#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239071.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_2239071
loop_
_publ_author_name
'Xie, Qianwen'
'Tong, Hongbo'
'Zhou, Meisu'
_publ_section_title
;
 catena-Poly[[(N,N-dimethylcyanamide-κN)lithium]-μ₃-bromido]
;
_journal_coeditor_code           SJ5383
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m69
_journal_page_last               m70
_journal_paper_doi               10.1107/S1600536814001652
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Li Br (C3 H6 N2)]'
_chemical_formula_moiety         'C3 H6 Br Li N2'
_chemical_formula_sum            'C3 H6 Br Li N2'
_chemical_formula_weight         156.85
_chemical_name_systematic
catena-Poly[[(N,N-dimethylcyanamide-κN)lithium]-μ₃-bromido]
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.089(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.2680(8)
_cell_length_b                   17.214(3)
_cell_length_c                   8.9685(17)
_cell_measurement_reflns_used    1538
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.483
_cell_measurement_theta_min      2.366
_cell_volume                     648.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3498
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    6.215
_exptl_absorpt_correction_T_max  0.2410
_exptl_absorpt_correction_T_min  0.2196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.382
_refine_ls_extinction_coef       0.0053(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0247
_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)+(0.0285P)²+0.3312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                965
_reflns_number_total             1140
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            sj5383sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239071
_cod_database_fobs_code          2239071
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_type_symbol
_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_symmetry_multiplicity
Li Li1 0.2655(11) 0.4372(3) 0.0594(6) 0.0289(11) Uani d . 1 1
Br Br1 0.81425(7) 0.485193(18) 0.18525(3) 0.03230(16) Uani d . 1 1
N N1 0.2914(7) 0.32132(16) 0.0517(3) 0.0475(8) Uani d . 1 1
N N2 0.5102(8) 0.18972(16) 0.0853(3) 0.0509(8) Uani d . 1 1
C C1 0.3896(8) 0.25987(19) 0.0667(4) 0.0352(8) Uani d . 1 1
C C2 0.3986(11) 0.1281(2) -0.0201(5) 0.0672(12) Uani d . 1 1
H H2A 0.2384 0.1487 -0.1023 0.101 Uiso calc R 1 1
H H2B 0.3037 0.0868 0.0327 0.101 Uiso calc R 1 1
H H2C 0.5779 0.1070 -0.0621 0.101 Uiso calc R 1 1
C C3 0.7254(9) 0.1720(2) 0.2260(5) 0.0581(11) Uani d . 1 1
H H3A 0.7997 0.2206 0.2775 0.087 Uiso calc R 1 1
H H3B 0.9081 0.1426 0.2035 0.087 Uiso calc R 1 1
H H3C 0.6130 0.1410 0.2916 0.087 Uiso calc R 1 1
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
Li1 0.025(3) 0.022(3) 0.038(3) 0.0034(19) 0.001(2) 0.004(2)
Br1 0.0248(2) 0.0371(2) 0.0339(2) 0.00073(13) 0.00223(13) 0.00497(14)
N1 0.052(2) 0.0287(17) 0.057(2) 0.0056(14) -0.0034(15) 0.0025(14)
N2 0.068(2) 0.0252(16) 0.053(2) 0.0129(14) -0.0071(16) -0.0022(14)
C1 0.035(2) 0.032(2) 0.0363(19) -0.0027(15) -0.0003(14) -0.0015(14)
C2 0.108(4) 0.036(2) 0.062(3) -0.003(2) 0.027(2) -0.0161(19)
C3 0.050(2) 0.058(3) 0.065(3) 0.0178(19) 0.003(2) 0.019(2)
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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N1 Li1 Br1 . 1_455 113.1(2)
N1 Li1 Br1 . 3_665 119.6(2)
Br1 Li1 Br1 1_455 3_665 102.45(16)
N1 Li1 Br1 . . 106.6(2)
Br1 Li1 Br1 1_455 . 114.03(19)
Br1 Li1 Br1 3_665 . 100.67(17)
N1 Li1 Li1 . 3_565 135.1(3)
Br1 Li1 Li1 1_455 3_565 51.30(14)
Br1 Li1 Li1 3_665 3_565 51.15(14)
Br1 Li1 Li1 . 3_565 118.2(2)
N1 Li1 Li1 . 3_665 127.7(3)
Br1 Li1 Li1 1_455 3_665 119.2(2)
Br1 Li1 Li1 3_665 3_665 50.50(13)
Br1 Li1 Li1 . 3_665 50.17(13)
Li1 Li1 Li1 3_565 3_665 83.2(2)
Li1 Br1 Li1 1_655 3_665 77.55(16)
Li1 Br1 Li1 1_655 . 114.03(19)
Li1 Br1 Li1 3_665 . 79.33(17)
C1 N1 Li1 . . 161.0(3)
C1 N2 C2 . . 121.0(3)
C1 N2 C3 . . 118.4(3)
C2 N2 C3 . . 119.9(3)
N1 C1 N2 . . 178.5(4)
N2 C2 H2A . . 109.5
N2 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
N2 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
N2 C3 H3A . . 109.5
N2 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
N2 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Li1 N1 . 1.999(5)
Li1 Br1 1_455 2.535(5)
Li1 Br1 3_665 2.541(5)
Li1 Br1 . 2.553(5)
Li1 Li1 3_565 3.179(9)
Li1 Li1 3_665 3.251(10)
Br1 Li1 1_655 2.535(5)
Br1 Li1 3_665 2.541(5)
N1 C1 . 1.137(4)
N2 C1 . 1.312(4)
N2 C2 . 1.445(5)
N2 C3 . 1.457(5)
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
