#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:47:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179347 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/44/4324449.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_4324449
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 Er2 N6 Na O8 Si8'
_chemical_formula_weight         1603.94
_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                 92.120(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.834(2)
_cell_length_b                   19.587(3)
_cell_length_c                   16.106(3)
_cell_measurement_temperature    163(2)
_cell_volume                     4045.9(12)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41476
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.229
_exptl_absorpt_correction_T_max  0.5544
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0225
_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)+(0.0292P)²+4.0659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                8635
_reflns_number_total             9756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102016k_si_002_3.cif
_cod_data_source_block           dbr7
_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        4046.1(11)
_cod_database_code               4324449
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
Er1 Er 0.050001(7) 0.095599(5) 0.462499(6) 0.01580(4) Uani 1 1 d .
Si1 Si -0.20403(4) 0.15303(3) 0.46451(4) 0.01878(12) Uani 1 1 d .
Si2 Si -0.04967(5) 0.25816(3) 0.41578(4) 0.02112(12) Uani 1 1 d .
Si3 Si 0.32715(5) 0.12071(3) 0.46986(4) 0.02228(13) Uani 1 1 d .
Si4 Si 0.20390(5) 0.15456(3) 0.61760(4) 0.02052(12) Uani 1 1 d .
O1 O 0.06592(15) 0.07902(10) 0.31520(11) 0.0318(4) Uani 1 1 d .
N1 N -0.07997(13) 0.17646(9) 0.44067(11) 0.0178(3) Uani 1 1 d .
N2 N 0.21125(14) 0.12618(10) 0.51797(11) 0.0194(4) Uani 1 1 d .
N3 N -0.01431(14) 0.01436(10) 0.53783(11) 0.0199(4) Uani 1 1 d .
C1 C -0.2208(2) 0.14391(16) 0.57887(16) 0.0344(6) Uani 1 1 d .
H1A H -0.1685 0.1120 0.6020 0.052 Uiso 1 1 calc R
H1B H -0.2908 0.1264 0.5888 0.052 Uiso 1 1 calc R
H1C H -0.2117 0.1885 0.6057 0.052 Uiso 1 1 calc R
C2 C -0.2413(2) 0.07034(13) 0.41331(19) 0.0336(6) Uani 1 1 d .
H2A H -0.1898 0.0353 0.4290 0.050 Uiso 1 1 calc R
H2B H -0.2435 0.0762 0.3528 0.050 Uiso 1 1 calc R
H2C H -0.3102 0.0562 0.4313 0.050 Uiso 1 1 calc R
C3 C -0.30892(18) 0.21518(13) 0.42924(17) 0.0290(5) Uani 1 1 d .
H3A H -0.3053 0.2226 0.3693 0.044 Uiso 1 1 calc R
H3B H -0.2985 0.2587 0.4585 0.044 Uiso 1 1 calc R
H3C H -0.3774 0.1965 0.4417 0.044 Uiso 1 1 calc R
C4 C 0.09392(18) 0.26543(13) 0.39695(18) 0.0304(5) Uani 1 1 d .
H4A H 0.1126 0.2332 0.3534 0.046 Uiso 1 1 calc R
H4B H 0.1339 0.2548 0.4483 0.046 Uiso 1 1 calc R
H4C H 0.1099 0.3120 0.3794 0.046 Uiso 1 1 calc R
C5 C -0.1177(2) 0.29262(15) 0.31887(18) 0.0347(6) Uani 1 1 d .
H5A H -0.1059 0.2618 0.2723 0.052 Uiso 1 1 calc R
H5B H -0.0900 0.3379 0.3064 0.052 Uiso 1 1 calc R
H5C H -0.1927 0.2961 0.3276 0.052 Uiso 1 1 calc R
C6 C -0.0783(2) 0.32167(13) 0.49994(19) 0.0342(6) Uani 1 1 d .
H6A H -0.0448 0.3067 0.5525 0.051 Uiso 1 1 calc R
H6B H -0.1539 0.3247 0.5062 0.051 Uiso 1 1 calc R
H6C H -0.0512 0.3666 0.4849 0.051 Uiso 1 1 calc R
C7 C 0.3203(2) 0.05851(17) 0.38170(19) 0.0425(7) Uani 1 1 d .
H7A H 0.2624 0.0708 0.3432 0.064 Uiso 1 1 calc R
H7B H 0.3092 0.0124 0.4033 0.064 Uiso 1 1 calc R
H7C H 0.3858 0.0597 0.3523 0.064 Uiso 1 1 calc R
C8 C 0.44029(19) 0.09282(15) 0.53939(19) 0.0364(6) Uani 1 1 d .
H8A H 0.4236 0.0492 0.5656 0.055 Uiso 1 1 calc R
H8B H 0.4538 0.1274 0.5825 0.055 Uiso 1 1 calc R
H8C H 0.5024 0.0874 0.5064 0.055 Uiso 1 1 calc R
C9 C 0.3688(2) 0.20417(14) 0.42349(18) 0.0337(6) Uani 1 1 d .
H9A H 0.3129 0.2216 0.3862 0.051 Uiso 1 1 calc R
H9B H 0.4319 0.1971 0.3921 0.051 Uiso 1 1 calc R
H9C H 0.3833 0.2373 0.4680 0.051 Uiso 1 1 calc R
C10 C 0.2753(2) 0.23708(14) 0.63927(18) 0.0363(6) Uani 1 1 d .
H10A H 0.3130 0.2341 0.6932 0.055 Uiso 1 1 calc R
H10B H 0.2250 0.2747 0.6404 0.055 Uiso 1 1 calc R
H10C H 0.3249 0.2454 0.5956 0.055 Uiso 1 1 calc R
C11 C 0.0639(2) 0.17096(15) 0.64106(16) 0.0332(6) Uani 1 1 d .
H11A H 0.0603 0.1940 0.6949 0.050 Uiso 1 1 calc R
H11B H 0.0263 0.1275 0.6430 0.050 Uiso 1 1 calc R
H11C H 0.0320 0.2000 0.5976 0.050 Uiso 1 1 calc R
C12 C 0.2532(2) 0.09338(14) 0.69974(17) 0.0337(6) Uani 1 1 d .
H12A H 0.2971 0.1179 0.7409 0.051 Uiso 1 1 calc R
H12B H 0.2943 0.0575 0.6740 0.051 Uiso 1 1 calc R
H12C H 0.1940 0.0728 0.7272 0.051 Uiso 1 1 calc R
C13 C 0.0833(3) 0.01197(15) 0.28032(17) 0.0402(7) Uani 1 1 d .
H13A H 0.0812 -0.0234 0.3241 0.048 Uiso 1 1 calc R
H13B H 0.1521 0.0100 0.2545 0.048 Uiso 1 1 calc R
C14 C -0.0025(3) 0.00070(17) 0.2163(3) 0.0548(9) Uani 1 1 d .
H14A H -0.0537 -0.0326 0.2366 0.066 Uiso 1 1 calc R
H14B H 0.0260 -0.0170 0.1642 0.066 Uiso 1 1 calc R
C15 C -0.0530(3) 0.06883(17) 0.2016(2) 0.0453(7) Uani 1 1 d .
H15A H -0.1250 0.0689 0.2217 0.054 Uiso 1 1 calc R
H15B H -0.0552 0.0804 0.1418 0.054 Uiso 1 1 calc R
C16 C 0.0147(3) 0.11889(15) 0.25052(16) 0.0363(6) Uani 1 1 d .
H16A H 0.0665 0.1402 0.2145 0.044 Uiso 1 1 calc R
H16B H -0.0283 0.1553 0.2746 0.044 Uiso 1 1 calc R
Na1 Na 0.5000 0.5000 0.5000 0.0177(2) Uani 1 2 d S
O2 O 0.33021(13) 0.45891(9) 0.48184(12) 0.0302(4) Uani 1 1 d .
O3 O 0.46061(17) 0.58646(9) 0.39951(11) 0.0341(4) Uani 1 1 d .
O4 O 0.44295(14) 0.57454(9) 0.60375(11) 0.0287(4) Uani 1 1 d .
C17 C 0.2921(2) 0.39644(14) 0.5153(2) 0.0428(8) Uani 1 1 d .
H17A H 0.3396 0.3795 0.5606 0.051 Uiso 1 1 calc R
H17B H 0.2855 0.3610 0.4717 0.051 Uiso 1 1 calc R
C18 C 0.1868(2) 0.41405(15) 0.5481(2) 0.0396(7) Uani 1 1 d .
H18A H 0.1394 0.3742 0.5454 0.048 Uiso 1 1 calc R
H18B H 0.1932 0.4305 0.6062 0.048 Uiso 1 1 calc R
C19 C 0.1491(2) 0.46976(19) 0.4905(3) 0.0617(11) Uani 1 1 d .
H19A H 0.1201 0.5081 0.5225 0.074 Uiso 1 1 calc R
H19B H 0.0940 0.4523 0.4514 0.074 Uiso 1 1 calc R
C20 C 0.2420(2) 0.49298(17) 0.4442(2) 0.0397(7) Uani 1 1 d .
H20A H 0.2339 0.4806 0.3847 0.048 Uiso 1 1 calc R
H20B H 0.2504 0.5431 0.4486 0.048 Uiso 1 1 calc R
C21 C 0.4675(4) 0.57759(19) 0.31168(19) 0.0605(11) Uani 1 1 d .
H21A H 0.4149 0.5441 0.2910 0.073 Uiso 1 1 calc R
H21B H 0.5376 0.5606 0.2983 0.073 Uiso 1 1 calc R
C22 C 0.4482(3) 0.6451(2) 0.2724(2) 0.0600(10) Uani 1 1 d .
H22A H 0.4148 0.6404 0.2163 0.072 Uiso 1 1 calc R
H22B H 0.5135 0.6716 0.2686 0.072 Uiso 1 1 calc R
C23 C 0.3757(3) 0.6771(2) 0.3324(3) 0.0682(12) Uani 1 1 d .
H23A H 0.3782 0.7276 0.3291 0.082 Uiso 1 1 calc R
H23B H 0.3030 0.6617 0.3214 0.082 Uiso 1 1 calc R
C24 C 0.4171(2) 0.65223(14) 0.41510(19) 0.0385(6) Uani 1 1 d .
H24A H 0.4713 0.6836 0.4382 0.046 Uiso 1 1 calc R
H24B H 0.3604 0.6488 0.4549 0.046 Uiso 1 1 calc R
C25 C 0.5121(3) 0.62328(17) 0.64246(19) 0.0433(7) Uani 1 1 d .
H25A H 0.5293 0.6597 0.6026 0.052 Uiso 1 1 calc R
H25B H 0.5777 0.6008 0.6619 0.052 Uiso 1 1 calc R
C26 C 0.4563(3) 0.65312(15) 0.71525(18) 0.0447(8) Uani 1 1 d .
H26A H 0.5051 0.6610 0.7633 0.054 Uiso 1 1 calc R
H26B H 0.4215 0.6967 0.6999 0.054 Uiso 1 1 calc R
C27 C 0.3777(3) 0.59868(18) 0.7343(2) 0.0530(9) Uani 1 1 d .
H27A H 0.4088 0.5629 0.7709 0.064 Uiso 1 1 calc R
H27B H 0.3161 0.6183 0.7608 0.064 Uiso 1 1 calc R
C28 C 0.3494(2) 0.57079(17) 0.64926(19) 0.0410(7) Uani 1 1 d .
H28A H 0.3251 0.5230 0.6531 0.049 Uiso 1 1 calc R
H28B H 0.2934 0.5985 0.6219 0.049 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'
Er Er -0.2586 4.9576 '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 Er1 N3 37.34(9) . 3_556
N3 Er1 N2 109.09(7) . .
N3 Er1 N2 116.06(7) 3_556 .
N3 Er1 N1 107.33(7) . .
N3 Er1 N1 121.30(7) 3_556 .
N2 Er1 N1 120.83(7) . .
N3 Er1 O1 119.78(7) . .
N3 Er1 O1 83.74(7) 3_556 .
N2 Er1 O1 108.01(7) . .
N1 Er1 O1 91.69(6) . .
N1 Si1 C1 112.80(10) . .
N1 Si1 C2 110.94(11) . .
C1 Si1 C2 108.32(14) . .
N1 Si1 C3 114.71(10) . .
C1 Si1 C3 104.57(12) . .
C2 Si1 C3 104.93(12) . .
N1 Si2 C4 110.06(10) . .
N1 Si2 C5 115.44(12) . .
C4 Si2 C5 105.41(12) . .
N1 Si2 C6 113.54(11) . .
C4 Si2 C6 106.49(12) . .
C5 Si2 C6 105.20(13) . .
N2 Si3 C7 111.63(11) . .
N2 Si3 C8 114.49(11) . .
C7 Si3 C8 106.03(14) . .
N2 Si3 C9 113.00(11) . .
C7 Si3 C9 105.69(14) . .
C8 Si3 C9 105.30(13) . .
N2 Si4 C11 109.40(10) . .
N2 Si4 C12 115.23(11) . .
C11 Si4 C12 105.52(13) . .
N2 Si4 C10 114.26(11) . .
C11 Si4 C10 106.16(13) . .
C12 Si4 C10 105.55(13) . .
N2 Si4 Er1 39.93(6) . .
C11 Si4 Er1 70.43(8) . .
C12 Si4 Er1 118.81(9) . .
C10 Si4 Er1 134.96(9) . .
C16 O1 C13 106.5(2) . .
C16 O1 Er1 125.84(15) . .
C13 O1 Er1 121.57(15) . .
Si2 N1 Si1 121.86(11) . .
Si2 N1 Er1 120.66(9) . .
Si1 N1 Er1 116.89(9) . .
Si4 N2 Si3 121.86(11) . .
Si4 N2 Er1 111.71(9) . .
Si3 N2 Er1 126.41(10) . .
N3 N3 Er1 72.11(15) 3_556 .
N3 N3 Er1 70.55(15) 3_556 3_556
Er1 N3 Er1 142.66(9) . 3_556
O1 C13 C14 106.3(2) . .
C13 C14 C15 106.2(3) . .
C14 C15 C16 105.0(3) . .
O1 C16 C15 105.2(2) . .
O2 Na1 O2 180.0 3_666 .
O2 Na1 O4 90.61(6) 3_666 .
O2 Na1 O4 89.39(6) . .
O2 Na1 O4 89.39(6) 3_666 3_666
O2 Na1 O4 90.61(6) . 3_666
O4 Na1 O4 180.00(8) . 3_666
O2 Na1 O3 89.21(7) 3_666 3_666
O2 Na1 O3 90.78(7) . 3_666
O4 Na1 O3 91.28(7) . 3_666
O4 Na1 O3 88.72(7) 3_666 3_666
O2 Na1 O3 90.79(7) 3_666 .
O2 Na1 O3 89.22(7) . .
O4 Na1 O3 88.72(7) . .
O4 Na1 O3 91.28(7) 3_666 .
O3 Na1 O3 180.00(10) 3_666 .
C20 O2 C17 106.4(2) . .
C20 O2 Na1 127.87(16) . .
C17 O2 Na1 125.36(16) . .
C24 O3 C21 108.8(2) . .
C24 O3 Na1 126.52(16) . .
C21 O3 Na1 124.42(17) . .
C25 O4 C28 109.3(2) . .
C25 O4 Na1 121.23(16) . .
C28 O4 Na1 128.31(16) . .
O2 C17 C18 105.0(2) . .
C19 C18 C17 102.9(3) . .
C18 C19 C20 106.4(2) . .
O2 C20 C19 106.2(2) . .
O3 C21 C22 107.3(3) . .
C21 C22 C23 101.3(3) . .
C24 C23 C22 103.1(3) . .
O3 C24 C23 105.4(3) . .
O4 C25 C26 106.9(2) . .
C27 C26 C25 102.9(2) . .
C28 C27 C26 102.3(2) . .
O4 C28 C27 105.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Er1 N3 2.1817(19) .
Er1 N3 2.2019(19) 3_556
Er1 N2 2.3029(18) .
Er1 N1 2.3177(18) .
Er1 O1 2.4108(18) .
Si1 N1 1.7142(18) .
Si1 C1 1.871(3) .
Si1 C2 1.872(3) .
Si1 C3 1.887(2) .
Si2 N1 1.6983(19) .
Si2 C4 1.884(2) .
Si2 C5 1.885(3) .
Si2 C6 1.886(3) .
Si3 N2 1.7058(19) .
Si3 C7 1.870(3) .
Si3 C8 1.882(3) .
Si3 C9 1.883(3) .
Si4 N2 1.704(2) .
Si4 C11 1.877(3) .
Si4 C12 1.878(3) .
Si4 C10 1.884(3) .
O1 C16 1.441(3) .
O1 C13 1.449(3) .
N3 N3 1.403(4) 3_556
N3 Er1 2.2018(19) 3_556
C13 C14 1.497(5) .
C14 C15 1.498(5) .
C15 C16 1.512(4) .
Na1 O2 2.3313(17) 3_666
Na1 O2 2.3313(17) .
Na1 O4 2.3560(17) .
Na1 O4 2.3560(17) 3_666
Na1 O3 2.3839(18) 3_666
Na1 O3 2.3839(18) .
O2 C20 1.430(3) .
O2 C17 1.431(3) .
O3 C24 1.430(3) .
O3 C21 1.431(4) .
O4 C25 1.431(3) .
O4 C28 1.432(3) .
C17 C18 1.509(4) .
C18 C19 1.501(4) .
C19 C20 1.501(4) .
C21 C22 1.482(5) .
C22 C23 1.504(5) .
C23 C24 1.498(5) .
C25 C26 1.514(4) .
C26 C27 1.507(5) .
C27 C28 1.506(4) .
