#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2008827.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008827
loop_
_publ_author_name
'Henderson, K. W.'
'Kennedy, A. R.'
'Kerr, W. J.'
'Moran, P. H.'
_publ_section_title
;
Redetermination of
di-\m-bromo-bis[(N,N,N',N'-tetramethylethylenediamine-N,N')lithium]
;
_journal_issue 8
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first IUC9900078
_journal_volume 55
_journal_year 1999
_chemical_formula_iupac '[Li2 Br2 (C6 H16 N2)2]'
_chemical_formula_moiety 'C12 H32 Br2 Li2 N4 '
_chemical_formula_sum 'C12 H32 Br2 Li2 N4'
_chemical_formula_weight 406.10
_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'
_audit_creation_method 'from TEXRAY.INF file'
_cell_angle_alpha 90
_cell_angle_beta 112.48(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.904(4)
_cell_length_b 12.042(2)
_cell_length_c 15.436(4)
_cell_measurement_reflns_used 18
_cell_measurement_temperature 173
_cell_measurement_theta_max 7.73
_cell_measurement_theta_min 6.30
_cell_volume 2044.6(10)
_computing_cell_refinement 'MSC/AFC Diffractometer Control'
_computing_data_collection
;
MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1985)
;
_computing_data_reduction
;
teXsan (Molecular Structure Corporation, 1993)
;
_computing_publication_material teXsan
_computing_structure_refinement teXsan
_computing_structure_solution 'DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature 173
_diffrn_measurement_device 'Rigaku AFC-7S'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0244
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 4993
_diffrn_reflns_theta_max 26.0
_diffrn_reflns_theta_min 2.5
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 3.972
_exptl_absorpt_correction_T_max 0.530
_exptl_absorpt_correction_T_min 0.337
_exptl_absorpt_correction_type '\y scan'
_exptl_absorpt_process_details '(North et al., 1968)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.319
_exptl_crystal_description tabular
_exptl_crystal_F_000 832.00
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.16
_refine_diff_density_max 0.70
_refine_diff_density_min -0.43
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_obs 1.228
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 181
_refine_ls_number_reflns 2393
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1066
_refine_ls_R_factor_obs 0.0363
_refine_ls_shift/esd_max <0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme 'w = 1/\s^2^(F)'
_refine_ls_wR_factor_all 0.0486
_refine_ls_wR_factor_obs 0.0403
_reflns_number_observed 2393
_reflns_number_total 3938
_reflns_observed_criterion I>2\s(I)
_[local]_cod_data_source_file qa0138.cif
_[local]_cod_data_source_block Pauls
_[local]_cod_cif_authors_sg_H-M 'P 21/n'
_[local]_cod_chemical_formula_sum_orig 'C12 H32 Br2 Li2 N4 '
_cod_original_cell_volume 2044.5(9)
_cod_database_code 2008827
loop_
_symmetry_equiv_pos_as_xyz
' +x, +y, +z'
1/2-x,1/2+y,1/2-z
' -x, -y, -z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0263(2) 0.0316(3) 0.0518(3) -0.0033(2) 0.0133(2) 0.0004(3)
Br2 0.0354(3) 0.0311(3) 0.0686(4) -0.0026(2) 0.0292(3) -0.0011(3)
N1 0.027(2) 0.035(2) 0.028(2) 0.003(2) 0.011(2) 0.000(2)
N2 0.032(2) 0.032(2) 0.032(2) -0.001(2) 0.014(2) 0.001(2)
N3 0.033(2) 0.043(2) 0.026(2) 0.000(2) 0.012(2) -0.003(2)
N4 0.028(2) 0.034(2) 0.028(2) 0.002(2) 0.010(2) -0.001(2)
C1 0.042(3) 0.070(4) 0.039(3) -0.001(3) 0.015(3) -0.001(3)
C2 0.046(3) 0.054(3) 0.052(4) -0.001(3) 0.033(3) -0.009(3)
C3 0.046(3) 0.029(3) 0.042(3) -0.006(2) 0.019(3) -0.005(2)
C4 0.044(3) 0.026(3) 0.050(3) 0.004(2) 0.018(3) 0.001(2)
C5 0.044(3) 0.069(4) 0.059(4) -0.005(3) 0.027(3) 0.011(3)
C6 0.047(3) 0.057(4) 0.037(3) 0.004(3) 0.009(3) 0.000(3)
C7 0.049(3) 0.078(5) 0.034(3) -0.008(3) 0.009(3) -0.018(3)
C8 0.048(3) 0.070(4) 0.048(3) 0.001(3) 0.028(3) 0.009(3)
C9 0.046(3) 0.038(3) 0.031(3) 0.010(2) 0.014(3) 0.008(2)
C10 0.051(3) 0.028(3) 0.043(3) -0.004(2) 0.020(3) -0.001(2)
C11 0.036(3) 0.051(3) 0.040(3) 0.007(3) 0.015(3) -0.005(3)
C12 0.033(3) 0.075(4) 0.047(4) 0.002(3) 0.003(3) -0.015(3)
Li1 0.036(4) 0.028(4) 0.041(5) 0.000(4) 0.019(4) -0.001(4)
Li2 0.034(5) 0.026(4) 0.035(5) -0.004(3) 0.014(4) 0.001(3)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Br1 0.18741(4) 0.13978(4) 0.29265(4) 0.0371 Uij
Br2 -0.15343(4) 0.12246(4) 0.27891(4) 0.0422 Uij
N1 -0.0076(3) -0.1054(3) 0.1665(3) 0.0299 Uij
N2 0.0644(3) -0.1278(3) 0.3693(3) 0.0319 Uij
N3 -0.0568(3) 0.3409(3) 0.1390(3) 0.0338 Uij
N4 0.0085(3) 0.4070(3) 0.3331(3) 0.0301 Uij
C1 -0.1244(5) -0.0946(5) 0.0874(4) 0.0503 Uij
C2 0.0905(5) -0.0920(5) 0.1322(4) 0.0462 Uij
C3 0.0023(4) -0.2144(4) 0.2118(4) 0.0384 Uij
C4 0.0959(5) -0.2108(4) 0.3121(4) 0.0402 Uij
C5 -0.0364(5) -0.1665(5) 0.3939(4) 0.0556 Uij
C6 0.1706(5) -0.1072(5) 0.4561(4) 0.0491 Uij
C7 -0.1593(5) 0.2844(5) 0.0664(4) 0.0555 Uij
C8 0.0399(5) 0.3568(5) 0.1033(4) 0.0525 Uij
C9 -0.0967(5) 0.4466(4) 0.1645(3) 0.0384 Uij
C10 -0.0080(5) 0.4874(4) 0.2582(4) 0.0401 Uij
C11 -0.0921(4) 0.4113(5) 0.3644(4) 0.0425 Uij
C12 0.1215(5) 0.4316(5) 0.4139(4) 0.0556 Uij
Li1 0.0196(7) 0.0071(6) 0.2781(6) 0.0338 Uij
Li2 0.0037(7) 0.2534(6) 0.2670(5) 0.0314 Uij
H1 -0.1319 -0.0217 0.0623 0.0604 Uij
H2 -0.1286 -0.1470 0.0403 0.0604 Uij
H3 -0.1887 -0.1080 0.1083 0.0604 Uij
H4 0.0807 -0.1446 0.0840 0.0555 Uij
H5 0.1666 -0.1036 0.1823 0.0555 Uij
H6 0.0879 -0.0190 0.1080 0.0555 Uij
H7 -0.0746 -0.2342 0.2126 0.0461 Uij
H8 0.0263 -0.2682 0.1773 0.0461 Uij
H9 0.1729 -0.1925 0.3108 0.0482 Uij
H10 0.1001 -0.2819 0.3397 0.0482 Uij
H11 -0.0428 -0.1204 0.4418 0.0667 Uij
H12 -0.1100 -0.1632 0.3401 0.0667 Uij
H13 -0.0216 -0.2409 0.4158 0.0667 Uij
H14 0.1875 -0.1716 0.4944 0.0589 Uij
H15 0.2389 -0.0899 0.4411 0.0589 Uij
H16 0.1540 -0.0466 0.4888 0.0589 Uij
H17 -0.2070 0.2475 0.0948 0.0666 Uij
H18 -0.2080 0.3375 0.0226 0.0666 Uij
H19 -0.1291 0.2316 0.0349 0.0666 Uij
H20 0.0616 0.2870 0.0855 0.0630 Uij
H21 0.0118 0.4047 0.0504 0.0630 Uij
H22 0.1088 0.3890 0.1509 0.0630 Uij
H23 -0.1028 0.5003 0.1178 0.0461 Uij
H24 -0.1741 0.4367 0.1678 0.0461 Uij
H25 -0.0377 0.5549 0.2732 0.0482 Uij
H26 0.0684 0.5004 0.2537 0.0482 Uij
H27 -0.0824 0.3547 0.4095 0.0510 Uij
H28 -0.0934 0.4817 0.3917 0.0510 Uij
H29 -0.1664 0.4002 0.3123 0.0510 Uij
H30 0.1256 0.5089 0.4270 0.0668 Uij
H31 0.1224 0.3913 0.4670 0.0668 Uij
H32 0.1895 0.4105 0.3997 0.0668 Uij
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.003 0.002 'International Tables'
H 0.000 0.000 'International Tables'
Br -0.290 2.459 'International Tables'
N 0.006 0.003 'International Tables'
Li 0.000 0.000 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 2 4
-3 3 3
0 4 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Li1 Br1 Li2 73.3(2) yes
Li1 Br2 Li2 73.0(3) yes
C1 N1 C2 108.9(4) no
C1 N1 C3 110.7(4) no
C1 N1 Li1 115.0(4) no
C2 N1 C3 109.9(4) no
C2 N1 Li1 109.2(4) no
C3 N1 Li1 103.0(3) no
C4 N2 C5 111.2(4) no
C4 N2 C6 109.5(4) no
C4 N2 Li1 100.5(3) no
C5 N2 C6 108.8(4) no
C5 N2 Li1 113.6(4) no
C6 N2 Li1 113.1(4) no
C7 N3 C8 108.4(4) no
C7 N3 C9 110.3(4) no
C7 N3 Li2 111.7(4) no
C8 N3 C9 111.7(4) no
C8 N3 Li2 112.4(4) no
C9 N3 Li2 102.2(3) no
C10 N4 C11 111.1(4) no
C10 N4 C12 109.8(4) no
C10 N4 Li2 103.2(3) no
C11 N4 C12 108.3(4) no
C11 N4 Li2 108.6(4) no
C12 N4 Li2 115.7(4) no
N1 C3 C4 110.6(4) no
N2 C4 C3 111.9(4) no
N3 C9 C10 111.1(4) no
N4 C10 C9 112.0(4) no
Br1 Li1 Br2 106.1(3) yes
Br1 Li1 N1 110.5(3) yes
Br1 Li1 N2 116.7(4) yes
Br2 Li1 N1 119.5(4) yes
Br2 Li1 N2 115.5(4) yes
N1 Li1 N2 88.3(3) yes
Br1 Li2 Br2 106.2(3) yes
Br1 Li2 N3 112.9(4) yes
Br1 Li2 N4 123.3(3) yes
Br2 Li2 N3 112.7(3) yes
Br2 Li2 N4 113.6(3) yes
N3 Li2 N4 87.2(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Li1 2.500(8) yes
Br1 Li2 2.480(8) yes
Br2 Li1 2.488(8) yes
Br2 Li2 2.507(8) yes
N1 C1 1.465(6) no
N1 C2 1.464(6) no
N1 C3 1.470(6) no
N1 Li1 2.117(9) yes
N2 C4 1.474(6) no
N2 C5 1.466(6) no
N2 C6 1.469(6) no
N2 Li1 2.081(9) yes
N3 C7 1.470(6) no
N3 C8 1.465(6) no
N3 C9 1.464(6) no
N3 Li2 2.108(9) yes
N4 C10 1.463(6) no
N4 C11 1.454(6) no
N4 C12 1.472(6) no
N4 Li2 2.102(9) yes
C3 C4 1.523(6) no
C9 C10 1.510(7) no