#------------------------------------------------------------------------------
#$Date: 2017-05-06 01:12:29 +0300 (Sat, 06 May 2017) $
#$Revision: 196459 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/25/7042507.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_7042507
loop_
_publ_author_name
'Szimhardt, Norbert'
'Bölter, Marc F'
'Born, Maximilian'
'Klapötke, Thomas M'
'Stierstorfer, Jörg'
_publ_section_title
;
 Metal salts and complexes of 1,1'-dinitramino-5,5'-bitetrazole.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5033
_journal_page_last               5040
_journal_paper_doi               10.1039/c7dt00536a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C H2 Li N6 O3'
_chemical_formula_sum            'C H2 Li N6 O3'
_chemical_formula_weight         153.03
_chemical_name_common
'lithium dinitramino-5,5-bitetrazolate monohydrate'
_chemical_name_systematic
;
lithium dinitramino-5,5-bitetrazolate monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date
;
'Fri Mar 11 16:36:00 2016'
;
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.073(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2760(9)
_cell_length_b                   10.8140(8)
_cell_length_c                   6.0650(4)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.4320
_cell_measurement_theta_min      4.5570
_cell_volume                     521.58(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -92.00  -65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -89.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   19.0000 -180.0000 133

#__ type_ start__ end____ width___ exp.time_
  3 omega -109.00  -72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
  4 omega  -28.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -90.0000   35.0000 31

#__ type_ start__ end____ width___ exp.time_
  5 omega    6.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  179.0000  -60.0000 35

#__ type_ start__ end____ width___ exp.time_
  7 omega   10.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 65

#__ type_ start__ end____ width___ exp.time_
  8 omega   45.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000  -90.0000 41

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0839389000
_diffrn_orient_matrix_UB_12      -0.0033356000
_diffrn_orient_matrix_UB_13      0.0705785000
_diffrn_orient_matrix_UB_21      -0.0086754000
_diffrn_orient_matrix_UB_22      0.0594818000
_diffrn_orient_matrix_UB_23      0.0447809000
_diffrn_orient_matrix_UB_31      -0.0288041000
_diffrn_orient_matrix_UB_32      -0.0274584000
_diffrn_orient_matrix_UB_33      0.0884395000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3905
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.746
_diffrn_reflns_theta_min         4.169
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.99999
_exptl_absorpt_correction_T_min  0.84687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0311P)²+0.1742P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                893
_reflns_number_total             1105
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00536a2.cif
_cod_data_source_block           lx129
_cod_depositor_comments
'Adding full bibliography for 7042497--7042508.cif.'
_cod_database_code               7042507
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
O3 O 0.31129(15) -0.03082(11) 0.86217(19) 0.0216(3) Uani 1 1 d
O1 O -0.00439(19) -0.38111(12) 0.6910(2) 0.0197(3) Uani 1 1 d
O2 O 0.08425(15) -0.13688(11) 0.7008(2) 0.0178(3) Uani 1 1 d
N5 N 0.31100(18) -0.18407(13) 0.6050(2) 0.0159(3) Uani 1 1 d
N3 N 0.60228(18) -0.22284(13) 0.7612(2) 0.0166(3) Uani 1 1 d
N4 N 0.47859(18) -0.14838(13) 0.6444(2) 0.0152(3) Uani 1 1 d
N6 N 0.23986(18) -0.11412(12) 0.7309(2) 0.0147(3) Uani 1 1 d
N1 N 0.71261(18) -0.06096(13) 0.6374(2) 0.0161(3) Uani 1 1 d
N2 N 0.74172(19) -0.17014(13) 0.7555(2) 0.0160(3) Uani 1 1 d
C1 C 0.5476(2) -0.04975(15) 0.5685(3) 0.0150(4) Uani 1 1 d
Li1 Li -0.0034(4) -0.2617(3) 0.4294(5) 0.0200(6) Uani 1 1 d
H1A H -0.095(3) -0.429(2) 0.661(4) 0.048(7) Uiso 1 1 d
H1B H 0.070(3) -0.424(2) 0.745(4) 0.046(8) Uiso 1 1 d
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'
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'
O O 0.0106 0.0060 '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'
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
Li1 O1 Li1 93.97(5) . 4_556
N6 O2 Li1 122.62(13) . 4_556
N6 O2 Li1 110.70(13) . .
Li1 O2 Li1 94.37(8) 4_556 .
N6 N5 N4 108.86(13) . .
N6 N5 Li1 82.50(11) . .
N4 N5 Li1 166.36(12) . .
N2 N3 N4 106.09(13) . .
N3 N4 C1 108.75(14) . .
N3 N4 N5 120.12(13) . .
C1 N4 N5 130.92(14) . .
O3 N6 O2 121.10(13) . .
O3 N6 N5 125.25(14) . .
O2 N6 N5 113.61(13) . .
C1 N1 N2 105.21(14) . .
N3 N2 N1 111.38(14) . .
N3 N2 Li1 125.50(13) . 4_656
N1 N2 Li1 123.02(13) . 4_656
N1 C1 N4 108.57(14) . .
N1 C1 C1 126.90(19) . 3_656
N4 C1 C1 124.53(19) . 3_656
O1 Li1 O2 105.36(14) . 4
O1 Li1 O2 82.67(11) . .
O2 Li1 O2 139.85(17) 4 .
O1 Li1 O1 172.14(16) . 4
O2 Li1 O1 82.15(11) 4 4
O2 Li1 O1 90.08(12) . 4
O1 Li1 N2 87.23(12) . 4_455
O2 Li1 N2 88.21(12) 4 4_455
O2 Li1 N2 131.84(15) . 4_455
O1 Li1 N2 95.45(13) 4 4_455
O1 Li1 N5 95.85(12) . .
O2 Li1 N5 87.11(11) 4 .
O2 Li1 N5 52.76(8) . .
O1 Li1 N5 82.03(11) 4 .
N2 Li1 N5 174.95(14) 4_455 .
O1 Li1 Li1 43.88(8) . 4_556
O2 Li1 Li1 144.66(16) 4 4_556
O2 Li1 Li1 42.23(9) . 4_556
O1 Li1 Li1 128.27(17) 4 4_556
N2 Li1 Li1 103.91(9) 4_455 4_556
N5 Li1 Li1 81.05(7) . 4_556
O1 Li1 Li1 145.69(18) . 4
O2 Li1 Li1 43.40(8) 4 4
O2 Li1 Li1 129.27(16) . 4
O1 Li1 Li1 42.15(9) 4 4
N2 Li1 Li1 79.36(8) 4_455 4
N5 Li1 Li1 95.90(8) . 4
Li1 Li1 Li1 170.4(2) 4_556 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O3 N6 1.2385(17) .
O1 Li1 2.047(3) .
O1 Li1 2.114(3) 4_556
O2 N6 1.2736(18) .
O2 Li1 2.051(3) 4_556
O2 Li1 2.097(3) .
N5 N6 1.3232(19) .
N5 N4 1.395(2) .
N5 Li1 2.660(3) .
N3 N2 1.296(2) .
N3 N4 1.340(2) .
N4 C1 1.350(2) .
N1 C1 1.318(2) .
N1 N2 1.3673(19) .
N2 Li1 2.207(3) 4_656
C1 C1 1.452(3) 3_656
Li1 O2 2.051(3) 4
Li1 O1 2.114(3) 4
Li1 N2 2.207(3) 4_455
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O3 0.89(3) 2.07(3) 2.9534(19) 171(2) 2_546
O1 H1A O2 0.89(3) 2.39(3) 2.9595(17) 122(2) 2_546
O1 H1A N6 0.89(3) 2.51(3) 3.2988(19) 148(2) 2_546
O1 H1B N1 0.76(3) 2.29(3) 3.050(2) 173(3) 2_646
