Na1 O2 180.0 . 3_666
O2 Na1 O4 90.53(13) . 3_666
O2 Na1 O4 89.47(13) 3_666 3_666
O2 Na1 O4 89.47(13) . .
O2 Na1 O4 90.53(13) 3_666 .
O4 Na1 O4 179.999(1) 3_666 .
O2 Na1 O3 89.06(14) . .
O2 Na1 O3 90.94(14) 3_666 .
O4 Na1 O3 91.40(12) 3_666 .
O4 Na1 O3 88.60(12) . .
O2 Na1 O3 90.94(14) . 3_666
O2 Na1 O3 89.06(14) 3_666 3_666
O4 Na1 O3 88.60(12) 3_666 3_666
O4 Na1 O3 91.40(12) . 3_666
O3 Na1 O3 179.999(1) . 3_666
C20 O2 C17 106.5(5) . .
C20 O2 Na1 127.8(3) . .
C17 O2 Na1 125.5(4) . .
C24 O3 C21 107.7(4) . .
C24 O3 Na1 127.4(3) . .
C21 O3 Na1 124.7(3) . .
C25 O4 C28 108.6(4) . .
C25 O4 Na1 121.8(3) . .
C28 O4 Na1 128.5(3) . .
O2 C17 C18 105.0(5) . .
C17 C18 C19 102.6(5) . .
C20 C19 C18 105.7(5) . .
O2 C20 C19 106.8(5) . .
O3 C21 C22 107.1(6) . .
C21 C22 C23 102.4(6) . .
C24 C23 C22 103.2(6) . .
O3 C24 C23 106.7(5) . .
O4 C25 C26 106.9(5) . .
C27 C26 C25 102.5(5) . .
C26 C27 C28 102.3(5) . .
O4 C28 C27 105.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 N3 2.199(4) .
Y1 N3 2.213(4) 3_556
Y1 N2 2.328(4) .
Y1 N1 2.334(4) .
Y1 O1 2.426(3) .
Si1 N1 1.725(4) .
Si1 C2 1.867(6) .
Si1 C1 1.878(6) .
Si1 C3 1.891(5) .
Si2 N1 1.693(4) .
Si2 C6 1.880(6) .
Si2 C4 1.882(5) .
Si2 C5 1.889(6) .
Si3 N2 1.698(4) .
Si3 C7 1.872(6) .
Si3 C8 1.880(6) .
Si3 C9 1.884(6) .
Si4 N2 1.706(4) .
Si4 C11 1.872(6) .
Si4 C10 1.878(6) .
Si4 C12 1.881(5) .
O1 C16 1.442(6) .
O1 C13 1.465(7) .
N3 N3 1.393(7) 3_556
N3 Y1 2.213(4) 3_556
C13 C14 1.465(9) .
C14 C15 1.515(9) .
C15 C16 1.490(9) .
Na1 O2 2.335(4) .
Na1 O2 2.335(4) 3_666
Na1 O4 2.355(3) 3_666
Na1 O4 2.355(3) .
Na1 O3 2.383(3) .
Na1 O3 2.383(3) 3_666
O2 C20 1.419(7) .
O2 C17 1.420(7) .
O3 C24 1.417(7) .
O3 C21 1.447(7) .
O4 C25 1.420(7) .
O4 C28 1.433(7) .
C17 C18 1.505(8) .
C18 C19 1.509(9) .
C19 C20 1.497(9) .
C21 C22 1.460(9) .
C22 C23 1.491(10) .
C23 C24 1.474(9) .
C25 C26 1.513(8) .
C26 C27 1.484(10) .
C27 C28 1.497(9) .
