# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kx346
_database_code_depnum_ccdc_archive 'CCDC 1500001'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_block_code                ?
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_audit_creation_date             
;
'Wed Sep 23 19:50:06 2015'
;

_chemical_name_systematic        'rubidium 1,1-dinitramino-5,5-bitetrazolate'
_chemical_compound_source        ?
_chemical_name_common            'rubidium 1,1-dinitramino-5,5-bitetrazolate'
_chemical_formula_moiety         'C2 N12 O4, 2(Rb)'
_chemical_formula_sum            'C2 N12 O4 Rb2'
_chemical_formula_weight         427.08


_cell_length_a                   5.3034(5)
_cell_length_b                   7.0632(6)
_cell_length_c                   8.5675(7)
_cell_angle_alpha                66.821(8)
_cell_angle_beta                 86.667(7)
_cell_angle_gamma                70.964(8)
_cell_volume                     277.98(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1482
_cell_measurement_theta_min      4.4890
_cell_measurement_theta_max      30.1460
_cell_special_details            ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             202
_exptl_absorpt_coefficient_mu    8.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1121
_exptl_absorpt_correction_T_max  0.7773
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173 # in K
_diffrn_source_type              'Spellman generator'
_diffrn_source_power             ? # in kW
_diffrn_source_voltage           50 # kV
_diffrn_source_current           40 # mA
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_collimation    0.5
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_detector_area_resol_mean 15.9809

_diffrn_reflns_number            3969
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.33
_diffrn_reflns_theta_max         26.00
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996

_reflns_number_total             1096
_reflns_number_gt                1000
_reflns_threshold_expression     >2sigma(I)

_diffrn_orient_matrix_UB_11      -0.0359323000
_diffrn_orient_matrix_UB_12      0.1043579000
_diffrn_orient_matrix_UB_13      -0.0681604000
_diffrn_orient_matrix_UB_21      0.0327472000
_diffrn_orient_matrix_UB_22      -0.0500571000
_diffrn_orient_matrix_UB_23      -0.0591837000
_diffrn_orient_matrix_UB_31      -0.1333597000
_diffrn_orient_matrix_UB_32      0.0003005000
_diffrn_orient_matrix_UB_33      -0.0039403000

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  -P1

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'
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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_exptl_special_details           ?


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

_diffrn_special_details          ?

_refine_diff_density_max         0.487
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.098

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+0.0812P] where P=(Fo²+2Fc²)/3'


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
# Plot Program for Crystal Structure Illustrations, Oak Ridge National
# Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
# Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
# Germany, 1995)'
;

_computing_publication_material  
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
# --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         1096
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0491
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3925(4) 0.8049(4) 0.5206(3) 0.0210(5) Uani 1 1 d . . .
O2 O 0.6591(4) 0.6649(4) 0.3615(3) 0.0223(5) Uani 1 1 d . . .
N2 N 0.1987(5) 0.7053(4) 0.0815(3) 0.0197(6) Uani 1 1 d . . .
N3 N 0.2829(5) 0.7192(4) -0.0674(3) 0.0213(6) Uani 1 1 d . . .
N4 N 0.4328(5) 0.8538(4) -0.1218(3) 0.0199(6) Uani 1 1 d . . .
N1 N 0.2950(5) 0.8323(4) 0.1268(3) 0.0168(5) Uani 1 1 d . . .
N5 N 0.2211(5) 0.8678(4) 0.2743(3) 0.0181(6) Uani 1 1 d . . .
N6 N 0.4346(5) 0.7722(4) 0.3863(3) 0.0166(5) Uani 1 1 d . . .
C1 C 0.4358(6) 0.9237(5) -0.0001(4) 0.0157(6) Uani 1 1 d . . .
Rb1 Rb 0.07635(5) 0.29417(5) 0.33881(4) 0.01919(11) Uani 1 1 d . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N6 1.254(3) . ?
O1 Rb1 2.871(2) 2_566 ?
O1 Rb1 2.885(2) 2_666 ?
O1 Rb1 3.077(2) 1_565 ?
O2 N6 1.243(3) . ?
O2 Rb1 2.892(2) 1_655 ?
O2 Rb1 3.148(2) 2_666 ?
N2 N3 1.304(4) . ?
N2 N1 1.347(3) . ?
N2 Rb1 3.120(3) . ?
N3 N4 1.362(4) . ?
N3 Rb1 3.139(2) 2_565 ?
N4 C1 1.320(4) . ?
N4 Rb1 3.243(3) 2_665 ?
N1 C1 1.351(4) . ?
N1 N5 1.393(3) . ?
N5 N6 1.333(3) . ?
N5 Rb1 3.117(3) 1_565 ?
N5 Rb1 3.517(2) 2_566 ?
N6 Rb1 3.397(2) 2_666 ?
N6 Rb1 3.422(3) 1_565 ?
N6 Rb1 3.511(2) 2_566 ?
C1 C1 1.451(6) 2_675 ?
Rb1 O1 2.871(2) 2_566 ?
Rb1 O1 2.885(2) 2_666 ?
Rb1 O2 2.892(2) 1_455 ?
Rb1 O1 3.077(2) 1_545 ?
Rb1 N5 3.117(3) 1_545 ?
Rb1 N3 3.139(2) 2_565 ?
Rb1 O2 3.148(2) 2_666 ?
Rb1 N4 3.243(3) 2_665 ?
Rb1 N6 3.397(2) 2_666 ?
Rb1 N6 3.422(3) 1_545 ?
Rb1 N6 3.511(2) 2_566 ?

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
_geom_angle_publ_flag
N6 O1 Rb1 110.39(16) . 2_566 ?
N6 O1 Rb1 103.15(15) . 2_666 ?
Rb1 O1 Rb1 134.24(8) 2_566 2_666 ?
N6 O1 Rb1 94.98(16) . 1_565 ?
Rb1 O1 Rb1 92.40(6) 2_566 1_565 ?
Rb1 O1 Rb1 115.09(7) 2_666 1_565 ?
N6 O2 Rb1 157.95(18) . 1_655 ?
N6 O2 Rb1 90.60(16) . 2_666 ?
Rb1 O2 Rb1 99.44(6) 1_655 2_666 ?
N3 N2 N1 106.4(2) . . ?
N3 N2 Rb1 122.46(19) . . ?
N1 N2 Rb1 124.30(18) . . ?
N2 N3 N4 111.2(2) . . ?
N2 N3 Rb1 120.36(18) . 2_565 ?
N4 N3 Rb1 118.59(17) . 2_565 ?
C1 N4 N3 105.4(2) . . ?
C1 N4 Rb1 127.95(18) . 2_665 ?
N3 N4 Rb1 114.30(18) . 2_665 ?
N2 N1 C1 108.1(2) . . ?
N2 N1 N5 120.6(2) . . ?
C1 N1 N5 130.9(2) . . ?
N6 N5 N1 108.8(2) . . ?
N6 N5 Rb1 91.47(16) . 1_565 ?
N1 N5 Rb1 129.99(18) . 1_565 ?
N6 N5 Rb1 78.80(14) . 2_566 ?
N1 N5 Rb1 146.88(18) . 2_566 ?
Rb1 N5 Rb1 80.46(5) 1_565 2_566 ?
O2 N6 O1 121.8(2) . . ?
O2 N6 N5 124.4(2) . . ?
O1 N6 N5 113.8(2) . . ?
O2 N6 Rb1 67.93(14) . 2_666 ?
O1 N6 Rb1 55.79(13) . 2_666 ?
N5 N6 Rb1 160.40(19) . 2_666 ?
O2 N6 Rb1 140.01(18) . 1_565 ?
O1 N6 Rb1 63.61(14) . 1_565 ?
N5 N6 Rb1 65.61(15) . 1_565 ?
Rb1 N6 Rb1 95.10(6) 2_666 1_565 ?
O2 N6 Rb1 140.16(18) . 2_566 ?
O1 N6 Rb1 50.05(13) . 2_566 ?
N5 N6 Rb1 79.33(14) . 2_566 ?
Rb1 N6 Rb1 100.29(6) 2_666 2_566 ?
Rb1 N6 Rb1 76.57(5) 1_565 2_566 ?
N4 C1 N1 109.0(3) . . ?
N4 C1 C1 126.7(3) . 2_675 ?
N1 C1 C1 124.3(3) . 2_675 ?
O1 Rb1 O1 134.24(8) 2_566 2_666 ?
O1 Rb1 O2 66.66(6) 2_566 1_455 ?
O1 Rb1 O2 117.53(6) 2_666 1_455 ?
O1 Rb1 O1 87.60(6) 2_566 1_545 ?
O1 Rb1 O1 64.91(7) 2_666 1_545 ?
O2 Rb1 O1 145.95(6) 1_455 1_545 ?
O1 Rb1 N5 85.79(6) 2_566 1_545 ?
O1 Rb1 N5 94.15(6) 2_666 1_545 ?
O2 Rb1 N5 147.27(6) 1_455 1_545 ?
O1 Rb1 N5 40.96(6) 1_545 1_545 ?
O1 Rb1 N2 136.09(6) 2_566 . ?
O1 Rb1 N2 81.52(6) 2_666 . ?
O2 Rb1 N2 74.32(7) 1_455 . ?
O1 Rb1 N2 135.96(6) 1_545 . ?
N5 Rb1 N2 121.45(7) 1_545 . ?
O1 Rb1 N3 68.44(6) 2_566 2_565 ?
O1 Rb1 N3 147.93(6) 2_666 2_565 ?
O2 Rb1 N3 91.06(6) 1_455 2_565 ?
O1 Rb1 N3 100.06(6) 1_545 2_565 ?
N5 Rb1 N3 61.36(7) 1_545 2_565 ?
N2 Rb1 N3 93.67(7) . 2_565 ?
O1 Rb1 O2 102.75(6) 2_566 2_666 ?
O1 Rb1 O2 42.11(5) 2_666 2_666 ?
O2 Rb1 O2 80.56(6) 1_455 2_666 ?
O1 Rb1 O2 84.13(6) 1_545 2_666 ?
N5 Rb1 O2 124.47(6) 1_545 2_666 ?
N2 Rb1 O2 89.54(6) . 2_666 ?
N3 Rb1 O2 169.87(6) 2_565 2_666 ?
O1 Rb1 N4 141.22(6) 2_566 2_665 ?
O1 Rb1 N4 63.57(6) 2_666 2_665 ?
O2 Rb1 N4 144.22(7) 1_455 2_665 ?
O1 Rb1 N4 69.36(6) 1_545 2_665 ?
N5 Rb1 N4 56.22(6) 1_545 2_665 ?
N2 Rb1 N4 70.51(7) . 2_665 ?
N3 Rb1 N4 84.86(6) 2_565 2_665 ?
O2 Rb1 N4 105.26(6) 2_666 2_665 ?
O1 Rb1 N6 117.64(6) 2_566 2_666 ?
O1 Rb1 N6 21.06(5) 2_666 2_666 ?
O2 Rb1 N6 100.78(6) 1_455 2_666 ?
O1 Rb1 N6 70.85(6) 1_545 2_666 ?
N5 Rb1 N6 107.77(6) 1_545 2_666 ?
N2 Rb1 N6 88.16(6) . 2_666 ?
N3 Rb1 N6 168.06(6) 2_565 2_666 ?
O2 Rb1 N6 21.46(5) 2_666 2_666 ?
N4 Rb1 N6 84.63(6) 2_665 2_666 ?
O1 Rb1 N6 95.16(6) 2_566 1_545 ?
O1 Rb1 N6 72.67(6) 2_666 1_545 ?
O2 Rb1 N6 161.61(6) 1_455 1_545 ?
O1 Rb1 N6 21.41(5) 1_545 1_545 ?
N5 Rb1 N6 22.92(6) 1_545 1_545 ?
N2 Rb1 N6 123.64(6) . 1_545 ?
N3 Rb1 N6 84.27(6) 2_565 1_545 ?
O2 Rb1 N6 101.92(6) 2_666 1_545 ?
N4 Rb1 N6 53.17(6) 2_665 1_545 ?
N6 Rb1 N6 84.90(6) 2_666 1_545 ?
O1 Rb1 N6 19.56(5) 2_566 2_566 ?
O1 Rb1 N6 119.30(6) 2_666 2_566 ?
O2 Rb1 N6 58.48(6) 1_455 2_566 ?
O1 Rb1 N6 89.81(6) 1_545 2_566 ?
N5 Rb1 N6 100.13(6) 1_545 2_566 ?
N2 Rb1 N6 132.79(6) . 2_566 ?
N3 Rb1 N6 87.12(6) 2_565 2_566 ?
O2 Rb1 N6 83.66(5) 2_666 2_566 ?
N4 Rb1 N6 155.90(6) 2_665 2_566 ?
N6 Rb1 N6 100.29(6) 2_666 2_566 ?
N6 Rb1 N6 103.43(5) 1_545 2_566 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N2 N3 N4 -0.2(3) . . . . ?
Rb1 N2 N3 N4 -152.20(18) . . . . ?
N1 N2 N3 Rb1 -145.42(18) . . . 2_565 ?
Rb1 N2 N3 Rb1 62.6(2) . . . 2_565 ?
N2 N3 N4 C1 -0.4(3) . . . . ?
Rb1 N3 N4 C1 145.49(19) 2_565 . . . ?
N2 N3 N4 Rb1 145.07(19) . . . 2_665 ?
Rb1 N3 N4 Rb1 -69.0(2) 2_565 . . 2_665 ?
N3 N2 N1 C1 0.7(3) . . . . ?
Rb1 N2 N1 C1 152.08(19) . . . . ?
N3 N2 N1 N5 174.4(2) . . . . ?
Rb1 N2 N1 N5 -34.3(3) . . . . ?
N2 N1 N5 N6 112.5(3) . . . . ?
C1 N1 N5 N6 -75.5(4) . . . . ?
N2 N1 N5 Rb1 -138.8(2) . . . 1_565 ?
C1 N1 N5 Rb1 33.2(4) . . . 1_565 ?
N2 N1 N5 Rb1 14.1(5) . . . 2_566 ?
C1 N1 N5 Rb1 -173.9(2) . . . 2_566 ?
Rb1 O2 N6 O1 102.4(5) 1_655 . . . ?
Rb1 O2 N6 O1 -15.2(3) 2_666 . . . ?
Rb1 O2 N6 N5 -79.8(6) 1_655 . . . ?
Rb1 O2 N6 N5 162.6(3) 2_666 . . . ?
Rb1 O2 N6 Rb1 117.6(5) 1_655 . . 2_666 ?
Rb1 O2 N6 Rb1 -171.9(3) 1_655 . . 1_565 ?
Rb1 O2 N6 Rb1 70.5(2) 2_666 . . 1_565 ?
Rb1 O2 N6 Rb1 38.3(6) 1_655 . . 2_566 ?
Rb1 O2 N6 Rb1 -79.3(2) 2_666 . . 2_566 ?
Rb1 O1 N6 O2 -131.2(2) 2_566 . . . ?
Rb1 O1 N6 O2 17.1(3) 2_666 . . . ?
Rb1 O1 N6 O2 134.3(2) 1_565 . . . ?
Rb1 O1 N6 N5 50.7(3) 2_566 . . . ?
Rb1 O1 N6 N5 -160.95(19) 2_666 . . . ?
Rb1 O1 N6 N5 -43.7(2) 1_565 . . . ?
Rb1 O1 N6 Rb1 -148.34(16) 2_566 . . 2_666 ?
Rb1 O1 N6 Rb1 117.22(10) 1_565 . . 2_666 ?
Rb1 O1 N6 Rb1 94.44(11) 2_566 . . 1_565 ?
Rb1 O1 N6 Rb1 -117.22(10) 2_666 . . 1_565 ?
Rb1 O1 N6 Rb1 148.34(16) 2_666 . . 2_566 ?
Rb1 O1 N6 Rb1 -94.44(11) 1_565 . . 2_566 ?
N1 N5 N6 O2 -1.7(4) . . . . ?
Rb1 N5 N6 O2 -135.2(2) 1_565 . . . ?
Rb1 N5 N6 O2 144.9(3) 2_566 . . . ?
N1 N5 N6 O1 176.3(2) . . . . ?
Rb1 N5 N6 O1 42.8(2) 1_565 . . . ?
Rb1 N5 N6 O1 -37.1(2) 2_566 . . . ?
N1 N5 N6 Rb1 122.7(5) . . . 2_666 ?
Rb1 N5 N6 Rb1 -10.8(5) 1_565 . . 2_666 ?
Rb1 N5 N6 Rb1 -90.7(5) 2_566 . . 2_666 ?
N1 N5 N6 Rb1 133.5(2) . . . 1_565 ?
Rb1 N5 N6 Rb1 -79.97(5) 2_566 . . 1_565 ?
N1 N5 N6 Rb1 -146.6(2) . . . 2_566 ?
Rb1 N5 N6 Rb1 79.97(5) 1_565 . . 2_566 ?
N3 N4 C1 N1 0.9(3) . . . . ?
Rb1 N4 C1 N1 -138.2(2) 2_665 . . . ?
N3 N4 C1 C1 -178.3(4) . . . 2_675 ?
Rb1 N4 C1 C1 42.6(5) 2_665 . . 2_675 ?
N2 N1 C1 N4 -1.0(3) . . . . ?
N5 N1 C1 N4 -173.8(3) . . . . ?
N2 N1 C1 C1 178.2(4) . . . 2_675 ?
N5 N1 C1 C1 5.4(6) . . . 2_675 ?
N3 N2 Rb1 O1 -112.5(2) . . . 2_566 ?
N1 N2 Rb1 O1 100.6(2) . . . 2_566 ?
N3 N2 Rb1 O1 98.0(2) . . . 2_666 ?
N1 N2 Rb1 O1 -49.0(2) . . . 2_666 ?
N3 N2 Rb1 O2 -140.2(2) . . . 1_455 ?
N1 N2 Rb1 O2 72.8(2) . . . 1_455 ?
N3 N2 Rb1 O1 58.4(2) . . . 1_545 ?
N1 N2 Rb1 O1 -88.5(2) . . . 1_545 ?
N3 N2 Rb1 N5 8.3(2) . . . 1_545 ?
N1 N2 Rb1 N5 -138.7(2) . . . 1_545 ?
N3 N2 Rb1 N3 -50.1(2) . . . 2_565 ?
N1 N2 Rb1 N3 162.9(2) . . . 2_565 ?
N3 N2 Rb1 O2 139.5(2) . . . 2_666 ?
N1 N2 Rb1 O2 -7.5(2) . . . 2_666 ?
N3 N2 Rb1 N4 33.1(2) . . . 2_665 ?
N1 N2 Rb1 N4 -113.9(2) . . . 2_665 ?
N3 N2 Rb1 N6 118.1(2) . . . 2_666 ?
N1 N2 Rb1 N6 -28.9(2) . . . 2_666 ?
N3 N2 Rb1 N6 35.4(2) . . . 1_545 ?
N1 N2 Rb1 N6 -111.5(2) . . . 1_545 ?
N3 N2 Rb1 N6 -139.61(19) . . . 2_566 ?
N1 N2 Rb1 N6 73.4(2) . . . 2_566 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
? ? ? ? ? ? ? ?

_geom_special_details            ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kx429
_database_code_depnum_ccdc_archive 'CCDC 1500002'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Nov 13 15:13:25 2015'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
disodium 1,1-dinitramino-5,5-bitetrazolate dihydrate
;
_chemical_name_common            
'disodium 1,1-dinitramino-5,5-bitetrazolate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 N12 Na2 O6'
_chemical_formula_sum            'C2 H4 N12 Na2 O6'
_chemical_formula_weight         338.08

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'


_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.
;

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'

_cell_length_a                   8.8347(5)
_cell_length_b                   9.4711(5)
_cell_length_c                   7.2402(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.804(5)
_cell_angle_gamma                90
_cell_volume                     582.92(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1090
_cell_measurement_theta_min      4.7480
_cell_measurement_theta_max      32.4970

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.236
_shelx_estimated_absorpt_T_min   0.937
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98689
_exptl_absorpt_correction_T_max  0.99999
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_F_000             340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            2933
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.304
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1136
_reflns_number_gt                956
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0393P)²+0.0474P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1136
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0812
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0451535000
_diffrn_orient_matrix_UB_12      0.0059706000
_diffrn_orient_matrix_UB_13      0.0669781000
_diffrn_orient_matrix_UB_21      0.0369202000
_diffrn_orient_matrix_UB_22      -0.0614002000
_diffrn_orient_matrix_UB_23      0.0479093000
_diffrn_orient_matrix_UB_31      0.0596990000
_diffrn_orient_matrix_UB_32      0.0424510000
_diffrn_orient_matrix_UB_33      0.0598706000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000    0.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega  -65.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000   80.0000  250.0000 104

;



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'
N N 0.0061 0.0033 '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'
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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.29860(15) 0.62812(13) 0.41067(17) 0.0211(3) Uani 1 1 d . . . . .
O2 O 0.47642(14) 0.63355(13) 0.68561(17) 0.0199(3) Uani 1 1 d . . . . .
N3 N 0.19352(17) 0.29375(15) 0.3840(2) 0.0208(4) Uani 1 1 d . . . . .
N1 N -0.05272(17) 0.35970(15) 0.3172(2) 0.0204(4) Uani 1 1 d . . . . .
N2 N 0.05268(17) 0.26707(17) 0.2786(2) 0.0255(4) Uani 1 1 d . . . . .
N4 N 0.18195(16) 0.40563(15) 0.49365(19) 0.0135(3) Uani 1 1 d . . . . .
N5 N 0.31403(16) 0.45447(14) 0.6329(2) 0.0145(3) Uani 1 1 d . . . . .
N6 N 0.36161(15) 0.57496(14) 0.56991(19) 0.0138(3) Uani 1 1 d . . . . .
C1 C 0.03019(19) 0.44308(17) 0.4530(2) 0.0139(4) Uani 1 1 d . . . . .
Na Na 0.44515(8) 0.15898(7) 0.46386(10) 0.0192(2) Uani 1 1 d . . . . .
O3 O 0.68719(16) 0.04800(14) 0.4726(2) 0.0207(3) Uani 1 1 d . . . . .
H3B H 0.711(3) 0.068(3) 0.361(4) 0.054(8) Uiso 1 1 d . . . . .
H3A H 0.752(4) 0.074(3) 0.559(4) 0.058(9) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N6 1.2422(17) . ?
O1 Na 2.9827(15) 3_666 ?
O2 N6 1.2552(17) . ?
O2 Na 2.4333(13) 3_666 ?
O2 Na 2.4538(13) 2_656 ?
N3 N2 1.295(2) . ?
N3 N4 1.344(2) . ?
N3 Na 2.4911(16) . ?
N1 C1 1.317(2) . ?
N1 N2 1.363(2) . ?
N4 C1 1.340(2) . ?
N4 N5 1.3967(18) . ?
N5 N6 1.338(2) . ?
N5 Na 2.5937(16) 4_566 ?
C1 C1 1.452(3) 3_566 ?
Na O3 2.3681(15) . ?
O3 H3B 0.91(3) . ?
O3 H3A 0.76(3) . ?

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
_geom_angle_publ_flag
N6 O1 Na 83.12(9) . 3_666 ?
N6 O2 Na 109.66(10) . 3_666 ?
N6 O2 Na 133.07(10) . 2_656 ?
Na O2 Na 110.26(5) 3_666 2_656 ?
N2 N3 N4 106.63(13) . . ?
N2 N3 Na 133.65(11) . . ?
N4 N3 Na 118.25(10) . . ?
C1 N1 N2 105.48(14) . . ?
N3 N2 N1 110.75(13) . . ?
C1 N4 N3 108.13(13) . . ?
C1 N4 N5 131.32(14) . . ?
N3 N4 N5 120.28(13) . . ?
N6 N5 N4 108.35(12) . . ?
N6 N5 Na 124.42(10) . 4_566 ?
N4 N5 Na 127.21(10) . 4_566 ?
O1 N6 O2 121.11(14) . . ?
O1 N6 N5 123.97(14) . . ?
O2 N6 N5 114.92(13) . . ?
N1 C1 N4 108.98(14) . . ?
N1 C1 C1 126.49(19) . 3_566 ?
N4 C1 C1 124.52(19) . 3_566 ?
O3 Na O3 96.68(5) . 3_656 ?
O3 Na O2 90.33(5) . 3_666 ?
O3 Na O2 164.00(5) 3_656 3_666 ?
O3 Na O2 86.00(5) . 2_646 ?
O3 Na O2 74.67(5) 3_656 2_646 ?
O2 Na O2 120.32(5) 3_666 2_646 ?
O3 Na N3 167.40(6) . . ?
O3 Na N3 90.72(5) 3_656 . ?
O2 Na N3 80.05(5) 3_666 . ?
O2 Na N3 105.85(5) 2_646 . ?
O3 Na N5 90.78(5) . 4_565 ?
O3 Na N5 73.70(5) 3_656 4_565 ?
O2 Na N5 91.91(5) 3_666 4_565 ?
O2 Na N5 147.59(5) 2_646 4_565 ?
N3 Na N5 81.49(5) . 4_565 ?
O3 Na O1 71.76(4) . 3_666 ?
O3 Na O1 150.02(5) 3_656 3_666 ?
O2 Na O1 45.98(4) 3_666 3_666 ?
O2 Na O1 76.95(4) 2_646 3_666 ?
N3 Na O1 106.24(5) . 3_666 ?
N5 Na O1 132.25(5) 4_565 3_666 ?
O3 Na Na 48.64(4) . 3_656 ?
O3 Na Na 48.04(4) 3_656 3_656 ?
O2 Na Na 136.96(4) 3_666 3_656 ?
O2 Na Na 75.40(4) 2_646 3_656 ?
N3 Na Na 137.74(5) . 3_656 ?
N5 Na Na 78.35(4) 4_565 3_656 ?
O1 Na Na 114.85(4) 3_666 3_656 ?
O3 Na Na 89.59(4) . 4_565 ?
O3 Na Na 130.29(4) 3_656 4_565 ?
O2 Na Na 35.04(3) 3_666 4_565 ?
O2 Na Na 155.03(4) 2_646 4_565 ?
N3 Na Na 77.85(4) . 4_565 ?
N5 Na Na 56.89(3) 4_565 4_565 ?
O1 Na Na 78.32(3) 3_666 4_565 ?
Na Na Na 118.91(3) 3_656 4_565 ?
O3 Na Na 112.88(4) . 4_566 ?
O3 Na Na 93.36(4) 3_656 4_566 ?
O2 Na Na 97.14(4) 3_666 4_566 ?
O2 Na Na 34.70(3) 2_646 4_566 ?
N3 Na Na 76.69(4) . 4_566 ?
N5 Na Na 154.49(3) 4_565 4_566 ?
O1 Na Na 67.73(3) 3_666 4_566 ?
Na Na Na 109.60(3) 3_656 4_566 ?
Na Na Na 129.06(3) 4_565 4_566 ?
Na O3 Na 83.32(5) . 3_656 ?
Na O3 H3B 108.0(16) . . ?
Na O3 H3B 126.2(16) 3_656 . ?
Na O3 H3A 110(2) . . ?
Na O3 H3A 114(2) 3_656 . ?
H3B O3 H3A 111(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 N3 N2 N1 -0.2(2) . . . . ?
Na N3 N2 N1 165.26(12) . . . . ?
C1 N1 N2 N3 -0.8(2) . . . . ?
N2 N3 N4 C1 1.07(19) . . . . ?
Na N3 N4 C1 -167.01(10) . . . . ?
N2 N3 N4 N5 175.81(14) . . . . ?
Na N3 N4 N5 7.73(18) . . . . ?
C1 N4 N5 N6 -80.3(2) . . . . ?
N3 N4 N5 N6 106.35(16) . . . . ?
C1 N4 N5 Na 97.87(19) . . . 4_566 ?
N3 N4 N5 Na -75.47(17) . . . 4_566 ?
Na O1 N6 O2 3.36(13) 3_666 . . . ?
Na O1 N6 N5 -177.29(14) 3_666 . . . ?
Na O2 N6 O1 -4.35(17) 3_666 . . . ?
Na O2 N6 O1 142.51(12) 2_656 . . . ?
Na O2 N6 N5 176.25(10) 3_666 . . . ?
Na O2 N6 N5 -36.9(2) 2_656 . . . ?
N4 N5 N6 O1 -2.2(2) . . . . ?
Na N5 N6 O1 179.59(11) 4_566 . . . ?
N4 N5 N6 O2 177.21(13) . . . . ?
Na N5 N6 O2 -1.03(18) 4_566 . . . ?
N2 N1 C1 N4 1.44(19) . . . . ?
N2 N1 C1 C1 -178.0(2) . . . 3_566 ?
N3 N4 C1 N1 -1.60(19) . . . . ?
N5 N4 C1 N1 -175.55(15) . . . . ?
N3 N4 C1 C1 177.85(19) . . . 3_566 ?
N5 N4 C1 C1 3.9(3) . . . 3_566 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
O3 H3B O1 0.91(3) 2.03(3) 2.9122(19) 164(2) 2_645
O3 H3A N1 0.76(3) 2.26(3) 3.024(2) 177(3) 4_666

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.265
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx381
_database_code_depnum_ccdc_archive 'CCDC 1500003'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Aug 12 16:56:28 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
disodium 1,1-dinitramino-5,5-bitetrazolate dihydrate
;
_chemical_name_common            
'disodium 1,1-dinitramino-5,5-bitetrazolate dihydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 N12 Na2 O6'
_chemical_formula_sum            'C2 H4 N12 Na2 O6'
_chemical_formula_weight         338.15

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.2136(3)
_cell_length_b                   10.9858(6)
_cell_length_c                   16.9609(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1157.77(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3554
_cell_measurement_theta_min      4.8110
_cell_measurement_theta_max      31.7390

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.449
_exptl_crystal_size_min          0.292
_exptl_absorpt_coefficient_mu    0.238
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88041
_exptl_absorpt_correction_T_max  0.99999
_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_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            8554
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.421
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1132
_reflns_number_gt                1059
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²+0.4644P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1132
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0845984000
_diffrn_orient_matrix_UB_12      0.0206981000
_diffrn_orient_matrix_UB_13      -0.0247017000
_diffrn_orient_matrix_UB_21      -0.0442115000
_diffrn_orient_matrix_UB_22      -0.0595286000
_diffrn_orient_matrix_UB_23      -0.0005657000
_diffrn_orient_matrix_UB_31      -0.0626697000
_diffrn_orient_matrix_UB_32      0.0141165000
_diffrn_orient_matrix_UB_33      0.0337070000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -10.00   96.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000    0.0000 106

#__ type_ start__ end____ width___ exp.time_
  2 omega   26.00   68.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   30.0000 42

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   12.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
  4 omega   38.00   75.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
  5 omega  -41.00   17.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
  6 omega   42.00   68.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   57.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  -99.00  -12.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000 -150.0000 87

#__ type_ start__ end____ width___ exp.time_
  8 omega -109.00  -39.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994 -179.0000 -150.0000 70

#__ type_ start__ end____ width___ exp.time_
  9 omega -101.00  -70.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000   30.0000 31

;



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'
N N 0.0061 0.0033 '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'
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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.09832(17) 0.50252(9) 0.24700(6) 0.0200(3) Uani 1 1 d . . . . .
O2 O 0.23669(17) 0.58480(9) 0.14164(6) 0.0217(3) Uani 1 1 d . . . . .
N4 N 0.2033(2) 0.42803(12) -0.06387(7) 0.0230(3) Uani 1 1 d . . . . .
N3 N 0.3566(2) 0.34937(12) -0.03762(7) 0.0244(3) Uani 1 1 d . . . . .
N2 N 0.3410(2) 0.33203(12) 0.03769(7) 0.0227(3) Uani 1 1 d . . . . .
N1 N 0.17421(19) 0.40037(11) 0.06181(7) 0.0179(3) Uani 1 1 d . . . . .
N5 N 0.1041(2) 0.39279(11) 0.14005(6) 0.0181(3) Uani 1 1 d . . . . .
N6 N 0.15016(18) 0.49670(10) 0.17592(7) 0.0155(3) Uani 1 1 d . . . . .
C1 C 0.0918(2) 0.45886(13) -0.00113(8) 0.0186(3) Uani 1 1 d . . . . .
O3 O 0.60067(17) 0.26624(11) 0.19497(6) 0.0205(3) Uani 1 1 d . . . . .
Na Na 0.45049(9) 0.18977(5) 0.31503(3) 0.01886(19) Uani 1 1 d . . . . .
H1A H 0.596(3) 0.338(2) 0.2016(11) 0.030(5) Uiso 1 1 d . . . . .
H1B H 0.526(3) 0.2556(19) 0.1567(12) 0.033(5) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N6 1.2495(15) . ?
O1 Na 2.3781(11) 7_665 ?
O2 N6 1.2505(15) . ?
O2 Na 2.3765(11) 4_655 ?
N4 C1 1.3145(19) . ?
N4 N3 1.3608(18) . ?
N4 Na 2.8726(13) 8_565 ?
N3 N2 1.2952(18) . ?
N3 Na 2.6020(13) 8_565 ?
N2 N1 1.3435(17) . ?
N1 C1 1.3471(18) . ?
N1 N5 1.3991(16) . ?
N5 N6 1.3249(16) . ?
O3 Na 2.3923(12) . ?
O3 H1A 0.79(2) . ?
O3 H1B 0.81(2) . ?
Na H1A 2.67(2) . ?

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
_geom_angle_publ_flag
N6 O1 Na 123.05(8) . 7_665 ?
N6 O2 Na 125.69(8) . 4_655 ?
C1 N4 N3 105.54(12) . . ?
C1 N4 Na 167.66(10) . 8_565 ?
N3 N4 Na 64.77(7) . 8_565 ?
N2 N3 N4 111.32(12) . . ?
N2 N3 Na 160.01(10) . 8_565 ?
N4 N3 Na 87.00(8) . 8_565 ?
N3 N2 N1 106.01(12) . . ?
N2 N1 C1 108.58(12) . . ?
N2 N1 N5 119.71(11) . . ?
C1 N1 N5 131.42(12) . . ?
N6 N5 N1 108.48(11) . . ?
N6 N5 Na 134.36(9) . 6_556 ?
N1 N5 Na 116.96(8) . 6_556 ?
O1 N6 O2 121.32(11) . . ?
O1 N6 N5 115.57(11) . . ?
O2 N6 N5 123.11(12) . . ?
N4 C1 N1 108.54(13) . . ?
N4 C1 C1 126.48(16) . 5_565 ?
N1 C1 C1 124.98(15) . 5_565 ?
Na O3 Na 107.36(5) 6_656 . ?
Na O3 H1A 113.8(14) 6_656 . ?
Na O3 H1A 102.1(14) . . ?
Na O3 H1B 115.0(14) 6_656 . ?
Na O3 H1B 114.3(14) . . ?
H1A O3 H1B 104(2) . . ?
O3 Na O2 163.29(5) 6_556 4_645 ?
O3 Na O1 99.04(4) 6_556 7_655 ?
O2 Na O1 80.48(4) 4_645 7_655 ?
O3 Na O3 100.07(4) 6_556 . ?
O2 Na O3 96.58(4) 4_645 . ?
O1 Na O3 86.59(4) 7_655 . ?
O3 Na N5 93.19(4) 6_556 6_656 ?
O2 Na N5 91.49(4) 4_645 6_656 ?
O1 Na N5 162.18(4) 7_655 6_656 ?
O3 Na N5 78.50(4) . 6_656 ?
O3 Na N3 85.44(4) 6_556 8_566 ?
O2 Na N3 78.82(4) 4_645 8_566 ?
O1 Na N3 107.12(4) 7_655 8_566 ?
O3 Na N3 164.36(5) . 8_566 ?
N5 Na N3 86.63(4) 6_656 8_566 ?
O3 Na N4 73.53(4) 6_556 8_566 ?
O2 Na N4 89.86(4) 4_645 8_566 ?
O1 Na N4 83.63(4) 7_655 8_566 ?
O3 Na N4 167.25(4) . 8_566 ?
N5 Na N4 112.43(4) 6_656 8_566 ?
N3 Na N4 28.23(4) 8_566 8_566 ?
O3 Na Na 36.82(3) 6_556 6_556 ?
O2 Na Na 147.77(3) 4_645 6_556 ?
O1 Na Na 67.36(3) 7_655 6_556 ?
O3 Na Na 79.94(3) . 6_556 ?
N5 Na Na 118.66(3) 6_656 6_556 ?
N3 Na Na 111.92(3) 8_566 6_556 ?
N4 Na Na 88.74(3) 8_566 6_556 ?
O3 Na Na 135.77(4) 6_556 6_656 ?
O2 Na Na 60.80(3) 4_645 6_656 ?
O1 Na Na 79.81(3) 7_655 6_656 ?
O3 Na Na 35.82(3) . 6_656 ?
N5 Na Na 82.38(3) 6_656 6_656 ?
N3 Na Na 137.63(3) 8_566 6_656 ?
N4 Na Na 148.20(3) 8_566 6_656 ?
Na Na Na 109.25(3) 6_556 6_656 ?
O3 Na H1A 92.5(4) 6_556 . ?
O2 Na H1A 104.0(4) 4_645 . ?
O1 Na H1A 102.7(5) 7_655 . ?
O3 Na H1A 16.8(5) . . ?
N5 Na H1A 63.7(5) 6_656 . ?
N3 Na H1A 150.1(5) 8_566 . ?
N4 Na H1A 165.5(4) 8_566 . ?
Na Na H1A 81.9(4) 6_556 . ?
Na Na H1A 46.2(4) 6_656 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.07(17) . . . . ?
Na N4 N3 N2 -171.78(13) 8_565 . . . ?
C1 N4 N3 Na 171.85(10) . . . 8_565 ?
N4 N3 N2 N1 0.05(16) . . . . ?
Na N3 N2 N1 -155.3(3) 8_565 . . . ?
N3 N2 N1 C1 -0.15(15) . . . . ?
N3 N2 N1 N5 174.35(12) . . . . ?
N2 N1 N5 N6 111.18(13) . . . . ?
C1 N1 N5 N6 -75.78(18) . . . . ?
N2 N1 N5 Na -64.44(14) . . . 6_556 ?
C1 N1 N5 Na 108.59(15) . . . 6_556 ?
Na O1 N6 O2 20.09(17) 7_665 . . . ?
Na O1 N6 N5 -158.87(9) 7_665 . . . ?
Na O2 N6 O1 53.20(16) 4_655 . . . ?
Na O2 N6 N5 -127.92(11) 4_655 . . . ?
N1 N5 N6 O1 -179.27(11) . . . . ?
Na N5 N6 O1 -4.73(18) 6_556 . . . ?
N1 N5 N6 O2 1.79(17) . . . . ?
Na N5 N6 O2 176.33(10) 6_556 . . . ?
N3 N4 C1 N1 -0.16(16) . . . . ?
Na N4 C1 N1 36.8(5) 8_565 . . . ?
N3 N4 C1 C1 -179.58(19) . . . 5_565 ?
Na N4 C1 C1 -142.7(4) 8_565 . . 5_565 ?
N2 N1 C1 N4 0.19(16) . . . . ?
N5 N1 C1 N4 -173.43(13) . . . . ?
N2 N1 C1 C1 179.63(17) . . . 5_565 ?
N5 N1 C1 C1 6.0(3) . . . 5_565 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
O3 H1A O1 0.79(2) 2.01(2) 2.7761(16) 162.3(19) 6_656
O3 H1B O2 0.81(2) 2.50(2) 3.0307(16) 124.5(18) 7_655
O3 H1B N2 0.81(2) 2.47(2) 3.2002(16) 151.2(19) .
O3 H1A O1 0.79(2) 2.01(2) 2.7761(16) 162.3(19) 6_656
O3 H1B O2 0.81(2) 2.50(2) 3.0307(16) 124.5(18) 7_655
O3 H1B N2 0.81(2) 2.47(2) 3.2002(16) 151.2(19) .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.369
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.047

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_uv608
_database_code_depnum_ccdc_archive 'CCDC 1524647'
_audit_update_record             
;
2016-12-27 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             ?
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
strontium 1,1-dinitramino-bitetrazolate tetrahydrate
;
_chemical_name_common            
'strontium 1,1-dinitramino-bitetrazolate tetrahydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H8 N12 O8 Sr'
_chemical_formula_sum            'C2 H8 N12 O8 Sr'
_chemical_formula_weight         415.82

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'




_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.
;

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'

_cell_length_a                   10.7948(3)
_cell_length_b                   15.0619(4)
_cell_length_c                   9.3539(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.3330(10)
_cell_angle_gamma                90
_cell_volume                     1426.09(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9870
_cell_measurement_theta_min      2.6873
_cell_measurement_theta_max      28.2857

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    3.849
_shelx_estimated_absorpt_T_min   0.699
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            23112
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.833
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3271
_reflns_number_gt                2910
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0192P)²+1.2394P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3271
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0501
_refine_ls_wR_factor_gt          0.0482
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N -0.11858(15) 0.08312(10) 0.47700(18) 0.0170(3) Uani 1 1 d . . . . .
N10 N -0.14291(14) 0.36219(10) 0.36576(17) 0.0147(3) Uani 1 1 d . . . . .
N8 N -0.32888(15) 0.43458(10) 0.31896(18) 0.0165(3) Uani 1 1 d . . . . .
N7 N -0.34865(14) 0.34864(10) 0.34247(16) 0.0131(3) Uani 1 1 d . . . . .
C2 C -0.23312(16) 0.30518(12) 0.37243(18) 0.0122(3) Uani 1 1 d . . . . .
N11 N -0.47360(13) 0.31681(10) 0.32601(16) 0.0129(3) Uani 1 1 d . . . . .
N9 N -0.20560(15) 0.44183(10) 0.33276(18) 0.0169(3) Uani 1 1 d . . . . .
O7 O 0.41649(13) 0.37736(10) 0.76213(16) 0.0150(3) Uani 1 1 d . . . . .
O8 O 0.14421(13) 0.38146(9) 0.52073(15) 0.0154(3) Uani 1 1 d . . . . .
O4 O -0.59669(12) 0.27878(8) 0.45402(14) 0.0149(3) Uani 1 1 d . . . . .
O5 O 0.34174(16) 0.09719(10) 0.52072(17) 0.0227(3) Uani 1 1 d . . . . .
O6 O 0.20422(16) 0.08995(10) 0.74765(18) 0.0240(3) Uani 1 1 d . . . . .
O3 O -0.39409(13) 0.32094(10) 0.58494(14) 0.0232(3) Uani 1 1 d . . . . .
N12 N -0.48350(14) 0.30669(10) 0.46322(16) 0.0131(3) Uani 1 1 d . . . . .
Sr1 Sr 0.27802(2) 0.23281(2) 0.63909(2) 0.01015(5) Uani 1 1 d . . . . .
O2 O 0.14605(12) 0.22612(9) 0.31926(14) 0.0168(3) Uani 1 1 d . . . . .
N6 N 0.03369(14) 0.20047(10) 0.31510(16) 0.0134(3) Uani 1 1 d . . . . .
O1 O -0.05734(13) 0.18248(10) 0.19660(14) 0.0242(3) Uani 1 1 d . . . . .
N1 N -0.09969(14) 0.16743(10) 0.44286(16) 0.0119(3) Uani 1 1 d . . . . .
N3 N -0.24152(15) 0.07805(10) 0.46673(18) 0.0169(3) Uani 1 1 d . . . . .
N4 N -0.30409(14) 0.15694(10) 0.42616(17) 0.0143(3) Uani 1 1 d . . . . .
N5 N 0.02497(13) 0.19676(10) 0.45377(16) 0.0131(3) Uani 1 1 d . . . . .
C1 C -0.21439(16) 0.21202(12) 0.41183(19) 0.0122(3) Uani 1 1 d . . . . .
H5A H 0.317(3) 0.0485(19) 0.520(3) 0.037(8) Uiso 1 1 d . . . . .
H8A H 0.147(3) 0.4249(19) 0.577(3) 0.036(7) Uiso 1 1 d . . . . .
H7A H 0.416(2) 0.4231(18) 0.725(3) 0.029(7) Uiso 1 1 d . . . . .
H6A H 0.147(3) 0.057(2) 0.697(4) 0.064(11) Uiso 1 1 d . . . . .
H5B H 0.366(3) 0.1025(18) 0.445(3) 0.041(8) Uiso 1 1 d . . . . .
H6B H 0.186(3) 0.0951(19) 0.830(3) 0.043(8) Uiso 1 1 d . . . . .
H8B H 0.065(3) 0.3702(18) 0.489(3) 0.035(7) Uiso 1 1 d . . . . .
H7B H 0.493(3) 0.368(2) 0.797(3) 0.049(9) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 N3 1.299(2) . ?
N2 N1 1.342(2) . ?
N10 C2 1.316(2) . ?
N10 N9 1.359(2) . ?
N8 N9 1.296(2) . ?
N8 N7 1.342(2) . ?
N7 C2 1.349(2) . ?
N7 N11 1.3887(19) . ?
C2 C1 1.447(3) . ?
N11 N12 1.3331(19) . ?
O7 Sr1 2.6652(14) . ?
O7 H7A 0.77(3) . ?
O7 H7B 0.79(3) . ?
O8 Sr1 2.6858(13) . ?
O8 H8A 0.84(3) . ?
O8 H8B 0.82(3) . ?
O4 N12 1.2665(18) . ?
O5 Sr1 2.5300(14) . ?
O5 H5A 0.78(3) . ?
O5 H5B 0.83(3) . ?
O6 Sr1 2.6188(15) . ?
O6 H6A 0.80(4) . ?
O6 H6B 0.86(3) . ?
O3 N12 1.2289(19) . ?
Sr1 N5 2.7333(14) . ?
Sr1 O2 2.8334(13) . ?
Sr1 N12 3.2786(14) 4_666 ?
Sr1 N6 3.2899(14) . ?
O2 N6 1.2607(18) . ?
O2 Sr1 2.6306(12) 4_565 ?
N6 O1 1.2291(19) . ?
N6 N5 1.3339(19) . ?
N1 C1 1.349(2) . ?
N1 N5 1.3859(19) . ?
N3 N4 1.354(2) . ?
N4 C1 1.317(2) . ?

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
_geom_angle_publ_flag
N3 N2 N1 105.89(14) . . ?
C2 N10 N9 105.57(14) . . ?
N9 N8 N7 106.33(14) . . ?
N8 N7 C2 108.29(14) . . ?
N8 N7 N11 121.22(14) . . ?
C2 N7 N11 130.37(15) . . ?
N10 C2 N7 108.63(16) . . ?
N10 C2 C1 127.20(16) . . ?
N7 C2 C1 124.11(15) . . ?
N12 N11 N7 109.42(13) . . ?
N12 N11 Sr1 101.22(9) . 4_465 ?
N7 N11 Sr1 149.32(10) . 4_465 ?
N8 N9 N10 111.17(14) . . ?
Sr1 O7 H7A 128.4(19) . . ?
Sr1 O7 H7B 113(2) . . ?
H7A O7 H7B 101(3) . . ?
Sr1 O8 H8A 119.6(18) . . ?
Sr1 O8 H8B 108.7(19) . . ?
H8A O8 H8B 101(2) . . ?
N12 O4 Sr1 138.29(10) . 1_455 ?
N12 O4 Sr1 101.24(9) . 4_465 ?
Sr1 O4 Sr1 120.46(4) 1_455 4_465 ?
Sr1 O5 H5A 128(2) . . ?
Sr1 O5 H5B 120.3(19) . . ?
H5A O5 H5B 107(3) . . ?
Sr1 O6 H6A 123(2) . . ?
Sr1 O6 H6B 117.8(19) . . ?
H6A O6 H6B 103(3) . . ?
O3 N12 O4 123.33(14) . . ?
O3 N12 N11 124.89(14) . . ?
O4 N12 N11 111.76(13) . . ?
O3 N12 Sr1 179.60(12) . 4_465 ?
O4 N12 Sr1 56.49(8) . 4_465 ?
N11 N12 Sr1 55.28(8) . 4_465 ?
O5 Sr1 O6 70.85(5) . . ?
O5 Sr1 O2 139.49(5) . 4_566 ?
O6 Sr1 O2 68.86(4) . 4_566 ?
O5 Sr1 O4 69.19(4) . 1_655 ?
O6 Sr1 O4 139.99(4) . 1_655 ?
O2 Sr1 O4 151.11(4) 4_566 1_655 ?
O5 Sr1 O7 130.66(5) . . ?
O6 Sr1 O7 134.77(5) . . ?
O2 Sr1 O7 83.03(4) 4_566 . ?
O4 Sr1 O7 74.33(4) 1_655 . ?
O5 Sr1 O8 132.97(5) . . ?
O6 Sr1 O8 130.72(5) . . ?
O2 Sr1 O8 74.62(4) 4_566 . ?
O4 Sr1 O8 80.52(4) 1_655 . ?
O7 Sr1 O8 68.75(4) . . ?
O5 Sr1 N5 85.75(5) . . ?
O6 Sr1 N5 73.20(5) . . ?
O2 Sr1 N5 78.97(4) 4_566 . ?
O4 Sr1 N5 105.29(4) 1_655 . ?
O7 Sr1 N5 136.31(5) . . ?
O8 Sr1 N5 68.18(4) . . ?
O5 Sr1 N11 72.86(5) . 4_666 ?
O6 Sr1 N11 83.73(5) . 4_666 ?
O2 Sr1 N11 106.40(4) 4_566 4_666 ?
O4 Sr1 N11 83.06(4) 1_655 4_666 ?
O7 Sr1 N11 70.76(4) . 4_666 ?
O8 Sr1 N11 139.05(4) . 4_666 ?
N5 Sr1 N11 152.74(5) . 4_666 ?
O5 Sr1 O4 107.83(4) . 4_666 ?
O6 Sr1 O4 68.90(4) . 4_666 ?
O2 Sr1 O4 60.63(4) 4_566 4_666 ?
O4 Sr1 O4 122.68(4) 1_655 4_666 ?
O7 Sr1 O4 66.51(4) . 4_666 ?
O8 Sr1 O4 118.81(4) . 4_666 ?
N5 Sr1 O4 131.98(4) . 4_666 ?
N11 Sr1 O4 45.77(4) 4_666 4_666 ?
O5 Sr1 O2 67.83(4) . . ?
O6 Sr1 O2 105.73(4) . . ?
O2 Sr1 O2 119.95(4) 4_566 . ?
O4 Sr1 O2 59.99(4) 1_655 . ?
O7 Sr1 O2 119.06(4) . . ?
O8 Sr1 O2 66.00(4) . . ?
N5 Sr1 O2 45.44(4) . . ?
N11 Sr1 O2 133.14(4) 4_666 . ?
O4 Sr1 O2 174.28(4) 4_666 . ?
O5 Sr1 N12 90.73(4) . 4_666 ?
O6 Sr1 N12 74.88(4) . 4_666 ?
O2 Sr1 N12 82.89(4) 4_566 4_666 ?
O4 Sr1 N12 103.77(4) 1_655 4_666 ?
O7 Sr1 N12 66.83(4) . 4_666 ?
O8 Sr1 N12 132.03(4) . 4_666 ?
N5 Sr1 N12 147.24(4) . 4_666 ?
N11 Sr1 N12 23.51(4) 4_666 4_666 ?
O4 Sr1 N12 22.26(3) 4_666 4_666 ?
O2 Sr1 N12 156.22(4) . 4_666 ?
O5 Sr1 N6 74.35(4) . . ?
O6 Sr1 N6 88.91(5) . . ?
O2 Sr1 N6 100.70(4) 4_566 . ?
O4 Sr1 N6 82.17(4) 1_655 . ?
O7 Sr1 N6 131.95(4) . . ?
O8 Sr1 N6 66.39(4) . . ?
N5 Sr1 N6 23.32(4) . . ?
N11 Sr1 N6 147.01(4) 4_666 . ?
O4 Sr1 N6 154.64(4) 4_666 . ?
O2 Sr1 N6 22.19(3) . . ?
N12 Sr1 N6 161.01(4) 4_666 . ?
N6 O2 Sr1 141.42(10) . 4_565 ?
N6 O2 Sr1 99.72(9) . . ?
Sr1 O2 Sr1 118.85(4) 4_565 . ?
O1 N6 O2 123.68(14) . . ?
O1 N6 N5 124.28(14) . . ?
O2 N6 N5 112.03(13) . . ?
O1 N6 Sr1 175.71(12) . . ?
O2 N6 Sr1 58.09(8) . . ?
N5 N6 Sr1 54.22(8) . . ?
N2 N1 C1 108.56(14) . . ?
N2 N1 N5 120.53(14) . . ?
C1 N1 N5 130.72(15) . . ?
N2 N3 N4 111.50(14) . . ?
C1 N4 N3 105.58(14) . . ?
N6 N5 N1 109.66(13) . . ?
N6 N5 Sr1 102.46(9) . . ?
N1 N5 Sr1 147.23(10) . . ?
N4 C1 N1 108.47(15) . . ?
N4 C1 C2 126.46(15) . . ?
N1 C1 C2 125.06(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N9 N8 N7 C2 0.71(19) . . . . ?
N9 N8 N7 N11 -175.73(14) . . . . ?
N9 N10 C2 N7 0.70(19) . . . . ?
N9 N10 C2 C1 -176.61(16) . . . . ?
N8 N7 C2 N10 -0.90(19) . . . . ?
N11 N7 C2 N10 175.11(15) . . . . ?
N8 N7 C2 C1 176.51(15) . . . . ?
N11 N7 C2 C1 -7.5(3) . . . . ?
N8 N7 N11 N12 -101.88(17) . . . . ?
C2 N7 N11 N12 82.5(2) . . . . ?
N8 N7 N11 Sr1 75.1(3) . . . 4_465 ?
C2 N7 N11 Sr1 -100.5(2) . . . 4_465 ?
N7 N8 N9 N10 -0.28(19) . . . . ?
C2 N10 N9 N8 -0.26(19) . . . . ?
Sr1 O4 N12 O3 -0.8(3) 1_455 . . . ?
Sr1 O4 N12 O3 -179.57(14) 4_465 . . . ?
Sr1 O4 N12 N11 178.04(11) 1_455 . . . ?
Sr1 O4 N12 N11 -0.70(15) 4_465 . . . ?
Sr1 O4 N12 Sr1 178.75(17) 1_455 . . 4_465 ?
N7 N11 N12 O3 -2.0(2) . . . . ?
Sr1 N11 N12 O3 179.56(15) 4_465 . . . ?
N7 N11 N12 O4 179.15(13) . . . . ?
Sr1 N11 N12 O4 0.71(15) 4_465 . . . ?
N7 N11 N12 Sr1 178.44(15) . . . 4_465 ?
Sr1 O2 N6 O1 3.2(3) 4_565 . . . ?
Sr1 O2 N6 O1 -175.35(15) . . . . ?
Sr1 O2 N6 N5 -175.68(12) 4_565 . . . ?
Sr1 O2 N6 N5 5.73(15) . . . . ?
Sr1 O2 N6 Sr1 178.58(19) 4_565 . . . ?
N3 N2 N1 C1 -0.14(19) . . . . ?
N3 N2 N1 N5 175.45(14) . . . . ?
N1 N2 N3 N4 0.20(19) . . . . ?
N2 N3 N4 C1 -0.2(2) . . . . ?
O1 N6 N5 N1 1.7(2) . . . . ?
O2 N6 N5 N1 -179.41(14) . . . . ?
Sr1 N6 N5 N1 -173.40(16) . . . . ?
O1 N6 N5 Sr1 175.09(15) . . . . ?
O2 N6 N5 Sr1 -6.00(16) . . . . ?
N2 N1 N5 N6 101.96(18) . . . . ?
C1 N1 N5 N6 -83.6(2) . . . . ?
N2 N1 N5 Sr1 -66.1(3) . . . . ?
C1 N1 N5 Sr1 108.4(2) . . . . ?
N3 N4 C1 N1 0.09(19) . . . . ?
N3 N4 C1 C2 -178.83(16) . . . . ?
N2 N1 C1 N4 0.03(19) . . . . ?
N5 N1 C1 N4 -174.96(15) . . . . ?
N2 N1 C1 C2 178.97(16) . . . . ?
N5 N1 C1 C2 4.0(3) . . . . ?
N10 C2 C1 N4 175.99(17) . . . . ?
N7 C2 C1 N4 -0.9(3) . . . . ?
N10 C2 C1 N1 -2.8(3) . . . . ?
N7 C2 C1 N1 -179.68(16) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
O5 H5A N3 0.78(3) 2.09(3) 2.870(2) 174(3) 3_556
O8 H8A N9 0.84(3) 2.18(3) 2.962(2) 155(2) 3_566
O7 H7A N8 0.77(3) 2.32(3) 2.999(2) 148(2) 3_566
O6 H6A N2 0.80(4) 2.62(4) 3.273(2) 140(3) 3_556
O5 H5B O7 0.83(3) 2.00(3) 2.829(2) 176(3) 4_565
O6 H6B O8 0.86(3) 2.02(3) 2.877(2) 175(3) 4_566
O8 H8B N10 0.82(3) 2.14(3) 2.944(2) 167(3) .
O7 H7B N4 0.79(3) 2.13(3) 2.916(2) 171(3) 4_666
O5 H5A N3 0.78(3) 2.09(3) 2.870(2) 174(3) 3_556
O8 H8A N9 0.84(3) 2.18(3) 2.962(2) 155(2) 3_566
O7 H7A N8 0.77(3) 2.32(3) 2.999(2) 148(2) 3_566
O6 H6A N2 0.80(4) 2.62(4) 3.273(2) 140(3) 3_556
O5 H5B O7 0.83(3) 2.00(3) 2.829(2) 176(3) 4_565
O6 H6B O8 0.86(3) 2.02(3) 2.877(2) 175(3) 4_566
O8 H8B N10 0.82(3) 2.14(3) 2.944(2) 167(3) .
O7 H7B N4 0.79(3) 2.13(3) 2.916(2) 171(3) 4_666

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.860
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.062

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx412
_database_code_depnum_ccdc_archive 'CCDC 1510459'
_audit_update_record             
;
2016-10-18 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Sep 08 08:00:33 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetrammine zinc(II) 1,1-dinitramino-5,5-bitetrazolate
;
_chemical_name_common            
'tetrammine zinc(II) 1,1-dinitramino-5,5-bitetrazolate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' 	C2 N12 O4, H12 N4 Zn'
_chemical_formula_sum            'C2 H12 N16 O4 Zn'
_chemical_formula_weight         389.65

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.2414(3)
_cell_length_b                   10.6483(3)
_cell_length_c                   13.1297(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.149(3)
_cell_angle_gamma                90
_cell_volume                     1428.09(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3837
_cell_measurement_theta_min      4.4010
_cell_measurement_theta_max      31.6790

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.774
_shelx_estimated_absorpt_T_min   0.718
_shelx_estimated_absorpt_T_max   0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94019
_exptl_absorpt_correction_T_max  0.99999
_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_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            10947
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.132
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2785
_reflns_number_gt                2310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0318P)²+0.7186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2785
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0675
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0211918000
_diffrn_orient_matrix_UB_12      -0.0580099000
_diffrn_orient_matrix_UB_13      0.0195753000
_diffrn_orient_matrix_UB_21      -0.0566496000
_diffrn_orient_matrix_UB_22      0.0020480000
_diffrn_orient_matrix_UB_23      -0.0344175000
_diffrn_orient_matrix_UB_31      0.0341044000
_diffrn_orient_matrix_UB_32      -0.0326462000
_diffrn_orient_matrix_UB_33      -0.0369845000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   43.00  111.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000  -90.0000 68

#__ type_ start__ end____ width___ exp.time_
  2 omega  -21.00   74.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -30.0000 95

#__ type_ start__ end____ width___ exp.time_
  3 omega   71.00  112.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932 -179.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00  102.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000 -120.0000 103

#__ type_ start__ end____ width___ exp.time_
  5 omega  -31.00   24.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -77.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
  6 omega  -27.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -19.0000  -60.0000 110

;



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'
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'
Zn Zn 0.2839 1.4301 '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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.37487(14) 0.24889(13) -0.04288(11) 0.0237(3) Uani 1 1 d . . . . .
O2 O 0.19270(15) 0.21657(15) -0.13650(12) 0.0290(4) Uani 1 1 d . . . . .
N1 N 0.34718(16) 0.05091(16) 0.05497(13) 0.0174(4) Uani 1 1 d . . . . .
N2 N 0.32261(18) 0.05451(17) 0.15470(14) 0.0228(4) Uani 1 1 d . . . . .
N3 N 0.42927(19) 0.01578(17) 0.20478(14) 0.0256(4) Uani 1 1 d . . . . .
N4 N 0.52316(18) -0.01301(17) 0.14066(14) 0.0226(4) Uani 1 1 d . . . . .
N5 N 0.24790(16) 0.07720(16) -0.01996(14) 0.0205(4) Uani 1 1 d . . . . .
N6 N 0.27549(16) 0.18512(16) -0.06624(13) 0.0200(4) Uani 1 1 d . . . . .
C1 C 0.46971(19) 0.00877(18) 0.04753(16) 0.0175(4) Uani 1 1 d . . . . .
O3 O 0.37142(16) 0.26353(16) 0.44820(13) 0.0362(4) Uani 1 1 d . . . . .
O4 O 0.19726(15) 0.27449(15) 0.53434(13) 0.0325(4) Uani 1 1 d . . . . .
N7 N 0.49374(16) 0.14007(16) 0.58422(14) 0.0218(4) Uani 1 1 d . . . . .
N8 N 0.59590(18) 0.19867(17) 0.63337(15) 0.0263(4) Uani 1 1 d . . . . .
N9 N 0.69991(18) 0.13819(17) 0.61131(15) 0.0270(4) Uani 1 1 d . . . . .
N10 N 0.66869(17) 0.03969(18) 0.54804(15) 0.0248(4) Uani 1 1 d . . . . .
N11 N 0.36609(17) 0.17387(18) 0.60438(15) 0.0258(4) Uani 1 1 d . . . . .
N12 N 0.31275(17) 0.23941(16) 0.52556(14) 0.0232(4) Uani 1 1 d . . . . .
C2 C 0.5398(2) 0.0430(2) 0.53189(17) 0.0204(4) Uani 1 1 d . . . . .
Zn Zn 0.53190(2) 0.49777(2) 0.22808(2) 0.01953(9) Uani 1 1 d . . . . .
N13 N 0.4096(2) 0.6261(2) 0.1598(2) 0.0333(5) Uani 1 1 d . . . . .
N14 N 0.4974(2) 0.3207(2) 0.1789(2) 0.0296(5) Uani 1 1 d . . . . .
N15 N 0.72127(19) 0.5363(2) 0.21838(19) 0.0263(4) Uani 1 1 d . . . . .
N16 N 0.4883(2) 0.5032(2) 0.37475(15) 0.0232(4) Uani 1 1 d . . . . .
H16B H 0.446(3) 0.569(3) 0.388(2) 0.037(8) Uiso 1 1 d . . . . .
H15B H 0.738(3) 0.608(3) 0.195(2) 0.033(7) Uiso 1 1 d . . . . .
H13B H 0.445(3) 0.674(3) 0.122(3) 0.063(11) Uiso 1 1 d . . . . .
H16C H 0.439(3) 0.441(3) 0.396(2) 0.059(10) Uiso 1 1 d . . . . .
H14C H 0.554(3) 0.297(3) 0.145(2) 0.054(10) Uiso 1 1 d . . . . .
H14B H 0.420(4) 0.317(3) 0.146(3) 0.058(10) Uiso 1 1 d . . . . .
H16A H 0.569(5) 0.499(4) 0.407(3) 0.095(15) Uiso 1 1 d . . . . .
H13A H 0.380(3) 0.674(3) 0.206(3) 0.063(11) Uiso 1 1 d . . . . .
H15C H 0.763(4) 0.474(3) 0.186(3) 0.068(11) Uiso 1 1 d . . . . .
H15A H 0.760(3) 0.533(3) 0.272(3) 0.055(11) Uiso 1 1 d . . . . .
H14A H 0.494(3) 0.274(4) 0.231(3) 0.074(12) Uiso 1 1 d . . . . .
H13C H 0.340(4) 0.594(4) 0.134(3) 0.073(12) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N6 1.243(2) . ?
O2 N6 1.253(2) . ?
N1 C1 1.343(3) . ?
N1 N2 1.352(2) . ?
N1 N5 1.391(2) . ?
N2 N3 1.301(3) . ?
N3 N4 1.358(3) . ?
N4 C1 1.324(3) . ?
N5 N6 1.340(2) . ?
C1 C1 1.446(4) 3_655 ?
O3 N12 1.244(2) . ?
O4 N12 1.254(2) . ?
N7 N8 1.343(2) . ?
N7 C2 1.345(3) . ?
N7 N11 1.400(2) . ?
N8 N9 1.295(3) . ?
N9 N10 1.362(3) . ?
N10 C2 1.322(3) . ?
N11 N12 1.332(3) . ?
C2 C2 1.451(4) 3_656 ?
Zn N15 1.995(2) . ?
Zn N16 2.0089(19) . ?
Zn N14 2.016(2) . ?
Zn N13 2.019(2) . ?
N13 H13B 0.81(4) . ?
N13 H13A 0.87(4) . ?
N13 H13C 0.84(4) . ?
N14 H14C 0.79(3) . ?
N14 H14B 0.88(4) . ?
N14 H14A 0.85(4) . ?
N15 H15B 0.84(3) . ?
N15 H15C 0.91(4) . ?
N15 H15A 0.79(4) . ?
N16 H16B 0.85(3) . ?
N16 H16C 0.89(4) . ?
N16 H16A 0.91(5) . ?

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
_geom_angle_publ_flag
C1 N1 N2 108.69(17) . . ?
C1 N1 N5 130.90(17) . . ?
N2 N1 N5 120.11(16) . . ?
N3 N2 N1 105.81(16) . . ?
N2 N3 N4 111.38(17) . . ?
C1 N4 N3 105.61(17) . . ?
N6 N5 N1 109.03(15) . . ?
O1 N6 O2 122.29(17) . . ?
O1 N6 N5 123.53(17) . . ?
O2 N6 N5 114.18(16) . . ?
N4 C1 N1 108.51(18) . . ?
N4 C1 C1 126.9(2) . 3_655 ?
N1 C1 C1 124.6(2) . 3_655 ?
N8 N7 C2 108.23(17) . . ?
N8 N7 N11 119.71(17) . . ?
C2 N7 N11 131.37(18) . . ?
N9 N8 N7 106.64(17) . . ?
N8 N9 N10 111.03(17) . . ?
C2 N10 N9 105.37(18) . . ?
N12 N11 N7 108.90(16) . . ?
O3 N12 O4 121.89(19) . . ?
O3 N12 N11 123.19(17) . . ?
O4 N12 N11 114.91(18) . . ?
N10 C2 N7 108.73(19) . . ?
N10 C2 C2 126.1(2) . 3_656 ?
N7 C2 C2 125.2(2) . 3_656 ?
N15 Zn N16 109.86(10) . . ?
N15 Zn N14 108.70(10) . . ?
N16 Zn N14 106.75(10) . . ?
N15 Zn N13 114.02(10) . . ?
N16 Zn N13 103.43(10) . . ?
N14 Zn N13 113.69(11) . . ?
Zn N13 H13B 114(2) . . ?
Zn N13 H13A 109(2) . . ?
H13B N13 H13A 105(3) . . ?
Zn N13 H13C 113(3) . . ?
H13B N13 H13C 114(3) . . ?
H13A N13 H13C 101(3) . . ?
Zn N14 H14C 111(2) . . ?
Zn N14 H14B 109(2) . . ?
H14C N14 H14B 113(3) . . ?
Zn N14 H14A 108(2) . . ?
H14C N14 H14A 110(3) . . ?
H14B N14 H14A 107(3) . . ?
Zn N15 H15B 115.6(18) . . ?
Zn N15 H15C 112(2) . . ?
H15B N15 H15C 112(3) . . ?
Zn N15 H15A 111(2) . . ?
H15B N15 H15A 106(3) . . ?
H15C N15 H15A 99(3) . . ?
Zn N16 H16B 112.3(18) . . ?
Zn N16 H16C 117(2) . . ?
H16B N16 H16C 104(3) . . ?
Zn N16 H16A 101(3) . . ?
H16B N16 H16A 114(3) . . ?
H16C N16 H16A 109(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.3(2) . . . . ?
N5 N1 N2 N3 174.69(17) . . . . ?
N1 N2 N3 N4 0.1(2) . . . . ?
N2 N3 N4 C1 -0.4(2) . . . . ?
C1 N1 N5 N6 -74.7(3) . . . . ?
N2 N1 N5 N6 112.41(19) . . . . ?
N1 N5 N6 O1 -0.4(2) . . . . ?
N1 N5 N6 O2 178.97(16) . . . . ?
N3 N4 C1 N1 0.6(2) . . . . ?
N3 N4 C1 C1 -179.4(2) . . . 3_655 ?
N2 N1 C1 N4 -0.6(2) . . . . ?
N5 N1 C1 N4 -174.15(19) . . . . ?
N2 N1 C1 C1 179.4(2) . . . 3_655 ?
N5 N1 C1 C1 5.9(4) . . . 3_655 ?
C2 N7 N8 N9 -0.2(2) . . . . ?
N11 N7 N8 N9 171.36(18) . . . . ?
N7 N8 N9 N10 -0.1(2) . . . . ?
N8 N9 N10 C2 0.3(2) . . . . ?
N8 N7 N11 N12 106.3(2) . . . . ?
C2 N7 N11 N12 -84.4(3) . . . . ?
N7 N11 N12 O3 0.2(3) . . . . ?
N7 N11 N12 O4 179.51(17) . . . . ?
N9 N10 C2 N7 -0.4(2) . . . . ?
N9 N10 C2 C2 179.4(3) . . . 3_656 ?
N8 N7 C2 N10 0.3(2) . . . . ?
N11 N7 C2 N10 -169.8(2) . . . . ?
N8 N7 C2 C2 -179.4(3) . . . 3_656 ?
N11 N7 C2 C2 10.4(4) . . . 3_656 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
N16 H16B N8 0.85(3) 2.52(3) 3.289(3) 150(2) 3_666
N15 H15B O2 0.84(3) 2.16(3) 2.999(3) 172(2) 3_665
N13 H13B O1 0.81(4) 2.33(4) 3.081(3) 153(3) 3_665
N13 H13B O4 0.81(4) 2.66(4) 3.129(3) 119(3) 2
N16 H16C O3 0.89(4) 2.14(4) 3.008(3) 164(3) .
N14 H14C O4 0.79(3) 2.28(3) 3.063(3) 173(3) 4_665
N14 H14B O1 0.88(4) 2.60(3) 3.180(3) 125(3) .
N14 H14B N9 0.88(4) 2.31(4) 3.141(3) 157(3) 4_565
N16 H16A N5 0.91(5) 2.16(5) 3.030(3) 161(3) 4_666
N13 H13A N8 0.87(4) 2.50(4) 3.299(3) 153(3) 3_666
N15 H15C N11 0.91(4) 2.21(4) 3.126(3) 178(3) 4_665
N15 H15A N4 0.79(4) 2.47(4) 3.139(3) 143(3) 2_655
N14 H14A O2 0.85(4) 2.57(4) 3.055(3) 117(3) 4_666
N13 H13C N10 0.84(4) 2.47(4) 3.291(3) 167(3) 4_565
N16 H16B N8 0.85(3) 2.52(3) 3.289(3) 150(2) 3_666
N15 H15B O2 0.84(3) 2.16(3) 2.999(3) 172(2) 3_665
N13 H13B O1 0.81(4) 2.33(4) 3.081(3) 153(3) 3_665
N13 H13B O4 0.81(4) 2.66(4) 3.129(3) 119(3) 2
N16 H16C O3 0.89(4) 2.14(4) 3.008(3) 164(3) .
N14 H14C O4 0.79(3) 2.28(3) 3.063(3) 173(3) 4_665
N14 H14B O1 0.88(4) 2.60(3) 3.180(3) 125(3) .
N14 H14B N9 0.88(4) 2.31(4) 3.141(3) 157(3) 4_565
N16 H16A N5 0.91(5) 2.16(5) 3.030(3) 161(3) 4_666
N13 H13A N8 0.87(4) 2.50(4) 3.299(3) 153(3) 3_666
N15 H15C N11 0.91(4) 2.21(4) 3.126(3) 178(3) 4_665
N15 H15A N4 0.79(4) 2.47(4) 3.139(3) 143(3) 2_655
N14 H14A O2 0.85(4) 2.57(4) 3.055(3) 117(3) 4_666
N13 H13C N10 0.84(4) 2.47(4) 3.291(3) 167(3) 4_565

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.585
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.060

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kx310
_database_code_depnum_ccdc_archive 'CCDC 1500004'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_block_code                ?
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_audit_creation_date             
;
'Sat Sep 05 10:27:31 2015'
;

_chemical_name_systematic        'dicesium 1,1-dinitramino-5,5-bitetrazolate'
_chemical_compound_source        ?
_chemical_name_common            'dicesium 1,1-dinitramino-5,5-bitetrazolate'
_chemical_formula_moiety         'C2 N12 O4, 2(Cs)'
_chemical_formula_sum            'C2 Cs2 N12 O4'
_chemical_formula_weight         521.96


_cell_length_a                   5.5885(2)
_cell_length_b                   12.4847(4)
_cell_length_c                   8.7893(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.250(3)
_cell_angle_gamma                90.00
_cell_volume                     612.76(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3426
_cell_measurement_theta_min      4.5340
_cell_measurement_theta_max      30.9800
_cell_special_details            ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             476
_exptl_absorpt_coefficient_mu    5.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2154
_exptl_absorpt_correction_T_max  0.7957
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173 # in K
_diffrn_source_type              'Spellman generator'
_diffrn_source_power             ? # in kW
_diffrn_source_voltage           50 # kV
_diffrn_source_current           40 # mA
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_collimation    0.5
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_detector_area_resol_mean 15.9809

_diffrn_reflns_number            8446
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.55
_diffrn_reflns_theta_max         26.00
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996

_reflns_number_total             1195
_reflns_number_gt                1061
_reflns_threshold_expression     >2sigma(I)

_diffrn_orient_matrix_UB_11      0.0095109000
_diffrn_orient_matrix_UB_12      -0.0563944000
_diffrn_orient_matrix_UB_13      -0.0074613000
_diffrn_orient_matrix_UB_21      0.0067605000
_diffrn_orient_matrix_UB_22      -0.0052176000
_diffrn_orient_matrix_UB_23      0.0804372000
_diffrn_orient_matrix_UB_31      -0.1264461000
_diffrn_orient_matrix_UB_32      -0.0045084000
_diffrn_orient_matrix_UB_33      0.0005538000

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  -P2ybc

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'
Cs Cs -0.3680 2.1192 '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_
_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'

_exptl_special_details           ?


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

_diffrn_special_details          ?

_refine_diff_density_max         0.771
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.092

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0161P)²+0.3529P] where P=(Fo²+2Fc²)/3'


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
# Plot Program for Crystal Structure Illustrations, Oak Ridge National
# Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
# Glasgow) used --- SCHAKAL (E. Keller, University of  Freiburg (Breisgau),
# Germany, 1995)'
;

_computing_publication_material  
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
# --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses).
;

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         1195
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0386
_refine_ls_wR_factor_gt          0.0370
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7006(4) 0.10864(18) 0.4371(3) 0.0296(5) Uani 1 1 d . . .
O2 O 0.4894(4) 0.16766(17) 0.2401(3) 0.0289(5) Uani 1 1 d . . .
N1 N 0.6661(4) 0.11829(19) 0.2961(3) 0.0222(6) Uani 1 1 d . . .
N2 N 0.8281(4) 0.0692(2) 0.2140(3) 0.0236(6) Uani 1 1 d . . .
N4 N 0.8085(5) 0.1321(2) -0.1676(3) 0.0290(6) Uani 1 1 d . . .
N5 N 0.6126(4) 0.0675(2) -0.1701(3) 0.0258(6) Uani 1 1 d . . .
C1 C 0.5905(5) 0.0359(2) -0.0280(4) 0.0209(6) Uani 1 1 d . . .
N7 N 0.7656(4) 0.08129(19) 0.0604(3) 0.0210(6) Uani 1 1 d . . .
N10 N 0.9018(5) 0.14143(19) -0.0305(3) 0.0263(6) Uani 1 1 d . . .
Cs1 Cs 0.21249(3) 0.351767(14) 0.06828(2) 0.02479(8) Uani 1 1 d . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N1 1.253(3) . ?
O1 Cs1 3.043(2) 4_566 ?
O1 Cs1 3.082(2) 4_666 ?
O1 Cs1 3.244(2) 2_645 ?
O2 N1 1.249(3) . ?
O2 Cs1 3.127(2) . ?
O2 Cs1 3.335(2) 4_566 ?
N1 N2 1.330(4) . ?
N1 Cs1 3.573(3) 4_566 ?
N1 Cs1 3.590(2) 2_645 ?
N1 Cs1 3.822(2) 4_666 ?
N2 N7 1.389(3) . ?
N2 Cs1 3.334(3) 2_645 ?
N2 Cs1 3.842(3) 4_666 ?
N4 N10 1.299(4) . ?
N4 N5 1.359(4) . ?
N4 Cs1 3.307(3) 4_665 ?
N5 C1 1.320(4) . ?
N5 Cs1 3.302(3) 4_565 ?
C1 N7 1.350(4) . ?
C1 C1 1.452(6) 3_655 ?
N7 N10 1.353(3) . ?
N10 Cs1 3.248(2) 1_655 ?
Cs1 O1 3.043(2) 4_565 ?
Cs1 O1 3.082(2) 4_465 ?
Cs1 O1 3.244(2) 2_655 ?
Cs1 N10 3.248(2) 1_455 ?
Cs1 N5 3.302(3) 4_566 ?
Cs1 N4 3.307(3) 4_466 ?
Cs1 N2 3.334(3) 2_655 ?
Cs1 O2 3.335(2) 4_565 ?
Cs1 N1 3.573(3) 4_565 ?
Cs1 N1 3.590(2) 2_655 ?
Cs1 N1 3.822(2) 4_465 ?

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
_geom_angle_publ_flag
N1 O1 Cs1 104.71(17) . 4_566 ?
N1 O1 Cs1 117.32(18) . 4_666 ?
Cs1 O1 Cs1 131.68(8) 4_566 4_666 ?
N1 O1 Cs1 95.62(16) . 2_645 ?
Cs1 O1 Cs1 107.64(7) 4_566 2_645 ?
Cs1 O1 Cs1 91.53(6) 4_666 2_645 ?
N1 O2 Cs1 157.22(19) . . ?
N1 O2 Cs1 90.57(17) . 4_566 ?
Cs1 O2 Cs1 103.51(6) . 4_566 ?
O2 N1 O1 121.7(3) . . ?
O2 N1 N2 123.9(3) . . ?
O1 N1 N2 114.3(2) . . ?
O2 N1 Cs1 68.97(16) . 4_566 ?
O1 N1 Cs1 55.47(15) . 4_566 ?
N2 N1 Cs1 158.10(18) . 4_566 ?
O2 N1 Cs1 136.42(18) . 2_645 ?
O1 N1 Cs1 64.06(15) . 2_645 ?
N2 N1 Cs1 68.22(15) . 2_645 ?
Cs1 N1 Cs1 90.26(6) 4_566 2_645 ?
O2 N1 Cs1 142.98(18) . 4_666 ?
O1 N1 Cs1 45.75(14) . 4_666 ?
N2 N1 Cs1 80.83(15) . 4_666 ?
Cs1 N1 Cs1 98.11(6) 4_566 4_666 ?
Cs1 N1 Cs1 75.35(5) 2_645 4_666 ?
N1 N2 N7 109.1(2) . . ?
N1 N2 Cs1 90.04(16) . 2_645 ?
N7 N2 Cs1 128.77(17) . 2_645 ?
N1 N2 Cs1 79.18(15) . 4_666 ?
N7 N2 Cs1 150.56(17) . 4_666 ?
Cs1 N2 Cs1 78.02(5) 2_645 4_666 ?
N10 N4 N5 111.2(3) . . ?
N10 N4 Cs1 112.66(18) . 4_665 ?
N5 N4 Cs1 126.6(2) . 4_665 ?
C1 N5 N4 105.5(3) . . ?
C1 N5 Cs1 131.62(19) . 4_565 ?
N4 N5 Cs1 110.67(18) . 4_565 ?
N5 C1 N7 109.1(3) . . ?
N5 C1 C1 126.7(3) . 3_655 ?
N7 C1 C1 124.3(3) . 3_655 ?
C1 N7 N10 107.7(3) . . ?
C1 N7 N2 131.5(2) . . ?
N10 N7 N2 120.6(2) . . ?
N4 N10 N7 106.5(2) . . ?
N4 N10 Cs1 120.77(18) . 1_655 ?
N7 N10 Cs1 126.73(19) . 1_655 ?
O1 Cs1 O1 131.68(8) 4_565 4_465 ?
O1 Cs1 O2 82.44(6) 4_565 . ?
O1 Cs1 O2 137.15(6) 4_465 . ?
O1 Cs1 O1 72.36(7) 4_565 2_655 ?
O1 Cs1 O1 88.47(6) 4_465 2_655 ?
O2 Cs1 O1 131.47(6) . 2_655 ?
O1 Cs1 N10 120.52(6) 4_565 1_455 ?
O1 Cs1 N10 63.32(6) 4_465 1_455 ?
O2 Cs1 N10 77.53(7) . 1_455 ?
O1 Cs1 N10 150.95(6) 2_655 1_455 ?
O1 Cs1 N5 67.76(6) 4_565 4_566 ?
O1 Cs1 N5 143.60(6) 4_465 4_566 ?
O2 Cs1 N5 65.12(6) . 4_566 ?
O1 Cs1 N5 67.09(6) 2_655 4_566 ?
N10 Cs1 N5 140.68(7) 1_455 4_566 ?
O1 Cs1 N4 154.52(6) 4_565 4_466 ?
O1 Cs1 N4 66.64(7) 4_465 4_466 ?
O2 Cs1 N4 92.54(6) . 4_466 ?
O1 Cs1 N4 93.26(6) 2_655 4_466 ?
N10 Cs1 N4 82.21(7) 1_455 4_466 ?
N5 Cs1 N4 87.42(7) 4_566 4_466 ?
O1 Cs1 N2 99.64(6) 4_565 2_655 ?
O1 Cs1 N2 90.05(6) 4_465 2_655 ?
O2 Cs1 N2 111.39(6) . 2_655 ?
O1 Cs1 N2 38.49(6) 2_655 2_655 ?
N10 Cs1 N2 139.82(6) 1_455 2_655 ?
N5 Cs1 N2 53.92(6) 4_566 2_655 ?
N4 Cs1 N2 58.92(6) 4_466 2_655 ?
O1 Cs1 O2 39.74(6) 4_565 4_565 ?
O1 Cs1 O2 98.26(6) 4_465 4_565 ?
O2 Cs1 O2 97.27(6) . 4_565 ?
O1 Cs1 O2 89.10(5) 2_655 4_565 ?
N10 Cs1 O2 88.35(6) 1_455 4_565 ?
N5 Cs1 O2 107.45(6) 4_566 4_565 ?
N4 Cs1 O2 164.61(7) 4_466 4_565 ?
N2 Cs1 O2 126.87(6) 2_655 4_565 ?
O1 Cs1 N1 19.82(6) 4_565 4_565 ?
O1 Cs1 N1 113.92(6) 4_465 4_565 ?
O2 Cs1 N1 92.84(6) . 4_565 ?
O1 Cs1 N1 77.07(6) 2_655 4_565 ?
N10 Cs1 N1 106.95(6) 1_455 4_565 ?
N5 Cs1 N1 87.44(6) 4_566 4_565 ?
N4 Cs1 N1 170.21(6) 4_466 4_565 ?
N2 Cs1 N1 111.42(6) 2_655 4_565 ?
O2 Cs1 N1 20.46(5) 4_565 4_565 ?
O1 Cs1 N1 79.32(6) 4_565 2_655 ?
O1 Cs1 N1 97.82(6) 4_465 2_655 ?
O2 Cs1 N1 115.95(6) . 2_655 ?
O1 Cs1 N1 20.32(6) 2_655 2_655 ?
N10 Cs1 N1 158.48(6) 1_455 2_655 ?
N5 Cs1 N1 51.08(6) 4_566 2_655 ?
N4 Cs1 N1 80.55(6) 4_466 2_655 ?
N2 Cs1 N1 21.74(6) 2_655 2_655 ?
O2 Cs1 N1 105.45(6) 4_565 2_655 ?
N1 Cs1 N1 89.74(6) 4_565 2_655 ?
O1 Cs1 N1 116.93(6) 4_565 4_465 ?
O1 Cs1 N1 16.93(6) 4_465 4_465 ?
O2 Cs1 N1 137.92(6) . 4_465 ?
O1 Cs1 N1 90.60(5) 2_655 4_465 ?
N10 Cs1 N1 60.40(6) 1_455 4_465 ?
N5 Cs1 N1 155.30(6) 4_566 4_465 ?
N4 Cs1 N1 83.26(7) 4_466 4_465 ?
N2 Cs1 N1 102.06(6) 2_655 4_465 ?
O2 Cs1 N1 81.50(6) 4_565 4_465 ?
N1 Cs1 N1 98.11(6) 4_565 4_465 ?
N1 Cs1 N1 104.65(5) 2_655 4_465 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cs1 O2 N1 O1 110.9(5) . . . . ?
Cs1 O2 N1 O1 -17.9(3) 4_566 . . . ?
Cs1 O2 N1 N2 -71.2(6) . . . . ?
Cs1 O2 N1 N2 160.0(2) 4_566 . . . ?
Cs1 O2 N1 Cs1 128.8(5) . . . 4_566 ?
Cs1 O2 N1 Cs1 -164.6(3) . . . 2_645 ?
Cs1 O2 N1 Cs1 66.6(2) 4_566 . . 2_645 ?
Cs1 O2 N1 Cs1 53.8(7) . . . 4_666 ?
Cs1 O2 N1 Cs1 -75.0(3) 4_566 . . 4_666 ?
Cs1 O1 N1 O2 20.4(3) 4_566 . . . ?
Cs1 O1 N1 O2 -135.1(2) 4_666 . . . ?
Cs1 O1 N1 O2 130.3(2) 2_645 . . . ?
Cs1 O1 N1 N2 -157.69(18) 4_566 . . . ?
Cs1 O1 N1 N2 46.9(3) 4_666 . . . ?
Cs1 O1 N1 N2 -47.8(2) 2_645 . . . ?
Cs1 O1 N1 Cs1 -155.43(19) 4_666 . . 4_566 ?
Cs1 O1 N1 Cs1 109.92(11) 2_645 . . 4_566 ?
Cs1 O1 N1 Cs1 -109.92(11) 4_566 . . 2_645 ?
Cs1 O1 N1 Cs1 94.65(13) 4_666 . . 2_645 ?
Cs1 O1 N1 Cs1 155.43(19) 4_566 . . 4_666 ?
Cs1 O1 N1 Cs1 -94.65(13) 2_645 . . 4_666 ?
O2 N1 N2 N7 -0.7(4) . . . . ?
O1 N1 N2 N7 177.3(2) . . . . ?
Cs1 N1 N2 N7 120.3(4) 4_566 . . . ?
Cs1 N1 N2 N7 131.5(2) 2_645 . . . ?
Cs1 N1 N2 N7 -150.70(19) 4_666 . . . ?
O2 N1 N2 Cs1 -132.2(2) . . . 2_645 ?
O1 N1 N2 Cs1 45.8(2) . . . 2_645 ?
Cs1 N1 N2 Cs1 -11.2(5) 4_566 . . 2_645 ?
Cs1 N1 N2 Cs1 77.79(5) 4_666 . . 2_645 ?
O2 N1 N2 Cs1 150.0(3) . . . 4_666 ?
O1 N1 N2 Cs1 -32.0(2) . . . 4_666 ?
Cs1 N1 N2 Cs1 -89.0(5) 4_566 . . 4_666 ?
Cs1 N1 N2 Cs1 -77.79(5) 2_645 . . 4_666 ?
N10 N4 N5 C1 -0.8(3) . . . . ?
Cs1 N4 N5 C1 142.6(2) 4_665 . . . ?
N10 N4 N5 Cs1 146.45(19) . . . 4_565 ?
Cs1 N4 N5 Cs1 -70.1(2) 4_665 . . 4_565 ?
N4 N5 C1 N7 1.0(3) . . . . ?
Cs1 N5 C1 N7 -136.4(2) 4_565 . . . ?
N4 N5 C1 C1 -179.0(4) . . . 3_655 ?
Cs1 N5 C1 C1 43.6(5) 4_565 . . 3_655 ?
N5 C1 N7 N10 -0.9(3) . . . . ?
C1 C1 N7 N10 179.1(3) 3_655 . . . ?
N5 C1 N7 N2 -175.8(3) . . . . ?
C1 C1 N7 N2 4.2(6) 3_655 . . . ?
N1 N2 N7 C1 -73.3(4) . . . . ?
Cs1 N2 N7 C1 32.9(4) 2_645 . . . ?
Cs1 N2 N7 C1 -175.3(2) 4_666 . . . ?
N1 N2 N7 N10 112.3(3) . . . . ?
Cs1 N2 N7 N10 -141.5(2) 2_645 . . . ?
Cs1 N2 N7 N10 10.3(5) 4_666 . . . ?
N5 N4 N10 N7 0.3(3) . . . . ?
Cs1 N4 N10 N7 -148.53(16) 4_665 . . . ?
N5 N4 N10 Cs1 -154.15(18) . . . 1_655 ?
Cs1 N4 N10 Cs1 57.1(2) 4_665 . . 1_655 ?
C1 N7 N10 N4 0.4(3) . . . . ?
N2 N7 N10 N4 176.0(2) . . . . ?
C1 N7 N10 Cs1 152.81(19) . . . 1_655 ?
N2 N7 N10 Cs1 -31.6(3) . . . 1_655 ?
N1 O2 Cs1 O1 21.9(5) . . . 4_565 ?
Cs1 O2 Cs1 O1 148.67(7) 4_566 . . 4_565 ?
N1 O2 Cs1 O1 169.4(5) . . . 4_465 ?
Cs1 O2 Cs1 O1 -63.84(10) 4_566 . . 4_465 ?
N1 O2 Cs1 O1 -36.4(5) . . . 2_655 ?
Cs1 O2 Cs1 O1 90.37(9) 4_566 . . 2_655 ?
N1 O2 Cs1 N10 145.6(5) . . . 1_455 ?
Cs1 O2 Cs1 N10 -87.68(7) 4_566 . . 1_455 ?
N1 O2 Cs1 N5 -47.0(5) . . . 4_566 ?
Cs1 O2 Cs1 N5 79.73(7) 4_566 . . 4_566 ?
N1 O2 Cs1 N4 -133.0(5) . . . 4_466 ?
Cs1 O2 Cs1 N4 -6.24(7) 4_566 . . 4_466 ?
N1 O2 Cs1 N2 -75.5(5) . . . 2_655 ?
Cs1 O2 Cs1 N2 51.24(8) 4_566 . . 2_655 ?
N1 O2 Cs1 O2 58.9(5) . . . 4_565 ?
Cs1 O2 Cs1 O2 -174.36(5) 4_566 . . 4_565 ?
N1 O2 Cs1 N1 38.8(5) . . . 4_565 ?
Cs1 O2 Cs1 N1 165.59(6) 4_566 . . 4_565 ?
N1 O2 Cs1 N1 -52.3(5) . . . 2_655 ?
Cs1 O2 Cs1 N1 74.49(8) 4_566 . . 2_655 ?
N1 O2 Cs1 N1 144.2(5) . . . 4_465 ?
Cs1 O2 Cs1 N1 -89.00(9) 4_566 . . 4_465 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
? ? ? ? ? ? ? ?

_geom_special_details            ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx409
_database_code_depnum_ccdc_archive 'CCDC 1502968'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Mon Sep 05 19:34:42 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
tetraammino copper(II) dinitraminobitetrazolate monohydrate
;
_chemical_name_common            
'tetraammino copper(II) dinitraminobitetrazolate monohydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H12 Cu N16 O4, H2 O'
_chemical_formula_sum            'C2 H14 Cu N16 O5'
_chemical_formula_weight         405.83

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'



_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.4131(5)
_cell_length_b                   7.4648(3)
_cell_length_c                   17.2079(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.739(5)
_cell_angle_gamma                90
_cell_volume                     1449.03(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1615
_cell_measurement_theta_min      4.6280
_cell_measurement_theta_max      30.2050

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.570
_shelx_estimated_absorpt_T_min   0.714
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95307
_exptl_absorpt_correction_T_max  0.99999
_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_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            5250
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.216
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1422
_reflns_number_gt                1205
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+1.5840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1422
_refine_ls_number_parameters     117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0526741000
_diffrn_orient_matrix_UB_12      -0.0045918000
_diffrn_orient_matrix_UB_13      -0.0171074000
_diffrn_orient_matrix_UB_21      0.0321063000
_diffrn_orient_matrix_UB_22      0.0400154000
_diffrn_orient_matrix_UB_23      0.0341370000
_diffrn_orient_matrix_UB_31      0.0121133500
_diffrn_orient_matrix_UB_32      -0.0860739500
_diffrn_orient_matrix_UB_33      0.0167743000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -84.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -38.0000 -180.0000 86

#__ type_ start__ end____ width___ exp.time_
  2 omega -111.00  -85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  179.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
  3 omega  -37.00   28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000  -60.0000 65

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
  5 omega  -34.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -57.0000    0.0000 59

#__ type_ start__ end____ width___ exp.time_
  6 omega    7.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   38.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  7 omega  -24.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -180.0000 97

;



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'
Cu Cu 0.3201 1.2651 '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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.01719(14) Uani 1 2 d S . P . .
O2 O -0.12771(16) 0.4472(3) 0.02377(11) 0.0280(4) Uani 1 1 d . . . . .
O1 O -0.03129(17) 0.5525(2) 0.13336(11) 0.0308(5) Uani 1 1 d . . . . .
N8 N -0.13259(17) -0.0924(3) 0.05338(13) 0.0232(5) Uani 1 1 d . . . . .
H8B H -0.1223 -0.2117 0.0630 0.035 Uiso 1 1 calc R U . . .
H8A H -0.2030 -0.0741 0.0217 0.035 Uiso 1 1 calc R U . . .
H8C H -0.1326 -0.0333 0.0996 0.035 Uiso 1 1 calc R U . . .
N7 N -0.11651(17) 0.1276(3) -0.08183(12) 0.0228(5) Uani 1 1 d . . . . .
H7C H -0.1333 0.2375 -0.0634 0.034 Uiso 1 1 calc R U . . .
H7B H -0.1844 0.0622 -0.0922 0.034 Uiso 1 1 calc R U . . .
H7A H -0.0842 0.1406 -0.1267 0.034 Uiso 1 1 calc R U . . .
N3 N 0.24436(18) 0.2425(3) 0.23630(13) 0.0294(5) Uani 1 1 d . . . . .
N4 N 0.16088(18) 0.2422(3) 0.28509(13) 0.0258(5) Uani 1 1 d . . . . .
N2 N 0.19597(18) 0.2581(3) 0.16301(13) 0.0260(5) Uani 1 1 d . . . . .
N1 N 0.07842(16) 0.2675(3) 0.16369(12) 0.0170(4) Uani 1 1 d . . . . .
N5 N 0.00049(17) 0.2702(3) 0.09288(12) 0.0196(5) Uani 1 1 d . . . . .
N6 N -0.05211(18) 0.4300(3) 0.08477(12) 0.0202(5) Uani 1 1 d . . . . .
C1 C 0.05829(19) 0.2568(3) 0.23840(13) 0.0169(5) Uani 1 1 d . . . . .
O3 O 0.5000 0.3624(4) 0.2500 0.0278(7) Uani 1 2 d S T P . .
H3 H 0.449(2) 0.302(4) 0.250(2) 0.036(10) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N8 2.008(2) . ?
Cu1 N8 2.008(2) 5 ?
Cu1 N7 2.0222(19) . ?
Cu1 N7 2.0223(19) 5 ?
O2 N6 1.260(3) . ?
O1 N6 1.237(3) . ?
N8 H8B 0.9100 . ?
N8 H8A 0.9100 . ?
N8 H8C 0.9100 . ?
N7 H7C 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7A 0.9100 . ?
N3 N2 1.303(3) . ?
N3 N4 1.362(3) . ?
N4 C1 1.320(3) . ?
N2 N1 1.345(3) . ?
N1 C1 1.342(3) . ?
N1 N5 1.395(3) . ?
N5 N6 1.334(3) . ?
C1 C1 1.446(4) 2 ?
O3 H3 0.74(3) . ?

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
_geom_angle_publ_flag
N8 Cu1 N8 180.0 . 5 ?
N8 Cu1 N7 91.08(8) . . ?
N8 Cu1 N7 88.92(8) 5 . ?
N8 Cu1 N7 88.92(8) . 5 ?
N8 Cu1 N7 91.08(8) 5 5 ?
N7 Cu1 N7 180.00(17) . 5 ?
Cu1 N8 H8B 109.5 . . ?
Cu1 N8 H8A 109.5 . . ?
H8B N8 H8A 109.5 . . ?
Cu1 N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
Cu1 N7 H7C 109.5 . . ?
Cu1 N7 H7B 109.5 . . ?
H7C N7 H7B 109.5 . . ?
Cu1 N7 H7A 109.5 . . ?
H7C N7 H7A 109.5 . . ?
H7B N7 H7A 109.5 . . ?
N2 N3 N4 111.30(19) . . ?
C1 N4 N3 105.3(2) . . ?
N3 N2 N1 105.84(19) . . ?
C1 N1 N2 108.74(19) . . ?
C1 N1 N5 131.16(19) . . ?
N2 N1 N5 119.83(19) . . ?
N6 N5 N1 108.74(18) . . ?
O1 N6 O2 121.7(2) . . ?
O1 N6 N5 123.6(2) . . ?
O2 N6 N5 114.7(2) . . ?
N4 C1 N1 108.8(2) . . ?
N4 C1 C1 126.9(3) . 2 ?
N1 C1 C1 124.3(3) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 N3 N4 C1 0.6(3) . . . . ?
N4 N3 N2 N1 -0.3(3) . . . . ?
N3 N2 N1 C1 -0.1(3) . . . . ?
N3 N2 N1 N5 -174.7(2) . . . . ?
C1 N1 N5 N6 73.9(3) . . . . ?
N2 N1 N5 N6 -112.9(2) . . . . ?
N1 N5 N6 O1 0.7(3) . . . . ?
N1 N5 N6 O2 -177.95(19) . . . . ?
N3 N4 C1 N1 -0.6(3) . . . . ?
N3 N4 C1 C1 177.83(13) . . . 2 ?
N2 N1 C1 N4 0.5(3) . . . . ?
N5 N1 C1 N4 174.3(2) . . . . ?
N2 N1 C1 C1 -178.02(12) . . . 2 ?
N5 N1 C1 C1 -4.2(3) . . . 2 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
N8 H8B O2 0.91 2.63 3.476(3) 154.5 1_545
N8 H8B O1 0.91 2.29 3.127(3) 151.9 1_545
N8 H8A O2 0.91 2.19 3.053(3) 158.6 7_455
N7 H7C O2 0.91 2.16 3.013(3) 155.3 .
N7 H7B O2 0.91 2.60 3.274(3) 131.5 7_455
N7 H7B N2 0.91 2.68 3.268(3) 123.4 5
N7 H7A O1 0.91 2.65 3.129(3) 113.4 5_565
N7 H7A O3 0.91 2.46 3.364(2) 173.3 7
O3 H3 N3 0.74(3) 2.35(3) 3.027(2) 153(3) .
N8 H8B O2 0.91 2.63 3.476(3) 154.5 1_545
N8 H8B O1 0.91 2.29 3.127(3) 151.9 1_545
N8 H8A O2 0.91 2.19 3.053(3) 158.6 7_455
N7 H7C O2 0.91 2.16 3.013(3) 155.3 .
N7 H7B O2 0.91 2.60 3.274(3) 131.5 7_455
N7 H7B N2 0.91 2.68 3.268(3) 123.4 5
N7 H7A O1 0.91 2.65 3.129(3) 113.4 5_565
N7 H7A O3 0.91 2.46 3.364(2) 173.3 7
O3 H3 N3 0.74(3) 2.35(3) 3.027(2) 153(3) .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.274
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_uv586
_database_code_depnum_ccdc_archive 'CCDC 1524646'
_audit_update_record             
;
2016-12-27 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;

_vrf_PLAT417_uv586               
; 
PROBLEM: Short Inter D-H..H-D     H9B   ..  H10B    ..      1.64 Ang.
RESPONSE: Both two non-ccordinated crystal water are disordered 
;
_audit_creation_date             11.10.2016
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
barium 1,1-dinitramino-5,5-bitetrazolate hexahydrate
;
_chemical_name_common            
'barium 1,1-dinitramino-5,5-bitetrazolate hexahydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H8 Ba N12 O8, 2(H2 O)'
_chemical_formula_sum            'C2 H12 Ba N12 O10'
_chemical_formula_weight         501.58

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.9593(3)
_cell_length_b                   9.5952(3)
_cell_length_c                   17.9981(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.7980(10)
_cell_angle_gamma                90
_cell_volume                     1545.38(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.5915
_cell_measurement_theta_max      36.4531

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.651
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            49826
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.266
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3024
_reflns_number_gt                2875
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0472P)²+1.2739P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3024
_refine_ls_number_parameters     246
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0162
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0561
_refine_ls_goodness_of_fit_ref   1.434
_refine_ls_restrained_S_all      1.434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba Ba 0.18040(2) 0.03630(2) 0.72804(2) 0.01074(11) Uani 1 1 d . . . . .
N5 N 0.1614(4) -0.0465(3) 0.88071(16) 0.0154(6) Uani 1 1 d . . . . .
N2 N 0.3136(3) 0.0450(3) 0.98118(17) 0.0183(6) Uani 1 1 d . . . . .
C1 C 0.0781(4) 0.0173(3) 1.00544(19) 0.0139(7) Uani 1 1 d . . . . .
O1 O 0.1750(3) -0.2621(2) 0.93249(13) 0.0239(5) Uani 1 1 d . . . . .
O3 O 0.5109(2) -0.2606(2) 0.60837(13) 0.0189(5) Uani 1 1 d . . . . .
O4 O 0.3177(2) -0.2324(2) 0.67723(12) 0.0167(5) Uani 1 1 d . . . . .
N10 N 0.6873(3) 0.0782(3) 0.51605(14) 0.0138(5) Uani 1 1 d . . . . .
N12 N 0.4241(3) -0.1851(3) 0.64113(14) 0.0115(5) Uani 1 1 d . . . . .
N9 N 0.7561(3) 0.0938(3) 0.58471(15) 0.0175(6) Uani 1 1 d . . . . .
N3 N 0.2920(3) 0.0887(3) 1.04823(16) 0.0208(6) Uani 1 1 d . . . . .
N6 N 0.1638(3) -0.1845(3) 0.87802(14) 0.0130(5) Uani 1 1 d . . . . .
N8 N 0.6742(3) 0.0469(3) 0.63635(16) 0.0159(6) Uani 1 1 d . . . . .
O2 O 0.1510(3) -0.2307(2) 0.81197(12) 0.0167(5) Uani 1 1 d . . . . .
N4 N 0.1462(3) 0.0728(3) 1.06510(15) 0.0176(6) Uani 1 1 d . . . . .
N11 N 0.4294(3) -0.0468(3) 0.64178(16) 0.0131(6) Uani 1 1 d . . . . .
N1 N 0.1801(3) -0.0017(3) 0.95400(15) 0.0138(5) Uani 1 1 d . . . . .
N7 N 0.5483(3) -0.0011(3) 0.60141(14) 0.0101(5) Uani 1 1 d . . . . .
C2 C 0.5578(4) 0.0192(3) 0.52787(18) 0.0102(6) Uani 1 1 d . . . . .
O5 O 0.4543(4) 0.0375(3) 0.81546(19) 0.0273(7) Uani 1 1 d . . . . .
O6 O -0.1122(3) -0.0303(3) 0.77176(15) 0.0275(7) Uani 1 1 d . . . . .
O8 O 0.0768(3) -0.0437(3) 0.58747(16) 0.0287(6) Uani 1 1 d . . . . .
O7 O -0.0084(4) 0.2454(3) 0.6739(2) 0.0464(9) Uani 1 1 d . . . . .
O9 O -0.1387(4) -0.2495(4) 0.5676(2) 0.0519(9) Uani 1 1 d . . . . .
H9C H -0.1008 -0.2449 0.5341 0.062 Uiso 1 1 d R U . . .
H9B H -0.2238 -0.3020 0.5801 0.062 Uiso 1 1 d R U . . .
O10 O 0.6959(4) 0.2102(4) 0.78959(19) 0.0592(11) Uani 1 1 d . . . . .
H10B H 0.6770 0.2430 0.8338 0.071 Uiso 1 1 d R U . . .
H8A H 0.1417 -0.0689 0.5561 0.071 Uiso 1 1 d R U . . .
H10A H 0.7082 0.2643 0.7645 0.071 Uiso 1 1 d R U . . .
H8B H 0.0195 -0.1111 0.5828 0.071 Uiso 1 1 d R U . . .
H6C H -0.1144 -0.0373 0.8216 0.071 Uiso 1 1 d R U . . .
H5A H 0.449(7) 0.051(6) 0.862(4) 0.054(17) Uiso 1 1 d . . . . .
H5B H 0.523(7) 0.077(6) 0.801(3) 0.045(17) Uiso 1 1 d . . . . .
H6A H -0.169(6) 0.029(6) 0.770(3) 0.04(2) Uiso 1 1 d . . . . .
H7A H -0.064(6) 0.228(5) 0.630(3) 0.042(13) Uiso 1 1 d . . . . .
H7B H -0.008(5) 0.327(6) 0.678(3) 0.033(13) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba O8 2.761(3) . ?
Ba O7 2.771(3) . ?
Ba O4 2.798(2) 2_556 ?
Ba O2 2.812(2) 2_556 ?
Ba O6 2.846(3) . ?
Ba O5 2.850(3) . ?
Ba N5 2.873(3) . ?
Ba N11 2.892(3) . ?
Ba O2 2.992(2) . ?
Ba O4 3.018(2) . ?
N5 N6 1.326(4) . ?
N5 N1 1.390(4) . ?
N2 N3 1.301(4) . ?
N2 N1 1.346(4) . ?
C1 N4 1.321(5) . ?
C1 N1 1.345(4) . ?
C1 C1 1.442(7) 3_557 ?
O1 N6 1.231(4) . ?
O3 N12 1.233(3) . ?
O4 N12 1.264(3) . ?
O4 Ba 2.798(2) 2_546 ?
N10 C2 1.317(4) . ?
N10 N9 1.362(4) . ?
N12 N11 1.327(4) . ?
N9 N8 1.293(4) . ?
N3 N4 1.364(4) . ?
N6 O2 1.268(3) . ?
N8 N7 1.345(4) . ?
O2 Ba 2.812(2) 2_546 ?
N11 N7 1.389(4) . ?
N7 C2 1.345(4) . ?
C2 C2 1.454(7) 3_656 ?
O5 H5A 0.85(6) . ?
O5 H5B 0.78(6) . ?
O6 H6C 0.9000 . ?
O6 H6A 0.77(6) . ?
O8 H8A 0.8655 . ?
O8 H8B 0.8277 . ?
O7 H7A 0.93(5) . ?
O7 H7B 0.78(5) . ?
O9 H9C 0.7087 . ?
O9 H9B 0.9497 . ?
O10 H10B 0.8789 . ?
O10 H10A 0.7007 . ?

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
_geom_angle_publ_flag
O8 Ba O7 72.94(9) . . ?
O8 Ba O4 140.41(7) . 2_556 ?
O7 Ba O4 68.01(8) . 2_556 ?
O8 Ba O2 98.46(7) . 2_556 ?
O7 Ba O2 70.14(9) . 2_556 ?
O4 Ba O2 62.48(7) 2_556 2_556 ?
O8 Ba O6 85.29(8) . . ?
O7 Ba O6 72.86(10) . . ?
O4 Ba O6 89.32(8) 2_556 . ?
O2 Ba O6 139.72(8) 2_556 . ?
O8 Ba O5 138.51(9) . . ?
O7 Ba O5 133.30(8) . . ?
O4 Ba O5 71.39(7) 2_556 . ?
O2 Ba O5 71.30(8) 2_556 . ?
O6 Ba O5 128.92(10) . . ?
O8 Ba N5 140.05(8) . . ?
O7 Ba N5 118.24(10) . . ?
O4 Ba N5 68.62(7) 2_556 . ?
O2 Ba N5 121.50(7) 2_556 . ?
O6 Ba N5 64.86(9) . . ?
O5 Ba N5 64.07(10) . . ?
O8 Ba N11 70.43(8) . . ?
O7 Ba N11 118.99(10) . . ?
O4 Ba N11 124.33(7) 2_556 . ?
O2 Ba N11 69.13(7) 2_556 . ?
O6 Ba N11 146.26(8) . . ?
O5 Ba N11 68.37(9) . . ?
N5 Ba N11 121.36(9) . . ?
O8 Ba O2 101.00(7) . . ?
O7 Ba O2 136.93(9) . . ?
O4 Ba O2 111.68(6) 2_556 . ?
O2 Ba O2 150.665(16) 2_556 . ?
O6 Ba O2 64.10(7) . . ?
O5 Ba O2 79.59(8) . . ?
N5 Ba O2 43.09(7) . . ?
N11 Ba O2 97.12(6) . . ?
O8 Ba O4 66.96(7) . . ?
O7 Ba O4 139.72(9) . . ?
O4 Ba O4 150.673(16) 2_556 . ?
O2 Ba O4 111.70(6) 2_556 . ?
O6 Ba O4 106.64(7) . . ?
O5 Ba O4 79.51(7) . . ?
N5 Ba O4 95.61(7) . . ?
N11 Ba O4 42.70(6) . . ?
O2 Ba O4 57.91(6) . . ?
N6 N5 N1 110.0(3) . . ?
N6 N5 Ba 103.86(19) . . ?
N1 N5 Ba 144.3(2) . . ?
N3 N2 N1 106.0(3) . . ?
N4 C1 N1 108.1(3) . . ?
N4 C1 C1 127.6(4) . 3_557 ?
N1 C1 C1 124.2(4) . 3_557 ?
N12 O4 Ba 128.00(18) . 2_546 ?
N12 O4 Ba 100.23(16) . . ?
Ba O4 Ba 118.91(7) 2_546 . ?
C2 N10 N9 105.3(3) . . ?
O3 N12 O4 122.9(3) . . ?
O3 N12 N11 124.6(3) . . ?
O4 N12 N11 112.5(3) . . ?
N8 N9 N10 111.5(3) . . ?
N2 N3 N4 110.9(3) . . ?
O1 N6 O2 122.3(3) . . ?
O1 N6 N5 125.2(3) . . ?
O2 N6 N5 112.5(3) . . ?
N9 N8 N7 106.0(3) . . ?
N6 O2 Ba 119.51(17) . 2_546 ?
N6 O2 Ba 99.67(16) . . ?
Ba O2 Ba 119.34(7) 2_546 . ?
C1 N4 N3 105.9(3) . . ?
N12 N11 N7 109.8(3) . . ?
N12 N11 Ba 104.60(19) . . ?
N7 N11 Ba 145.57(18) . . ?
C1 N1 N2 109.0(3) . . ?
C1 N1 N5 129.8(3) . . ?
N2 N1 N5 120.8(3) . . ?
C2 N7 N8 108.6(3) . . ?
C2 N7 N11 130.3(3) . . ?
N8 N7 N11 120.7(3) . . ?
N10 C2 N7 108.6(3) . . ?
N10 C2 C2 126.9(4) . 3_656 ?
N7 C2 C2 124.4(4) . 3_656 ?
Ba O5 H5A 117(4) . . ?
Ba O5 H5B 120(4) . . ?
H5A O5 H5B 109(6) . . ?
Ba O6 H6C 110.9 . . ?
Ba O6 H6A 116(4) . . ?
H6C O6 H6A 93.3 . . ?
Ba O8 H8A 118.0 . . ?
Ba O8 H8B 119.4 . . ?
H8A O8 H8B 98.5 . . ?
Ba O7 H7A 117(3) . . ?
Ba O7 H7B 133(4) . . ?
H7A O7 H7B 105(5) . . ?
H9C O9 H9B 131.2 . . ?
H10B O10 H10A 111.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ba O4 N12 O3 41.6(4) 2_546 . . . ?
Ba O4 N12 O3 -178.5(2) . . . . ?
Ba O4 N12 N11 -139.4(2) 2_546 . . . ?
Ba O4 N12 N11 0.5(3) . . . . ?
C2 N10 N9 N8 0.1(3) . . . . ?
N1 N2 N3 N4 -0.7(4) . . . . ?
N1 N5 N6 O1 2.7(5) . . . . ?
Ba N5 N6 O1 171.2(2) . . . . ?
N1 N5 N6 O2 -178.3(2) . . . . ?
Ba N5 N6 O2 -9.7(3) . . . . ?
N10 N9 N8 N7 0.1(3) . . . . ?
O1 N6 O2 Ba -39.8(3) . . . 2_546 ?
N5 N6 O2 Ba 141.1(2) . . . 2_546 ?
O1 N6 O2 Ba -171.7(2) . . . . ?
N5 N6 O2 Ba 9.2(3) . . . . ?
N1 C1 N4 N3 0.8(4) . . . . ?
C1 C1 N4 N3 -178.7(4) 3_557 . . . ?
N2 N3 N4 C1 -0.1(4) . . . . ?
O3 N12 N11 N7 -1.1(4) . . . . ?
O4 N12 N11 N7 180.0(2) . . . . ?
O3 N12 N11 Ba 178.4(2) . . . . ?
O4 N12 N11 Ba -0.5(3) . . . . ?
N4 C1 N1 N2 -1.2(4) . . . . ?
C1 C1 N1 N2 178.3(4) 3_557 . . . ?
N4 C1 N1 N5 -174.5(3) . . . . ?
C1 C1 N1 N5 5.0(6) 3_557 . . . ?
N3 N2 N1 C1 1.1(3) . . . . ?
N3 N2 N1 N5 175.1(3) . . . . ?
N6 N5 N1 C1 -86.4(4) . . . . ?
Ba N5 N1 C1 112.9(4) . . . . ?
N6 N5 N1 N2 101.1(3) . . . . ?
Ba N5 N1 N2 -59.7(5) . . . . ?
N9 N8 N7 C2 -0.2(3) . . . . ?
N9 N8 N7 N11 -173.7(3) . . . . ?
N12 N11 N7 C2 83.6(4) . . . . ?
Ba N11 N7 C2 -95.6(4) . . . . ?
N12 N11 N7 N8 -104.5(3) . . . . ?
Ba N11 N7 N8 76.3(4) . . . . ?
N9 N10 C2 N7 -0.2(3) . . . . ?
N9 N10 C2 C2 179.8(4) . . . 3_656 ?
N8 N7 C2 N10 0.3(4) . . . . ?
N11 N7 C2 N10 173.0(3) . . . . ?
N8 N7 C2 C2 -179.7(4) . . . 3_656 ?
N11 N7 C2 C2 -7.1(6) . . . 3_656 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
O9 H9B O3 0.95 2.49 3.261(4) 138.6 1_455
O10 H10B O9 0.88 1.83 2.673(5) 161.3 2_556
O8 H8A N10 0.87 2.06 2.904(4) 165.7 3_656
O10 H10A O6 0.70 2.23 2.811(5) 140.4 2_556
O8 H8B O9 0.83 1.95 2.773(4) 171.4 .
O6 H6C N4 0.90 2.10 2.995(4) 171.7 3_557
O5 H5A N2 0.85(6) 2.51(6) 3.295(5) 153(5) .
O5 H5B O10 0.78(6) 2.03(6) 2.783(6) 165(6) .
O6 H6A O10 0.77(6) 2.15(6) 2.905(4) 166(5) 1_455
O7 H7A N9 0.93(5) 2.19(5) 2.969(4) 141(4) 1_455
O7 H7A N3 0.93(5) 2.60(5) 3.232(4) 126(4) 4_565
O7 H7B O5 0.78(5) 2.08(5) 2.849(4) 167(5) 2_556

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.803
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.366

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx413
_database_code_depnum_ccdc_archive 'CCDC 1510458'
_audit_update_record             
;
2016-10-18 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Sep 08 16:19:15 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
hexaammine nickel(II) 1,1-dinitramino-5,5-bitetrazolate
;
_chemical_name_common            
'hexaammine nickel(II) 1,1-dinitramino-5,5-bitetrazolate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         '	C2 N12 O4, H18 N6 Ni'
_chemical_formula_sum            'C2 H18 N18 Ni O4'
_chemical_formula_weight         417.05



_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'


_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.
;

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'

_cell_length_a                   13.5062(12)
_cell_length_b                   11.5426(8)
_cell_length_c                   10.4455(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.176(7)
_cell_angle_gamma                90
_cell_volume                     1621.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1134
_cell_measurement_theta_min      4.2740
_cell_measurement_theta_max      23.7470

_exptl_crystal_description       rod
_exptl_crystal_colour            'clear light purple'
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    1.255
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99040
_exptl_absorpt_correction_T_max  1.00000
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            7466
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.2088
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.148
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             2837
_reflns_number_gt                1838
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0111P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2837
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      -0.0277269000
_diffrn_orient_matrix_UB_12      0.0099222000
_diffrn_orient_matrix_UB_13      0.0534609000
_diffrn_orient_matrix_UB_21      -0.0448632000
_diffrn_orient_matrix_UB_22      -0.0056294000
_diffrn_orient_matrix_UB_23      -0.0404303000
_diffrn_orient_matrix_UB_31      -0.0003518000
_diffrn_orient_matrix_UB_32      -0.0603646000
_diffrn_orient_matrix_UB_33      0.0125635000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000    0.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega  -65.00   39.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000   80.0000  250.0000 104

;



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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4597(3) 0.2816(3) 0.1387(3) 0.0448(10) Uani 1 1 d . . . . .
O2 O 0.5005(3) 0.3183(3) 0.3423(3) 0.0448(10) Uani 1 1 d . . . . .
N1 N 0.5981(3) 0.4004(3) 0.0703(4) 0.0300(10) Uani 1 1 d . . . . .
N2 N 0.6698(3) 0.3489(3) 0.0111(4) 0.0339(10) Uani 1 1 d . . . . .
N3 N 0.6576(3) 0.3838(4) -0.1081(4) 0.0392(11) Uani 1 1 d . . . . .
N4 N 0.5793(3) 0.4566(4) -0.1280(4) 0.0384(11) Uani 1 1 d . . . . .
N5 N 0.5954(3) 0.3897(4) 0.2031(4) 0.0363(11) Uani 1 1 d . . . . .
N6 N 0.5155(3) 0.3265(4) 0.2261(4) 0.0355(11) Uani 1 1 d . . . . .
C1 C 0.5428(3) 0.4660(4) -0.0146(4) 0.0274(11) Uani 1 1 d . . . . .
O3 O 0.0620(3) 0.7299(3) 0.9021(3) 0.0435(10) Uani 1 1 d . . . . .
O4 O -0.0273(3) 0.7569(3) 0.7177(4) 0.0569(11) Uani 1 1 d . . . . .
N7 N 0.0764(3) 0.5196(3) 0.8629(3) 0.0251(9) Uani 1 1 d . . . . .
N8 N 0.1665(3) 0.4737(4) 0.8497(4) 0.0325(10) Uani 1 1 d . . . . .
N9 N 0.1900(3) 0.4124(4) 0.9530(4) 0.0361(11) Uani 1 1 d . . . . .
N10 N 0.1169(3) 0.4180(3) 1.0344(4) 0.0331(10) Uani 1 1 d . . . . .
N11 N 0.0256(3) 0.5811(3) 0.7628(4) 0.0328(10) Uani 1 1 d . . . . .
N12 N 0.0209(3) 0.6927(4) 0.7980(4) 0.0372(11) Uani 1 1 d . . . . .
C2 C 0.0470(3) 0.4848(4) 0.9759(4) 0.0243(11) Uani 1 1 d . . . . .
Ni1 Ni 0.24600(5) 0.48105(5) 0.46866(6) 0.0271(2) Uani 1 1 d . . . . .
N13 N 0.2147(3) 0.6253(3) 0.5835(3) 0.0276(10) Uani 1 1 d . . . . .
H13A H 0.2124 0.6906 0.5346 0.041 Uiso 1 1 calc R U . . .
H13B H 0.2633 0.6325 0.6493 0.041 Uiso 1 1 calc R U . . .
H13C H 0.1551 0.6146 0.6159 0.041 Uiso 1 1 calc R U . . .
N14 N 0.3210(3) 0.4058(3) 0.6364(3) 0.0358(11) Uani 1 1 d . . . . .
H14A H 0.3618 0.4595 0.6774 0.054 Uiso 1 1 calc R U . . .
H14B H 0.3576 0.3442 0.6137 0.054 Uiso 1 1 calc R U . . .
H14C H 0.2755 0.3817 0.6899 0.054 Uiso 1 1 calc R U . . .
N15 N 0.3816(3) 0.5582(3) 0.4264(3) 0.0346(10) Uani 1 1 d . . . . .
H15A H 0.4237 0.5023 0.4023 0.052 Uiso 1 1 calc R U . . .
H15B H 0.4098 0.5952 0.4974 0.052 Uiso 1 1 calc R U . . .
H15C H 0.3696 0.6101 0.3613 0.052 Uiso 1 1 calc R U . . .
N16 N 0.2746(3) 0.3329(4) 0.3570(4) 0.0517(13) Uani 1 1 d . . . . .
H16A H 0.2362 0.3358 0.2809 0.078 Uiso 1 1 calc R U . . .
H16B H 0.2599 0.2677 0.4005 0.078 Uiso 1 1 calc R U . . .
H16C H 0.3399 0.3319 0.3419 0.078 Uiso 1 1 calc R U . . .
N17 N 0.1719(3) 0.5597(3) 0.3061(3) 0.0360(11) Uani 1 1 d . . . . .
H17A H 0.1367 0.6217 0.3309 0.054 Uiso 1 1 calc R U . . .
H17B H 0.1297 0.5077 0.2646 0.054 Uiso 1 1 calc R U . . .
H17C H 0.2171 0.5837 0.2524 0.054 Uiso 1 1 calc R U . . .
N18 N 0.1093(3) 0.4023(3) 0.5154(4) 0.0427(12) Uani 1 1 d . . . . .
H18A H 0.0683 0.4578 0.5430 0.064 Uiso 1 1 calc R U . . .
H18B H 0.1226 0.3488 0.5786 0.064 Uiso 1 1 calc R U . . .
H18C H 0.0791 0.3671 0.4443 0.064 Uiso 1 1 calc R U . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N6 1.243(5) . ?
O2 N6 1.252(4) . ?
N1 N2 1.335(5) . ?
N1 C1 1.341(6) . ?
N1 N5 1.397(5) . ?
N2 N3 1.306(5) . ?
N3 N4 1.352(5) . ?
N4 C1 1.328(5) . ?
N5 N6 1.343(5) . ?
C1 C1 1.452(9) 3_665 ?
O3 N12 1.252(5) . ?
O4 N12 1.256(5) . ?
N7 C2 1.341(5) . ?
N7 N8 1.346(5) . ?
N7 N11 1.392(5) . ?
N8 N9 1.306(5) . ?
N9 N10 1.361(5) . ?
N10 C2 1.325(5) . ?
N11 N12 1.343(5) . ?
C2 C2 1.451(8) 3_567 ?
Ni1 N17 2.098(4) . ?
Ni1 N13 2.116(3) . ?
Ni1 N15 2.119(3) . ?
Ni1 N16 2.124(4) . ?
Ni1 N14 2.128(4) . ?
Ni1 N18 2.154(4) . ?
N13 H13A 0.9100 . ?
N13 H13B 0.9100 . ?
N13 H13C 0.9100 . ?
N14 H14A 0.9100 . ?
N14 H14B 0.9100 . ?
N14 H14C 0.9100 . ?
N15 H15A 0.9100 . ?
N15 H15B 0.9100 . ?
N15 H15C 0.9100 . ?
N16 H16A 0.9100 . ?
N16 H16B 0.9100 . ?
N16 H16C 0.9100 . ?
N17 H17A 0.9100 . ?
N17 H17B 0.9100 . ?
N17 H17C 0.9100 . ?
N18 H18A 0.9100 . ?
N18 H18B 0.9100 . ?
N18 H18C 0.9100 . ?

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
_geom_angle_publ_flag
N2 N1 C1 109.3(4) . . ?
N2 N1 N5 120.3(4) . . ?
C1 N1 N5 130.1(4) . . ?
N3 N2 N1 105.6(4) . . ?
N2 N3 N4 111.6(4) . . ?
C1 N4 N3 105.2(4) . . ?
N6 N5 N1 108.6(4) . . ?
O1 N6 O2 122.7(4) . . ?
O1 N6 N5 122.6(4) . . ?
O2 N6 N5 114.7(4) . . ?
N4 C1 N1 108.3(4) . . ?
N4 C1 C1 126.7(6) . 3_665 ?
N1 C1 C1 124.9(5) . 3_665 ?
C2 N7 N8 108.3(4) . . ?
C2 N7 N11 130.5(4) . . ?
N8 N7 N11 120.9(4) . . ?
N9 N8 N7 106.4(4) . . ?
N8 N9 N10 110.8(4) . . ?
C2 N10 N9 105.4(4) . . ?
N12 N11 N7 108.4(4) . . ?
O3 N12 O4 122.7(4) . . ?
O3 N12 N11 122.6(4) . . ?
O4 N12 N11 114.7(4) . . ?
N10 C2 N7 109.0(4) . . ?
N10 C2 C2 126.2(5) . 3_567 ?
N7 C2 C2 124.8(5) . 3_567 ?
N17 Ni1 N13 90.76(15) . . ?
N17 Ni1 N15 90.45(15) . . ?
N13 Ni1 N15 90.46(14) . . ?
N17 Ni1 N16 90.06(17) . . ?
N13 Ni1 N16 178.18(15) . . ?
N15 Ni1 N16 91.16(15) . . ?
N17 Ni1 N14 178.36(15) . . ?
N13 Ni1 N14 87.63(14) . . ?
N15 Ni1 N14 89.25(15) . . ?
N16 Ni1 N14 91.56(17) . . ?
N17 Ni1 N18 90.55(16) . . ?
N13 Ni1 N18 89.11(14) . . ?
N15 Ni1 N18 178.91(16) . . ?
N16 Ni1 N18 89.26(15) . . ?
N14 Ni1 N18 89.73(16) . . ?
Ni1 N13 H13A 109.5 . . ?
Ni1 N13 H13B 109.5 . . ?
H13A N13 H13B 109.5 . . ?
Ni1 N13 H13C 109.5 . . ?
H13A N13 H13C 109.5 . . ?
H13B N13 H13C 109.5 . . ?
Ni1 N14 H14A 109.5 . . ?
Ni1 N14 H14B 109.5 . . ?
H14A N14 H14B 109.5 . . ?
Ni1 N14 H14C 109.5 . . ?
H14A N14 H14C 109.5 . . ?
H14B N14 H14C 109.5 . . ?
Ni1 N15 H15A 109.5 . . ?
Ni1 N15 H15B 109.5 . . ?
H15A N15 H15B 109.5 . . ?
Ni1 N15 H15C 109.5 . . ?
H15A N15 H15C 109.5 . . ?
H15B N15 H15C 109.5 . . ?
Ni1 N16 H16A 109.5 . . ?
Ni1 N16 H16B 109.5 . . ?
H16A N16 H16B 109.5 . . ?
Ni1 N16 H16C 109.5 . . ?
H16A N16 H16C 109.5 . . ?
H16B N16 H16C 109.5 . . ?
Ni1 N17 H17A 109.5 . . ?
Ni1 N17 H17B 109.5 . . ?
H17A N17 H17B 109.5 . . ?
Ni1 N17 H17C 109.5 . . ?
H17A N17 H17C 109.5 . . ?
H17B N17 H17C 109.5 . . ?
Ni1 N18 H18A 109.5 . . ?
Ni1 N18 H18B 109.5 . . ?
H18A N18 H18B 109.5 . . ?
Ni1 N18 H18C 109.5 . . ?
H18A N18 H18C 109.5 . . ?
H18B N18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 0.3(5) . . . . ?
N5 N1 N2 N3 -174.1(4) . . . . ?
N1 N2 N3 N4 -0.3(5) . . . . ?
N2 N3 N4 C1 0.2(5) . . . . ?
N2 N1 N5 N6 -112.1(4) . . . . ?
C1 N1 N5 N6 74.9(6) . . . . ?
N1 N5 N6 O1 4.0(6) . . . . ?
N1 N5 N6 O2 -174.6(4) . . . . ?
N3 N4 C1 N1 0.0(5) . . . . ?
N3 N4 C1 C1 -179.4(6) . . . 3_665 ?
N2 N1 C1 N4 -0.1(5) . . . . ?
N5 N1 C1 N4 173.5(4) . . . . ?
N2 N1 C1 C1 179.2(5) . . . 3_665 ?
N5 N1 C1 C1 -7.1(9) . . . 3_665 ?
C2 N7 N8 N9 0.2(5) . . . . ?
N11 N7 N8 N9 -173.7(4) . . . . ?
N7 N8 N9 N10 -0.4(5) . . . . ?
N8 N9 N10 C2 0.4(5) . . . . ?
C2 N7 N11 N12 75.2(6) . . . . ?
N8 N7 N11 N12 -112.3(4) . . . . ?
N7 N11 N12 O3 3.6(6) . . . . ?
N7 N11 N12 O4 -177.0(4) . . . . ?
N9 N10 C2 N7 -0.3(5) . . . . ?
N9 N10 C2 C2 179.0(6) . . . 3_567 ?
N8 N7 C2 N10 0.0(5) . . . . ?
N11 N7 C2 N10 173.2(4) . . . . ?
N8 N7 C2 C2 -179.2(5) . . . 3_567 ?
N11 N7 C2 C2 -6.0(9) . . . 3_567 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
N13 H13A N2 0.91 2.50 3.217(5) 136.3 2_655
N13 H13A O3 0.91 2.52 3.151(5) 126.5 4_575
N13 H13B N5 0.91 2.36 3.247(5) 165.9 3_666
N13 H13C N11 0.91 2.46 3.341(5) 163.1 .
N14 H14A N5 0.91 2.19 3.052(6) 157.9 3_666
N14 H14B O1 0.91 2.00 2.861(5) 156.4 4_566
N14 H14C N8 0.91 2.55 3.281(5) 137.2 .
N15 H15A O2 0.91 2.47 3.356(5) 165.2 .
N15 H15B O2 0.91 2.21 3.117(5) 171.5 3_666
N15 H15C N3 0.91 2.64 3.386(6) 140.0 3_665
N16 H16B N9 0.91 2.37 3.246(6) 162.0 4_565
N16 H16C O2 0.91 2.17 3.073(6) 169.4 .
N17 H17A O3 0.91 2.15 3.061(5) 175.5 4_575
N17 H17A N12 0.91 2.66 3.508(6) 156.1 4_575
N17 H17B N10 0.91 2.61 3.302(5) 133.5 1_554
N17 H17B N11 0.91 2.33 3.150(6) 150.1 3_566
N17 H17C N3 0.91 2.39 3.296(5) 171.2 3_665
N18 H18C O4 0.91 2.28 3.169(5) 166.4 3_566
N18 H18C N11 0.91 2.55 3.293(6) 139.6 3_566
N13 H13A N2 0.91 2.50 3.217(5) 136.3 2_655
N13 H13A O3 0.91 2.52 3.151(5) 126.5 4_575
N13 H13B N5 0.91 2.36 3.247(5) 165.9 3_666
N13 H13C N11 0.91 2.46 3.341(5) 163.1 .
N14 H14A N5 0.91 2.19 3.052(6) 157.9 3_666
N14 H14B O1 0.91 2.00 2.861(5) 156.4 4_566
N14 H14C N8 0.91 2.55 3.281(5) 137.2 .
N15 H15A O2 0.91 2.47 3.356(5) 165.2 .
N15 H15B O2 0.91 2.21 3.117(5) 171.5 3_666
N15 H15C N3 0.91 2.64 3.386(6) 140.0 3_665
N16 H16B N9 0.91 2.37 3.246(6) 162.0 4_565
N16 H16C O2 0.91 2.17 3.073(6) 169.4 .
N17 H17A O3 0.91 2.15 3.061(5) 175.5 4_575
N17 H17A N12 0.91 2.66 3.508(6) 156.1 4_575
N17 H17B N10 0.91 2.61 3.302(5) 133.5 1_554
N17 H17B N11 0.91 2.33 3.150(6) 150.1 3_566
N17 H17C N3 0.91 2.39 3.296(5) 171.2 3_665
N18 H18C O4 0.91 2.28 3.169(5) 166.4 3_566
N18 H18C N11 0.91 2.55 3.293(6) 139.6 3_566

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.812
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.086

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_uv285
_database_code_depnum_ccdc_archive 'CCDC 1502966'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             08.06.2016
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
'dimethyl 2,2-(1,2-diazidoethane-1,2-diylidene)bis(hydrazinecarboxylate)'
_chemical_name_common            
'dimethyl 2,2-(1,2-diazidoethane-1,2-diylidene)bis(hydrazinecarboxylate)'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H8 N10 O4'
_chemical_formula_sum            'C6 H8 N10 O4'
_chemical_formula_weight         284.22

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        P-1
_space_group_name_Hall           '-P 1'


_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.1866(7)
_cell_length_b                   7.2348(10)
_cell_length_c                   10.3368(13)
_cell_angle_alpha                81.092(5)
_cell_angle_beta                 83.309(6)
_cell_angle_gamma                75.044(6)
_cell_volume                     297.88(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1761
_cell_measurement_theta_min      2.9392
_cell_measurement_theta_max      28.1990

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.134
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_F_000             146
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode generator'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            3156
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.334
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1159
_reflns_number_gt                880
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0457P)²+0.1107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1159
_refine_ls_number_parameters     96
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  ?
_diffrn_measurement_device       ?

_diffrn_detector                 ?
_diffrn_detector_type            ?



_diffrn_orient_matrix_UB_11      ?
_diffrn_orient_matrix_UB_12      ?
_diffrn_orient_matrix_UB_13      ?
_diffrn_orient_matrix_UB_21      ?
_diffrn_orient_matrix_UB_22      ?
_diffrn_orient_matrix_UB_23      ?
_diffrn_orient_matrix_UB_31      ?
_diffrn_orient_matrix_UB_32      ?
_diffrn_orient_matrix_UB_33      ?
_diffrn_measurement_details      ?



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'
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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4581(4) 0.0262(2) 0.33507(14) 0.0286(4) Uani 1 1 d . . . . .
O2 O 0.6122(4) 0.2782(2) 0.21065(14) 0.0300(4) Uani 1 1 d . . . . .
N1 N 0.8779(5) 0.3103(3) 0.63183(17) 0.0284(5) Uani 1 1 d . . . . .
N2 N 0.9990(5) 0.3308(2) 0.73122(19) 0.0310(5) Uani 1 1 d . . . . .
N3 N 1.0870(6) 0.3252(3) 0.8309(2) 0.0459(6) Uani 1 1 d . . . . .
N4 N 0.8326(4) 0.3712(2) 0.40732(17) 0.0220(4) Uani 1 1 d . . . . .
N5 N 0.6929(4) 0.2174(2) 0.42582(18) 0.0239(4) Uani 1 1 d . . . . .
C1 C 0.9261(5) 0.4168(3) 0.50926(19) 0.0208(5) Uani 1 1 d . . . . .
C5 C 0.5790(5) 0.1641(3) 0.3233(2) 0.0224(5) Uani 1 1 d . . . . .
C10 C 0.4838(7) 0.2282(4) 0.1011(2) 0.0396(6) Uani 1 1 d . . . . .
H10A H 0.5978 0.0957 0.0867 0.059 Uiso 1 1 calc R U . . .
H10B H 0.5205 0.3168 0.0222 0.059 Uiso 1 1 calc R U . . .
H10C H 0.2455 0.2380 0.1199 0.059 Uiso 1 1 calc R U . . .
H5 H 0.658(7) 0.152(4) 0.505(3) 0.053(8) Uiso 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C5 1.214(2) . ?
O2 C5 1.334(2) . ?
O2 C10 1.439(3) . ?
N1 N2 1.242(2) . ?
N1 C1 1.399(3) . ?
N2 N3 1.126(3) . ?
N4 C1 1.282(3) . ?
N4 N5 1.364(2) . ?
N5 C5 1.356(3) . ?
N5 H5 0.89(3) . ?
C1 C1 1.468(4) 2_766 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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
_geom_angle_publ_flag
C5 O2 C10 114.39(16) . . ?
N2 N1 C1 122.53(17) . . ?
N3 N2 N1 168.7(2) . . ?
C1 N4 N5 116.92(17) . . ?
C5 N5 N4 120.30(17) . . ?
C5 N5 H5 116.3(18) . . ?
N4 N5 H5 123.2(18) . . ?
N4 C1 N1 119.35(18) . . ?
N4 C1 C1 117.4(2) . 2_766 ?
N1 C1 C1 123.2(2) . 2_766 ?
O1 C5 O2 124.29(18) . . ?
O1 C5 N5 122.40(19) . . ?
O2 C5 N5 113.32(17) . . ?
O2 C10 H10A 109.5 . . ?
O2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -176.1(11) . . . . ?
C1 N4 N5 C5 178.05(18) . . . . ?
N5 N4 C1 N1 -0.7(3) . . . . ?
N5 N4 C1 C1 -179.4(2) . . . 2_766 ?
N2 N1 C1 N4 170.7(2) . . . . ?
N2 N1 C1 C1 -10.6(4) . . . 2_766 ?
C10 O2 C5 O1 1.5(3) . . . . ?
C10 O2 C5 N5 -178.18(18) . . . . ?
N4 N5 C5 O1 178.71(18) . . . . ?
N4 N5 C5 O2 -1.6(3) . . . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
N5 H5 O1 0.89(3) 2.03(3) 2.912(2) 169(3) 2_656
N5 H5 O1 0.89(3) 2.03(3) 2.912(2) 169(3) 2_656

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.215
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx129
_database_code_depnum_ccdc_archive 'CCDC 1500005'
_audit_update_record             
;
2016-08-19 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Mar 11 16:36:00 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
lithium dinitramino-5,5-bitetrazolate monohydrate
;
_chemical_name_common            
'lithium dinitramino-5,5-bitetrazolate monohydrate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C H2 Li N6 O3'
_chemical_formula_sum            'C H2 Li N6 O3'
_chemical_formula_weight         153.03

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'


_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.
;

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'

_cell_length_a                   8.2760(9)
_cell_length_b                   10.8140(8)
_cell_length_c                   6.0650(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.073(10)
_cell_angle_gamma                90
_cell_volume                     521.58(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1023
_cell_measurement_theta_min      4.5570
_cell_measurement_theta_max      31.4320

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.176
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84687
_exptl_absorpt_correction_T_max  0.99999
_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_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            3905
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.169
_diffrn_reflns_theta_max         26.746
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1105
_reflns_number_gt                893
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0311P)²+0.1742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1105
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_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_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

;



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_
_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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
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_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.257
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.054

_shelxl_version_number           2013-4


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lx406
_database_code_depnum_ccdc_archive 'CCDC 1502967'
_audit_update_record             
;
2016-09-06 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Sep 02 12:08:28 2016'
;
_audit_creation_method           SHELXL-2013


_chemical_name_systematic        
;
disilver 1,1-dinitramino-5,5-bitetrazolate
;
_chemical_name_common            'disilver 1,1-dinitramino-5,5-bitetrazolate'
_chemical_compound_source        ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 Ag2 N12 O4'
_chemical_formula_weight         471.88

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P  2/c'
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'




_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   6.7520(4)
_cell_length_b                   5.0649(4)
_cell_length_c                   14.1529(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.180(6)
_cell_angle_gamma                90
_cell_volume                     483.65(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    760
_cell_measurement_theta_min      5.0150
_cell_measurement_theta_max      33.0050

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0200
_exptl_absorpt_coefficient_mu    4.097
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73327
_exptl_absorpt_correction_T_max  0.99999
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.240
_exptl_crystal_F_000             444
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?



_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_reflns_number            2377
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.274
_diffrn_reflns_theta_max         25.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             955
_reflns_number_gt                761
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+1.8998P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?

_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         955
_refine_ls_number_parameters     93
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3



_diffrn_orient_matrix_UB_11      0.0145195000
_diffrn_orient_matrix_UB_12      -0.1177094000
_diffrn_orient_matrix_UB_13      0.0265533000
_diffrn_orient_matrix_UB_21      -0.1030937000
_diffrn_orient_matrix_UB_22      -0.0266455000
_diffrn_orient_matrix_UB_23      -0.0042729000
_diffrn_orient_matrix_UB_31      0.0146690000
_diffrn_orient_matrix_UB_32      -0.0710944000
_diffrn_orient_matrix_UB_33      -0.0423144000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000    0.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega  -65.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000   80.0000  250.0000 104

;



loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.8971 1.1015 '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'
C C 0.0033 0.0016 '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'


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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.0000 0.01400(11) 0.2500 0.01764(19) Uani 1 2 d S T P . .
Ag2 Ag 0.0000 0.0000 0.0000 0.0490(3) Uani 1 2 d S . P . .
N3 N 0.2667(6) 0.1653(9) 0.0798(3) 0.0160(10) Uani 1 1 d . . . . .
N4 N 0.2744(6) 0.1468(8) 0.1757(3) 0.0139(9) Uani 1 1 d . . . . .
C1 C 0.4589(7) 0.2032(10) 0.2020(4) 0.0129(11) Uani 1 1 d . . . . .
N1 N 0.5584(6) 0.2541(8) 0.1241(3) 0.0107(9) Uani 1 1 d . . . . .
N2 N 0.4362(6) 0.2303(9) 0.0475(3) 0.0161(9) Uani 1 1 d . . . . .
N5 N 0.7609(6) 0.3039(8) 0.1125(3) 0.0154(10) Uani 1 1 d . . . . .
N6 N 0.8004(7) 0.5521(8) 0.1415(3) 0.0153(10) Uani 1 1 d . . . . .
O2 O 0.9767(5) 0.6227(8) 0.1319(3) 0.0219(9) Uani 1 1 d . . . . .
O1 O 0.6753(6) 0.6950(7) 0.1774(3) 0.0251(9) Uani 1 1 d . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N4 2.267(4) . ?
Ag1 N4 2.267(4) 2 ?
Ag1 O2 2.593(4) 1_445 ?
Ag1 O2 2.593(4) 2_645 ?
Ag2 N3 2.251(4) 3 ?
Ag2 N3 2.251(4) . ?
N3 N2 1.291(6) . ?
N3 N4 1.359(6) . ?
N4 C1 1.318(6) . ?
C1 N1 1.338(6) . ?
C1 C1 1.447(10) 2_655 ?
N1 N2 1.343(6) . ?
N1 N5 1.406(5) . ?
N5 N6 1.346(6) . ?
N6 O1 1.237(5) . ?
N6 O2 1.255(5) . ?
O2 Ag1 2.593(4) 1_665 ?

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
_geom_angle_publ_flag
N4 Ag1 N4 145.5(2) . 2 ?
N4 Ag1 O2 87.61(13) . 1_445 ?
N4 Ag1 O2 119.67(13) 2 1_445 ?
N4 Ag1 O2 119.67(13) . 2_645 ?
N4 Ag1 O2 87.61(13) 2 2_645 ?
O2 Ag1 O2 80.35(17) 1_445 2_645 ?
N3 Ag2 N3 180.0 3 . ?
N2 N3 N4 111.8(4) . . ?
N2 N3 Ag2 128.3(3) . . ?
N4 N3 Ag2 118.4(3) . . ?
C1 N4 N3 105.5(4) . . ?
C1 N4 Ag1 135.5(4) . . ?
N3 N4 Ag1 118.8(3) . . ?
N4 C1 N1 107.9(4) . . ?
N4 C1 C1 126.1(6) . 2_655 ?
N1 C1 C1 126.0(6) . 2_655 ?
C1 N1 N2 109.6(4) . . ?
C1 N1 N5 130.7(4) . . ?
N2 N1 N5 119.5(4) . . ?
N3 N2 N1 105.2(4) . . ?
N6 N5 N1 108.3(4) . . ?
O1 N6 O2 122.9(4) . . ?
O1 N6 N5 122.8(4) . . ?
O2 N6 N5 114.3(4) . . ?
N6 O2 Ag1 100.5(3) . 1_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 N3 N4 C1 -0.2(6) . . . . ?
Ag2 N3 N4 C1 166.7(3) . . . . ?
N2 N3 N4 Ag1 -176.8(3) . . . . ?
Ag2 N3 N4 Ag1 -9.9(5) . . . . ?
N3 N4 C1 N1 0.0(5) . . . . ?
Ag1 N4 C1 N1 175.8(3) . . . . ?
N3 N4 C1 C1 -178.4(3) . . . 2_655 ?
Ag1 N4 C1 C1 -2.7(6) . . . 2_655 ?
N4 C1 N1 N2 0.1(6) . . . . ?
C1 C1 N1 N2 178.6(3) 2_655 . . . ?
N4 C1 N1 N5 -174.4(5) . . . . ?
C1 C1 N1 N5 4.0(7) 2_655 . . . ?
N4 N3 N2 N1 0.2(5) . . . . ?
Ag2 N3 N2 N1 -165.0(3) . . . . ?
C1 N1 N2 N3 -0.2(5) . . . . ?
N5 N1 N2 N3 175.1(4) . . . . ?
C1 N1 N5 N6 -75.8(6) . . . . ?
N2 N1 N5 N6 110.1(5) . . . . ?
N1 N5 N6 O1 4.3(6) . . . . ?
N1 N5 N6 O2 -178.0(4) . . . . ?
O1 N6 O2 Ag1 17.8(5) . . . 1_665 ?
N5 N6 O2 Ag1 -159.9(3) . . . 1_665 ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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
? ? ? ? ? ? ? ?

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;



_refine_diff_density_max         0.849
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.151

_shelxl_version_number           2013-4


