#------------------------------------------------------------------------------
#$Date: 2016-02-19 15:29:56 +0100 (vie 19 de feb de 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/85/2008583.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_2008583
loop_
_publ_author_name
'Clegg, William'
'Horsburgh, Lynne'
'Couper, Scott A.'
'Mulvey, Robert E.'
_publ_section_title
catena-Poly[[bis(μ-2,6-dimethylpiperidinido-N:N)dilithium]-μ-(N,N,N',N'-tetramethylethylenediamine-N:N')]
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              867
_journal_page_last               869
_journal_paper_doi               10.1107/S0108270199001171
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'Li2 (C6 H16 N2) (C7 H14 N)2'
_chemical_formula_sum            'C20 H44 Li2 N4'
_chemical_formula_weight         354.47
_chemical_name_systematic
;
catena-poly[[bis[μ-(2,6-dimethylpiperidinido)-N:N]dilithium]-μ-(N,N,N',N'-
tetramethylethylenediamine-N:N')]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                108.26(4)
_cell_angle_beta                 112.63(3)
_cell_angle_gamma                91.41(3)
_cell_formula_units_Z            1
_cell_length_a                   7.904(5)
_cell_length_b                   8.899(6)
_cell_length_c                   9.335(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      8.52
_cell_volume                     567.6(7)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Stoe-Siemens diffractometer with Cryostream cooler (Cosier & Glazer, 1986)'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4012
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             198
_exptl_crystal_size_max          1.15
_exptl_crystal_size_mid          0.85
_exptl_crystal_size_min          0.65
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0552P)²+0.1264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.109
_reflns_number_gt                1631
_reflns_number_total             2004
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ln1078.cif
_cod_data_source_block           rem59
_cod_database_code               2008583
_cod_database_fobs_code          2008583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Li .4472(3) .6233(2) .4892(3) .0253(4) Uani d . 1 . . Li
N1 .59448(13) .58437(11) .70404(12) .0238(3) Uani d . 1 . . N
C1 .49778(18) .56225(15) .80393(16) .0286(3) Uani d . 1 . . C
H1 .5781 .5111 .8814 .034 Uiso calc R 1 . . H
C2 .4659(2) .71986(16) .91008(18) .0368(3) Uani d . 1 . . C
H2A .3828 .7719 .8369 .044 Uiso calc R 1 . . H
H2B .4041 .6967 .9769 .044 Uiso calc R 1 . . H
C3 .6480(2) .83313(16) 1.02436(17) .0395(4) Uani d . 1 . . C
H3A .6227 .9400 1.0773 .047 Uiso calc R 1 . . H
H3B .7205 .7919 1.1128 .047 Uiso calc R 1 . . H
C4 .75924(19) .84824(16) .92790(17) .0360(3) Uani d . 1 . . C
H4A .8851 .9088 1.0059 .043 Uiso calc R 1 . . H
H4B .6983 .9093 .8552 .043 Uiso calc R 1 . . H
C5 .77594(17) .68274(15) .82182(16) .0296(3) Uani d . 1 . . C
H5 .8382 .6250 .8992 .035 Uiso calc R 1 . . H
C6 .90167(19) .70195(18) .73852(19) .0411(4) Uani d . 1 . . C
H6A 1.0232 .7627 .8228 .062 Uiso calc R 1 . . H
H6B .8460 .7597 .6626 .062 Uiso calc R 1 . . H
H6C .9172 .5959 .6763 .062 Uiso calc R 1 . . H
C7 .3142(2) .44993(17) .69851(18) .0379(4) Uani d . 1 . . C
H7A .2559 .4351 .7698 .057 Uiso calc R 1 . . H
H7B .3355 .3460 .6373 .057 Uiso calc R 1 . . H
H7C .2321 .4959 .6200 .057 Uiso calc R 1 . . H
N2 .31558(14) .82032(12) .43349(13) .0268(3) Uani d . 1 . . N
C8 .41197(17) .98801(14) .51236(16) .0283(3) Uani d . 1 . . C
H8A .4437 1.0232 .6326 .034 Uiso calc R 1 . . H
H8B .3263 1.0569 .4663 .034 Uiso calc R 1 . . H
C9 .2419(2) .76955(16) .25212(17) .0381(4) Uani d . 1 . . C
H9A .3452 .7699 .2187 .057 Uiso calc R 1 . . H
H9B .1615 .8439 .2142 .057 Uiso calc R 1 . . H
H9C .1699 .6611 .2024 .057 Uiso calc R 1 . . H
C10 .1593(2) .81009(18) .4807(2) .0417(4) Uani d . 1 . . C
H10A .2062 .8477 .6017 .062 Uiso calc R 1 . . H
H10B .0966 .6985 .4340 .062 Uiso calc R 1 . . H
H10C .0711 .8773 .4377 .062 Uiso calc R 1 . . H
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
Li .0263(10) .0199(10) .0278(10) .0063(8) .0094(8) .0081(8)
N1 .0253(5) .0200(5) .0226(5) .0034(4) .0076(4) .0059(4)
C1 .0363(7) .0239(7) .0265(7) .0072(5) .0130(5) .0098(5)
C2 .0521(8) .0302(7) .0345(8) .0113(6) .0250(7) .0103(6)
C3 .0607(9) .0244(7) .0261(7) .0109(6) .0140(6) .0040(6)
C4 .0386(7) .0240(7) .0303(7) -.0005(5) .0027(6) .0052(6)
C5 .0291(6) .0248(7) .0270(7) .0039(5) .0042(5) .0083(5)
C6 .0299(7) .0410(8) .0443(9) .0012(6) .0105(6) .0109(7)
C7 .0416(8) .0319(8) .0431(8) .0031(6) .0216(7) .0117(6)
N2 .0288(5) .0199(5) .0283(6) .0059(4) .0085(4) .0081(4)
C8 .0331(7) .0193(6) .0299(7) .0081(5) .0115(5) .0068(5)
C9 .0436(8) .0279(7) .0287(7) .0056(6) .0011(6) .0090(6)
C10 .0348(7) .0341(8) .0566(10) .0068(6) .0195(7) .0157(7)
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'
Li Li -0.0003 0.0001 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Li N1 . 2_666 107.89(11) yes
N1 Li N2 . . 133.67(11) yes
N1 Li N2 2_666 . 118.15(11) yes
C1 N1 C5 . . 106.17(11) yes
C1 N1 Li . . 118.93(11) no
C5 N1 Li . . 120.72(10) no
C1 N1 Li . 2_666 111.19(10) no
C5 N1 Li . 2_666 125.23(10) no
Li N1 Li . 2_666 72.11(11) yes
N1 C1 C7 . . 111.86(12) no
N1 C1 C2 . . 113.57(11) no
C7 C1 C2 . . 109.30(12) no
C3 C2 C1 . . 111.12(13) no
C4 C3 C2 . . 110.21(12) no
C3 C4 C5 . . 111.42(12) no
N1 C5 C6 . . 112.66(12) no
N1 C5 C4 . . 112.68(11) no
C6 C5 C4 . . 110.03(12) no
C9 N2 C10 . . 108.67(12) no
C9 N2 C8 . . 111.03(11) no
C10 N2 C8 . . 107.98(11) no
C9 N2 Li . . 104.03(10) no
C10 N2 Li . . 101.24(10) no
C8 N2 Li . . 122.92(10) yes
N2 C8 C8 . 2_676 113.35(13) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li N1 . 2.038(3) yes
Li N1 2_666 2.050(3) yes
Li N2 . 2.161(2) yes
N1 C1 . 1.466(2) no
N1 C5 . 1.468(2) no
N1 Li 2_666 2.050(3) no
C1 C7 . 1.512(2) no
C1 C2 . 1.533(2) no
C2 C3 . 1.516(2) no
C3 C4 . 1.510(2) no
C4 C5 . 1.537(2) no
C5 C6 . 1.514(2) no
N2 C9 . 1.469(2) no
N2 C10 . 1.472(2) no
N2 C8 . 1.474(2) no
C8 C8 2_676 1.516(3) no
