# 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_140605f
_database_code_depnum_ccdc_archive 'CCDC 1018900'
_audit_update_record             
;
2014-08-11 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C H3 N4 Na O2'
_chemical_formula_weight         126.06

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   3.5385(2)
_cell_length_b                   15.1510(12)
_cell_length_c                   8.3696(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.465(2)
_cell_angle_gamma                90.00
_cell_volume                     447.35(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1566
_cell_measurement_theta_min      2.689
_cell_measurement_theta_max      28.136

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             256
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8919
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2125
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         24.97
_reflns_number_total             782
_reflns_number_gt                691
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0699P)²+0.2405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.15(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         782
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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
Na1 Na 0.2255(3) 0.42613(5) 0.37522(10) 0.0256(4) Uani 1 1 d . . .
N1 N 0.2047(6) 0.72366(12) 0.3236(2) 0.0229(5) Uani 1 1 d . . .
H1 H 0.1212 0.7506 0.4041 0.027 Uiso 1 1 calc R . .
N2 N 0.2863(6) 0.76264(13) 0.1850(2) 0.0262(6) Uani 1 1 d . . .
N3 N 0.4026(6) 0.70013(12) 0.0963(2) 0.0268(6) Uani 1 1 d . . .
N4 N 0.4002(6) 0.62159(12) 0.1711(2) 0.0250(6) Uani 1 1 d . . .
O1 O 0.2320(5) 0.58149(9) 0.42738(19) 0.0249(5) Uani 1 1 d . . .
O2 O -0.2939(5) 0.44866(11) 0.1795(2) 0.0319(6) Uani 1 1 d . . .
H2A H -0.3054 0.4101 0.1055 0.038 Uiso 1 1 d R . .
H2B H -0.2991 0.5003 0.1398 0.038 Uiso 1 1 d R . .
C1 C 0.2737(6) 0.63628(14) 0.3168(2) 0.0204(6) Uani 1 1 d . . .


_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. 
;

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
Na1 O2 2.3896(19) . ?
Na1 O1 2.3938(17) . ?
Na1 O1 2.4042(19) 3_566 ?
Na1 O1 2.4360(19) 3_666 ?
Na1 O2 2.475(2) 1_655 ?
Na1 N2 2.527(2) 2_545 ?
Na1 Na1 3.5271(17) 3_566 ?
Na1 Na1 3.5376(17) 3_666 ?
Na1 Na1 3.5385(2) 1_455 ?
Na1 Na1 3.5385(2) 1_655 ?
N1 C1 1.348(3) . ?
N1 N2 1.353(3) . ?
N1 H1 0.8600 . ?
N2 N3 1.290(3) . ?
N2 Na1 2.527(2) 2 ?
N3 N4 1.345(3) . ?
N4 C1 1.349(3) . ?
O1 C1 1.261(3) . ?
O1 Na1 2.4042(19) 3_566 ?
O1 Na1 2.4360(19) 3_666 ?
O2 Na1 2.475(2) 1_455 ?
O2 H2A 0.8500 . ?
O2 H2B 0.8501 . ?

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
O2 Na1 O1 88.88(7) . . ?
O2 Na1 O1 87.41(7) . 3_566 ?
O1 Na1 O1 85.37(6) . 3_566 ?
O2 Na1 O1 174.40(6) . 3_666 ?
O1 Na1 O1 85.82(6) . 3_666 ?
O1 Na1 O1 93.95(6) 3_566 3_666 ?
O2 Na1 O2 93.32(6) . 1_655 ?
O1 Na1 O2 89.30(6) . 1_655 ?
O1 Na1 O2 174.60(6) 3_566 1_655 ?
O1 Na1 O2 84.82(6) 3_666 1_655 ?
O2 Na1 N2 90.20(7) . 2_545 ?
O1 Na1 N2 178.96(7) . 2_545 ?
O1 Na1 N2 95.07(6) 3_566 2_545 ?
O1 Na1 N2 95.09(6) 3_666 2_545 ?
O2 Na1 N2 90.27(7) 1_655 2_545 ?
O2 Na1 Na1 87.47(5) . 3_566 ?
O1 Na1 Na1 42.80(4) . 3_566 ?
O1 Na1 Na1 42.57(4) 3_566 3_566 ?
O1 Na1 Na1 89.85(5) 3_666 3_566 ?
O2 Na1 Na1 132.09(6) 1_655 3_566 ?
N2 Na1 Na1 137.63(6) 2_545 3_566 ?
O2 Na1 Na1 132.23(6) . 3_666 ?
O1 Na1 Na1 43.37(5) . 3_666 ?
O1 Na1 Na1 89.59(5) 3_566 3_666 ?
O1 Na1 Na1 42.44(4) 3_666 3_666 ?
O2 Na1 Na1 85.96(5) 1_655 3_666 ?
N2 Na1 Na1 137.53(6) 2_545 3_666 ?
Na1 Na1 Na1 60.11(3) 3_566 3_666 ?
O2 Na1 Na1 44.29(5) . 1_455 ?
O1 Na1 Na1 89.73(5) . 1_455 ?
O1 Na1 Na1 43.38(4) 3_566 1_455 ?
O1 Na1 Na1 137.33(4) 3_666 1_455 ?
O2 Na1 Na1 137.61(4) 1_655 1_455 ?
N2 Na1 Na1 89.94(5) 2_545 1_455 ?
Na1 Na1 Na1 60.09(3) 3_566 1_455 ?
Na1 Na1 Na1 120.21(3) 3_666 1_455 ?
O2 Na1 Na1 135.71(5) . 1_655 ?
O1 Na1 Na1 90.27(5) . 1_655 ?
O1 Na1 Na1 136.62(4) 3_566 1_655 ?
O1 Na1 Na1 42.67(4) 3_666 1_655 ?
O2 Na1 Na1 42.39(4) 1_655 1_655 ?
N2 Na1 Na1 90.06(5) 2_545 1_655 ?
Na1 Na1 Na1 119.91(3) 3_566 1_655 ?
Na1 Na1 Na1 59.79(3) 3_666 1_655 ?
Na1 Na1 Na1 180.00(5) 1_455 1_655 ?
C1 N1 N2 109.94(18) . . ?
C1 N1 H1 125.0 . . ?
N2 N1 H1 125.0 . . ?
N3 N2 N1 105.76(18) . . ?
N3 N2 Na1 127.29(14) . 2 ?
N1 N2 Na1 126.70(14) . 2 ?
N2 N3 N4 111.59(18) . . ?
N3 N4 C1 106.80(17) . . ?
C1 O1 Na1 120.90(14) . . ?
C1 O1 Na1 131.29(15) . 3_566 ?
Na1 O1 Na1 94.63(6) . 3_566 ?
C1 O1 Na1 113.46(14) . 3_666 ?
Na1 O1 Na1 94.18(6) . 3_666 ?
Na1 O1 Na1 93.95(6) 3_566 3_666 ?
Na1 O2 Na1 93.32(6) . 1_455 ?
Na1 O2 H2A 113.1 . . ?
Na1 O2 H2A 113.0 1_455 . ?
Na1 O2 H2B 113.0 . . ?
Na1 O2 H2B 113.0 1_455 . ?
H2A O2 H2B 110.5 . . ?
O1 C1 N1 125.7(2) . . ?
O1 C1 N4 128.4(2) . . ?
N1 C1 N4 105.90(18) . . ?

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 -0.1(3) . . . . ?
C1 N1 N2 Na1 -174.56(14) . . . 2 ?
N1 N2 N3 N4 0.1(3) . . . . ?
Na1 N2 N3 N4 174.52(15) 2 . . . ?
N2 N3 N4 C1 0.0(3) . . . . ?
O2 Na1 O1 C1 -57.60(17) . . . . ?
O1 Na1 O1 C1 -145.09(19) 3_566 . . . ?
O1 Na1 O1 C1 120.59(19) 3_666 . . . ?
O2 Na1 O1 C1 35.74(17) 1_655 . . . ?
N2 Na1 O1 C1 -30(4) 2_545 . . . ?
Na1 Na1 O1 C1 -145.09(19) 3_566 . . . ?
Na1 Na1 O1 C1 120.59(19) 3_666 . . . ?
Na1 Na1 O1 C1 -101.88(17) 1_455 . . . ?
Na1 Na1 O1 C1 78.12(17) 1_655 . . . ?
O2 Na1 O1 Na1 87.49(7) . . . 3_566 ?
O1 Na1 O1 Na1 0.0 3_566 . . 3_566 ?
O1 Na1 O1 Na1 -94.31(6) 3_666 . . 3_566 ?
O2 Na1 O1 Na1 -179.17(7) 1_655 . . 3_566 ?
N2 Na1 O1 Na1 115(4) 2_545 . . 3_566 ?
Na1 Na1 O1 Na1 -94.31(6) 3_666 . . 3_566 ?
Na1 Na1 O1 Na1 43.21(5) 1_455 . . 3_566 ?
Na1 Na1 O1 Na1 -136.79(5) 1_655 . . 3_566 ?
O2 Na1 O1 Na1 -178.20(7) . . . 3_666 ?
O1 Na1 O1 Na1 94.31(6) 3_566 . . 3_666 ?
O1 Na1 O1 Na1 0.0 3_666 . . 3_666 ?
O2 Na1 O1 Na1 -84.86(6) 1_655 . . 3_666 ?
N2 Na1 O1 Na1 -151(4) 2_545 . . 3_666 ?
Na1 Na1 O1 Na1 94.31(6) 3_566 . . 3_666 ?
Na1 Na1 O1 Na1 137.52(5) 1_455 . . 3_666 ?
Na1 Na1 O1 Na1 -42.48(5) 1_655 . . 3_666 ?
O1 Na1 O2 Na1 -90.77(7) . . . 1_455 ?
O1 Na1 O2 Na1 -5.35(6) 3_566 . . 1_455 ?
O1 Na1 O2 Na1 -109.5(7) 3_666 . . 1_455 ?
O2 Na1 O2 Na1 180.0 1_655 . . 1_455 ?
N2 Na1 O2 Na1 89.72(7) 2_545 . . 1_455 ?
Na1 Na1 O2 Na1 -47.97(6) 3_566 . . 1_455 ?
Na1 Na1 O2 Na1 -92.44(8) 3_666 . . 1_455 ?
Na1 Na1 O2 Na1 180.0 1_655 . . 1_455 ?
Na1 O1 C1 N1 165.43(17) . . . . ?
Na1 O1 C1 N1 34.8(3) 3_566 . . . ?
Na1 O1 C1 N1 -83.9(2) 3_666 . . . ?
Na1 O1 C1 N4 -16.0(3) . . . . ?
Na1 O1 C1 N4 -146.59(19) 3_566 . . . ?
Na1 O1 C1 N4 94.7(2) 3_666 . . . ?
N2 N1 C1 O1 178.9(2) . . . . ?
N2 N1 C1 N4 0.0(3) . . . . ?
N3 N4 C1 O1 -178.8(2) . . . . ?
N3 N4 C1 N1 0.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.082
####################################################################### 
# 
# 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_140716h
_database_code_depnum_ccdc_archive 'CCDC 1018915'
_audit_update_record             
;
2014-08-11 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H10 Mg N8 O6'
_chemical_formula_weight         266.49

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmca

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

_cell_length_a                   6.6379(5)
_cell_length_b                   16.5198(14)
_cell_length_c                   9.1359(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1001.81(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    780
_cell_measurement_theta_min      2.466
_cell_measurement_theta_max      26.361

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9237
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1997
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         25.01
_reflns_number_total             486
_reflns_number_gt                425
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0848P)²+0.6172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         486
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1354
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
Mg1 Mg 0.5000 0.5000 0.0000 0.0208(6) Uani 1 4 d S . .
N1 N 0.5000 0.30296(15) 0.1880(3) 0.0255(8) Uani 1 2 d S A .
H1 H 0.5000 0.2964 0.0946 0.031 Uiso 1 2 calc SR . .
N3 N 0.5000 0.27715(17) 0.4126(3) 0.0308(8) Uani 1 2 d S A .
N4 N 0.5000 0.35865(16) 0.4010(3) 0.0290(8) Uani 1 2 d S A .
C1 C 0.5000 0.37475(19) 0.2566(4) 0.0279(9) Uani 1 2 d S . .
N2 N 0.5000 0.24328(16) 0.2866(3) 0.0338(8) Uani 1 2 d S . .
O2' O 0.7633(6) 0.5438(2) 0.0871(3) 0.0308(12) Uani 0.495(5) 1 d P A 2
H2'C H 0.8307 0.5158 0.1478 0.037 Uiso 0.495(5) 1 d PR A 2
H2'D H 0.8448 0.5714 0.0355 0.037 Uiso 0.495(5) 1 d PR A 2
O1 O 0.4538(5) 0.44274(16) 0.1979(3) 0.0263(15) Uani 0.50 1 d P . .
O2 O 0.6598(6) 0.5952(2) 0.0852(3) 0.0308(13) Uani 0.505(5) 1 d P A 1
H2C H 0.6123 0.6381 0.1232 0.037 Uiso 0.505(5) 1 d PR A 1
H2D H 0.7593 0.6081 0.0315 0.037 Uiso 0.505(5) 1 d PR A 1


_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. 
;

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
Mg1 O2 2.051(3) 9_665 ?
Mg1 O2 2.051(3) . ?
Mg1 O2 2.051(3) 4_565 ?
Mg1 O2 2.051(3) 12_655 ?
Mg1 O2' 2.052(3) 9_665 ?
Mg1 O2' 2.052(3) . ?
Mg1 O2' 2.052(3) 4_565 ?
Mg1 O2' 2.052(3) 12_655 ?
Mg1 O1 2.064(3) 12_655 ?
Mg1 O1 2.064(3) . ?
Mg1 O1 2.064(3) 4_565 ?
Mg1 O1 2.064(3) 9_665 ?
N1 N2 1.336(3) . ?
N1 C1 1.342(4) . ?
N1 H1 0.8600 . ?
N3 N2 1.280(4) . ?
N3 N4 1.350(4) . ?
N4 C1 1.346(4) . ?
C1 O1 1.282(4) . ?
C1 O1 1.282(4) 12_655 ?
O2' H2'C 0.8500 . ?
O2' H2'D 0.8499 . ?
O2' H2D 1.1785 . ?
O1 O1 0.613(7) 12_655 ?
O2 H2'D 1.3672 . ?
O2 H2C 0.8501 . ?
O2 H2D 0.8500 . ?

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
O2 Mg1 O2 180.00(13) 9_665 . ?
O2 Mg1 O2 62.3(2) 9_665 4_565 ?
O2 Mg1 O2 117.7(2) . 4_565 ?
O2 Mg1 O2 117.7(2) 9_665 12_655 ?
O2 Mg1 O2 62.3(2) . 12_655 ?
O2 Mg1 O2 180.000(1) 4_565 12_655 ?
O2 Mg1 O2' 30.88(12) 9_665 9_665 ?
O2 Mg1 O2' 149.12(12) . 9_665 ?
O2 Mg1 O2' 91.30(18) 4_565 9_665 ?
O2 Mg1 O2' 88.70(18) 12_655 9_665 ?
O2 Mg1 O2' 149.12(12) 9_665 . ?
O2 Mg1 O2' 30.88(12) . . ?
O2 Mg1 O2' 88.70(18) 4_565 . ?
O2 Mg1 O2' 91.30(18) 12_655 . ?
O2' Mg1 O2' 180.0(2) 9_665 . ?
O2 Mg1 O2' 91.31(18) 9_665 4_565 ?
O2 Mg1 O2' 88.70(18) . 4_565 ?
O2 Mg1 O2' 30.88(12) 4_565 4_565 ?
O2 Mg1 O2' 149.12(12) 12_655 4_565 ?
O2' Mg1 O2' 116.8(2) 9_665 4_565 ?
O2' Mg1 O2' 63.2(2) . 4_565 ?
O2 Mg1 O2' 88.70(18) 9_665 12_655 ?
O2 Mg1 O2' 91.30(18) . 12_655 ?
O2 Mg1 O2' 149.12(12) 4_565 12_655 ?
O2 Mg1 O2' 30.88(12) 12_655 12_655 ?
O2' Mg1 O2' 63.2(2) 9_665 12_655 ?
O2' Mg1 O2' 116.8(2) . 12_655 ?
O2' Mg1 O2' 180.0 4_565 12_655 ?
O2 Mg1 O1 93.31(12) 9_665 12_655 ?
O2 Mg1 O1 86.69(12) . 12_655 ?
O2 Mg1 O1 84.50(12) 4_565 12_655 ?
O2 Mg1 O1 95.50(12) 12_655 12_655 ?
O2' Mg1 O1 107.74(13) 9_665 12_655 ?
O2' Mg1 O1 72.26(13) . 12_655 ?
O2' Mg1 O1 92.97(13) 4_565 12_655 ?
O2' Mg1 O1 87.03(13) 12_655 12_655 ?
O2 Mg1 O1 84.50(12) 9_665 . ?
O2 Mg1 O1 95.50(12) . . ?
O2 Mg1 O1 93.31(12) 4_565 . ?
O2 Mg1 O1 86.69(12) 12_655 . ?
O2' Mg1 O1 92.97(13) 9_665 . ?
O2' Mg1 O1 87.03(13) . . ?
O2' Mg1 O1 107.74(13) 4_565 . ?
O2' Mg1 O1 72.26(13) 12_655 . ?
O1 Mg1 O1 17.1(2) 12_655 . ?
O2 Mg1 O1 86.69(12) 9_665 4_565 ?
O2 Mg1 O1 93.31(12) . 4_565 ?
O2 Mg1 O1 95.50(12) 4_565 4_565 ?
O2 Mg1 O1 84.50(12) 12_655 4_565 ?
O2' Mg1 O1 72.26(13) 9_665 4_565 ?
O2' Mg1 O1 107.74(13) . 4_565 ?
O2' Mg1 O1 87.03(13) 4_565 4_565 ?
O2' Mg1 O1 92.97(13) 12_655 4_565 ?
O1 Mg1 O1 180.0 12_655 4_565 ?
O1 Mg1 O1 162.9(2) . 4_565 ?
O2 Mg1 O1 95.50(12) 9_665 9_665 ?
O2 Mg1 O1 84.50(12) . 9_665 ?
O2 Mg1 O1 86.69(12) 4_565 9_665 ?
O2 Mg1 O1 93.31(12) 12_655 9_665 ?
O2' Mg1 O1 87.03(13) 9_665 9_665 ?
O2' Mg1 O1 92.97(13) . 9_665 ?
O2' Mg1 O1 72.26(13) 4_565 9_665 ?
O2' Mg1 O1 107.74(13) 12_655 9_665 ?
O1 Mg1 O1 162.9(2) 12_655 9_665 ?
O1 Mg1 O1 180.00(13) . 9_665 ?
O1 Mg1 O1 17.1(2) 4_565 9_665 ?
N2 N1 C1 109.7(3) . . ?
N2 N1 H1 125.1 . . ?
C1 N1 H1 125.1 . . ?
N2 N3 N4 111.4(2) . . ?
C1 N4 N3 105.9(2) . . ?
O1 C1 O1 27.7(3) . 12_655 ?
O1 C1 N1 125.4(3) . . ?
O1 C1 N1 125.4(3) 12_655 . ?
O1 C1 N4 125.7(3) . . ?
O1 C1 N4 125.7(3) 12_655 . ?
N1 C1 N4 106.5(3) . . ?
N3 N2 N1 106.5(2) . . ?
Mg1 O2' H2'C 120.6 . . ?
Mg1 O2' H2'D 121.1 . . ?
H2'C O2' H2'D 108.6 . . ?
Mg1 O2' H2D 97.6 . . ?
H2'C O2' H2D 141.7 . . ?
H2'D O2' H2D 44.9 . . ?
O1 O1 C1 76.17(16) 12_655 . ?
O1 O1 Mg1 81.46(10) 12_655 . ?
C1 O1 Mg1 137.1(2) . . ?
Mg1 O2 H2'D 96.8 . . ?
Mg1 O2 H2C 127.1 . . ?
H2'D O2 H2C 135.2 . . ?
Mg1 O2 H2D 112.0 . . ?
H2'D O2 H2D 35.2 . . ?
H2C O2 H2D 108.4 . . ?

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
N2 N3 N4 C1 0.0 . . . . ?
N2 N1 C1 O1 -162.9(2) . . . . ?
N2 N1 C1 O1 162.9(2) . . . 12_655 ?
N2 N1 C1 N4 0.0 . . . . ?
N3 N4 C1 O1 162.9(2) . . . . ?
N3 N4 C1 O1 -162.9(2) . . . 12_655 ?
N3 N4 C1 N1 0.0 . . . . ?
N4 N3 N2 N1 0.0 . . . . ?
C1 N1 N2 N3 0.0 . . . . ?
N1 C1 O1 O1 -100.08(16) . . . 12_655 ?
N4 C1 O1 O1 100.18(17) . . . 12_655 ?
O1 C1 O1 Mg1 60.7(3) 12_655 . . . ?
N1 C1 O1 Mg1 -39.4(4) . . . . ?
N4 C1 O1 Mg1 160.9(2) . . . . ?
O2 Mg1 O1 O1 120.73(12) 9_665 . . 12_655 ?
O2 Mg1 O1 O1 -59.27(12) . . . 12_655 ?
O2 Mg1 O1 O1 58.99(11) 4_565 . . 12_655 ?
O2 Mg1 O1 O1 -121.01(11) 12_655 . . 12_655 ?
O2' Mg1 O1 O1 150.47(11) 9_665 . . 12_655 ?
O2' Mg1 O1 O1 -29.53(11) . . . 12_655 ?
O2' Mg1 O1 O1 31.12(12) 4_565 . . 12_655 ?
O2' Mg1 O1 O1 -148.88(12) 12_655 . . 12_655 ?
O1 Mg1 O1 O1 180.000(1) 4_565 . . 12_655 ?
O1 Mg1 O1 O1 -94.4(4) 9_665 . . 12_655 ?
O2 Mg1 O1 C1 61.8(4) 9_665 . . . ?
O2 Mg1 O1 C1 -118.2(4) . . . . ?
O2 Mg1 O1 C1 0.1(4) 4_565 . . . ?
O2 Mg1 O1 C1 -179.9(4) 12_655 . . . ?
O2' Mg1 O1 C1 91.6(4) 9_665 . . . ?
O2' Mg1 O1 C1 -88.4(4) . . . . ?
O2' Mg1 O1 C1 -27.8(4) 4_565 . . . ?
O2' Mg1 O1 C1 152.2(4) 12_655 . . . ?
O1 Mg1 O1 C1 -58.9(3) 12_655 . . . ?
O1 Mg1 O1 C1 121.1(3) 4_565 . . . ?
O1 Mg1 O1 C1 -153.3(6) 9_665 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_140725g
_database_code_depnum_ccdc_archive 'CCDC 1018917'
_audit_update_record             
;
2017-05-25 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Calcium 5-oxotetrazolate pentahydrate '
_chemical_formula_moiety         
'C4 H24 Ca2 N16 O14, 0.5(C2 H4 N8 O2), 0.5(H4 O2)'
_chemical_formula_sum            'C5 H28 Ca2 N20 O16'
_chemical_formula_weight         704.63
_chemical_melting_point          ?
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z-1/2'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.9853(10)
_cell_length_b                   24.4542(15)
_cell_length_c                   6.7717(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2481.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.433
_cell_measurement_theta_min      2.843
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.803
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.8026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1171
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         2.845
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1000
_reflns_number_total             1171
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1171
_refine_ls_number_restraints     268
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.1290
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1272P)²+64.1440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2995
_refine_ls_wR_factor_ref         0.3075
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.889(9)
 0.111(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 N12-C3 = N9-C3
 1.33 with sigma of 0.02
 N12-N11 = N9-N10
 1.33 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.01
5. Others
 Fixed Sof: N9(0.25) H9(0.25) N10(0.25) N11(0.25) N12(0.25) H12(0.25) O3(0.25)
 O7(0.25) H7A(0.25) H7B(0.25) C3(0.25)
6.a Fixed occupancy and ADP/Uiso:
 H4
6.b Riding coordinates:
 N9(H9), N12(H12), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ca1 Ca 0.28648(17) 0.33200(10) 0.5000 0.0153(7) Uani 1 2 d S TU P . .
N1 N 0.3914(7) 0.4711(4) 0.5000 0.016(2) Uani 1 2 d S TU P . .
H1 H 0.4437 0.4566 0.5000 0.019 Uiso 1 2 calc RS T P . .
N2 N 0.3157(7) 0.4427(4) 0.5000 0.018(2) Uani 1 2 d S TU P . .
N3 N 0.2522(8) 0.4793(5) 0.5000 0.025(2) Uani 1 2 d S TU P . .
N4 N 0.2864(8) 0.5311(5) 0.5000 0.026(2) Uani 1 2 d S TU P . .
N5 N 0.5091(7) 0.2649(4) 0.5000 0.017(2) Uani 1 2 d S TU P . .
N6 N 0.4193(8) 0.2569(4) 0.5000 0.019(2) Uani 1 2 d S TU P . .
N7 N 0.4005(8) 0.2071(4) 0.5000 0.023(2) Uani 1 2 d S TU P . .
N8 N 0.4724(8) 0.1796(4) 0.5000 0.025(2) Uani 1 2 d S TU P . .
H8 H 0.4757 0.1445 0.5000 0.030 Uiso 1 2 calc RS T P . .
N9 N 0.071(2) 0.4906(10) 0.5000 0.037(4) Uani 0.5 2 d DS TU P A 1
H9 H 0.1172 0.4701 0.5000 0.044 Uiso 0.5 2 d RS T P A 1
N10 N 0.075(2) 0.5447(10) 0.5000 0.039(4) Uani 0.5 2 d DS TU P A 1
N11 N -0.007(2) 0.5611(10) 0.5000 0.037(4) Uani 0.5 2 d DS TU P A 1
N12 N -0.062(2) 0.5171(10) 0.5000 0.031(4) Uani 0.5 2 d DS TU P A 1
H12 H -0.1195 0.5170 0.5000 0.038 Uiso 0.5 2 d RS T P A 1
O1 O 0.4329(6) 0.5634(4) 0.5000 0.025(2) Uani 1 2 d S TU P . .
O2 O 0.6255(6) 0.2033(4) 0.5000 0.027(2) Uani 1 2 d S TU P . .
O3 O -0.0433(17) 0.4229(10) 0.5000 0.041(4) Uani 0.5 2 d S TU P A 1
O4 O 0.2500 0.2500 0.7312(14) 0.023(2) Uani 1 2 d S TU P . .
H4 H 0.213(7) 0.257(5) 0.794(17) 0.027 Uiso 1 1 d . . . . .
O5 O 0.3954(5) 0.3509(3) 0.7499(11) 0.0363(19) Uani 1 1 d . U . . .
H5A H 0.4039 0.3797 0.8176 0.044 Uiso 1 1 d R . . . .
H5B H 0.4200 0.3244 0.8099 0.044 Uiso 1 1 d R . . . .
O6 O 0.1928(4) 0.3794(3) 0.2626(11) 0.0293(17) Uani 1 1 d . U . . .
H6A H 0.1736 0.3569 0.1767 0.035 Uiso 1 1 d R . . . .
H6B H 0.2232 0.4038 0.2039 0.035 Uiso 1 1 d R . . . .
O7 O 0.0759(17) 0.4372(10) 0.5000 0.043(4) Uani 0.5 2 d S TU P B 2
H7A H 0.1293 0.4475 0.5000 0.052 Uiso 0.5 2 d RS T P B 2
H7B H 0.0403 0.4629 0.4756 0.052 Uiso 0.25 1 d R . . B 2
C1 C 0.3766(9) 0.5244(5) 0.5000 0.021(2) Uani 1 2 d S TU P . .
C2 C 0.5439(9) 0.2145(5) 0.5000 0.021(2) Uani 1 2 d S TU P . .
C3 C -0.013(2) 0.4722(11) 0.5000 0.036(4) Uani 0.5 2 d DS TU P A 1


_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.
;
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
Ca1 Ca1 4.157(5) 13_556 ?
Ca1 N2 2.741(10) . ?
Ca1 N6 2.707(11) . ?
Ca1 N7 2.960(12) 13_556 ?
Ca1 O4 2.602(6) . ?
Ca1 O4 2.602(6) 13_556 ?
Ca1 O5 2.397(7) 10_556 ?
Ca1 O5 2.397(7) . ?
Ca1 O6 2.428(7) . ?
Ca1 O6 2.428(7) 10_556 ?
N1 H1 0.8600 . ?
N1 N2 1.330(14) . ?
N1 C1 1.321(16) . ?
N2 N3 1.306(15) . ?
N3 N4 1.367(16) . ?
N4 C1 1.363(18) . ?
N5 N6 1.359(15) . ?
N5 C2 1.337(16) . ?
N6 N7 1.252(15) . ?
N7 Ca1 2.960(12) 13_556 ?
N7 N8 1.270(16) . ?
N8 H8 0.8600 . ?
N8 C2 1.368(18) . ?
N9 H9 0.8598 . ?
N9 N10 1.324(19) . ?
N9 N11 1.58(4) 9_566 ?
N9 N12 0.23(4) 9_566 ?
N9 C3 1.33(2) . ?
N9 C3 1.25(6) 9_566 ?
N10 N11 1.29(4) . ?
N10 N12 1.52(4) 9_566 ?
N10 O3 0.92(3) 9_566 ?
N10 C3 1.01(3) 9_566 ?
N11 N9 1.58(4) 9_566 ?
N11 N12 1.355(19) . ?
N11 O3 0.85(3) 9_566 ?
N11 C3 0.87(3) 9_566 ?
N12 N9 0.23(4) 9_566 ?
N12 N10 1.52(4) 9_566 ?
N12 H12 0.8600 . ?
N12 C3 1.16(5) 9_566 ?
N12 C3 1.32(2) . ?
O1 C1 1.273(16) . ?
O2 C2 1.253(17) . ?
O3 N10 0.92(3) 9_566 ?
O3 N11 0.85(3) 9_566 ?
O3 C3 1.29(4) . ?
O4 Ca1 2.602(6) 13_556 ?
O4 H4 0.72(11) . ?
O5 H5A 0.8499 . ?
O5 H5B 0.8500 . ?
O6 H6A 0.8499 . ?
O6 H6B 0.8504 . ?
O7 H7A 0.8378 . ?
O7 H7B 0.8402 . ?
C3 N9 1.25(6) 9_566 ?
C3 N10 1.01(3) 9_566 ?
C3 N11 0.87(3) 9_566 ?
C3 N12 1.16(5) 9_566 ?
C3 C3 1.41(5) 9_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
N2 Ca1 Ca1 173.9(3) . 13_556 ?
N2 Ca1 N7 118.0(3) . 13_556 ?
N6 Ca1 Ca1 62.6(2) . 13_556 ?
N6 Ca1 N2 123.5(3) . . ?
N6 Ca1 N7 118.5(3) . 13_556 ?
N7 Ca1 Ca1 55.9(2) 13_556 13_556 ?
O4 Ca1 Ca1 36.99(17) . 13_556 ?
O4 Ca1 Ca1 36.99(17) 13_556 13_556 ?
O4 Ca1 N2 142.58(17) 13_556 . ?
O4 Ca1 N2 142.58(17) . . ?
O4 Ca1 N6 68.41(19) 13_556 . ?
O4 Ca1 N6 68.41(19) . . ?
O4 Ca1 N7 63.41(18) . 13_556 ?
O4 Ca1 N7 63.41(18) 13_556 13_556 ?
O4 Ca1 O4 74.0(3) . 13_556 ?
O5 Ca1 Ca1 111.45(19) . 13_556 ?
O5 Ca1 Ca1 111.45(19) 10_556 13_556 ?
O5 Ca1 N2 72.6(2) . . ?
O5 Ca1 N2 72.6(2) 10_556 . ?
O5 Ca1 N6 68.3(2) 10_556 . ?
O5 Ca1 N6 68.3(2) . . ?
O5 Ca1 N7 135.0(2) . 13_556 ?
O5 Ca1 N7 135.0(2) 10_556 13_556 ?
O5 Ca1 O4 135.8(2) 10_556 . ?
O5 Ca1 O4 135.8(2) . 13_556 ?
O5 Ca1 O4 82.4(2) 10_556 13_556 ?
O5 Ca1 O4 82.4(2) . . ?
O5 Ca1 O5 89.8(4) 10_556 . ?
O5 Ca1 O6 80.5(2) 10_556 . ?
O5 Ca1 O6 80.5(2) . 10_556 ?
O5 Ca1 O6 140.3(3) . . ?
O5 Ca1 O6 140.3(3) 10_556 10_556 ?
O6 Ca1 Ca1 107.94(17) 10_556 13_556 ?
O6 Ca1 Ca1 107.94(17) . 13_556 ?
O6 Ca1 N2 67.8(2) 10_556 . ?
O6 Ca1 N2 67.8(2) . . ?
O6 Ca1 N6 138.46(18) 10_556 . ?
O6 Ca1 N6 138.45(18) . . ?
O6 Ca1 N7 66.8(2) . 13_556 ?
O6 Ca1 N7 66.8(2) 10_556 13_556 ?
O6 Ca1 O4 130.1(2) 10_556 13_556 ?
O6 Ca1 O4 81.2(2) . 13_556 ?
O6 Ca1 O4 130.1(2) . . ?
O6 Ca1 O4 81.2(2) 10_556 . ?
O6 Ca1 O6 82.9(4) . 10_556 ?
N2 N1 H1 124.1 . . ?
C1 N1 H1 124.1 . . ?
C1 N1 N2 111.9(11) . . ?
N1 N2 Ca1 130.7(8) . . ?
N3 N2 Ca1 124.1(8) . . ?
N3 N2 N1 105.2(10) . . ?
N2 N3 N4 111.3(11) . . ?
C1 N4 N3 105.0(11) . . ?
C2 N5 N6 104.8(10) . . ?
N5 N6 Ca1 129.1(7) . . ?
N7 N6 Ca1 119.7(9) . . ?
N7 N6 N5 111.2(11) . . ?
N6 N7 Ca1 121.9(9) . 13_556 ?
N6 N7 N8 108.8(12) . . ?
N8 N7 Ca1 129.3(8) . 13_556 ?
N7 N8 H8 125.2 . . ?
N7 N8 C2 109.6(11) . . ?
C2 N8 H8 125.2 . . ?
N10 N9 H9 122.9 . . ?
N10 N9 N11 146(3) . 9_566 ?
N10 N9 C3 112(3) . . ?
N11 N9 H9 91.3 9_566 . ?
N12 N9 H9 88.6 9_566 . ?
N12 N9 N10 148(10) 9_566 . ?
N12 N9 N11 3(10) 9_566 9_566 ?
N12 N9 C3 102(10) 9_566 9_566 ?
N12 N9 C3 36(10) 9_566 . ?
C3 N9 H9 124.6 . . ?
C3 N9 H9 169.1 9_566 . ?
C3 N9 N10 46.2(18) 9_566 . ?
C3 N9 N11 100(3) 9_566 9_566 ?
C3 N9 N11 33.3(15) . 9_566 ?
C3 N9 C3 66(3) 9_566 . ?
N9 N10 N12 4(3) . 9_566 ?
N11 N10 N9 105(3) . . ?
N11 N10 N12 100.9(19) . 9_566 ?
O3 N10 N9 146(4) 9_566 . ?
O3 N10 N11 41(2) 9_566 . ?
O3 N10 N12 142(3) 9_566 9_566 ?
O3 N10 C3 83(3) 9_566 9_566 ?
C3 N10 N9 63(3) 9_566 . ?
C3 N10 N11 42(2) 9_566 . ?
C3 N10 N12 58.8(18) 9_566 9_566 ?
N10 N11 N9 109(2) . 9_566 ?
N10 N11 N12 109(3) . . ?
N12 N11 N9 0(2) . 9_566 ?
O3 N11 N9 154(4) 9_566 9_566 ?
O3 N11 N10 46(2) 9_566 . ?
O3 N11 N12 155(4) 9_566 . ?
O3 N11 C3 97(4) 9_566 9_566 ?
C3 N11 N9 57(2) 9_566 9_566 ?
C3 N11 N10 51(3) 9_566 . ?
C3 N11 N12 58(3) 9_566 . ?
N9 N12 N10 27(10) 9_566 9_566 ?
N9 N12 N11 177(10) 9_566 . ?
N9 N12 H12 55.5 9_566 . ?
N9 N12 C3 68(10) 9_566 . ?
N9 N12 C3 137(10) 9_566 9_566 ?
N10 N12 H12 82.6 9_566 . ?
N11 N12 N10 150(3) . 9_566 ?
N11 N12 H12 127.6 . . ?
C3 N12 N10 41.0(16) . 9_566 ?
C3 N12 N10 110(4) 9_566 9_566 ?
C3 N12 N11 109(3) . . ?
C3 N12 N11 39.5(17) 9_566 . ?
C3 N12 H12 123.6 . . ?
C3 N12 H12 167.1 9_566 . ?
C3 N12 C3 69(3) 9_566 . ?
N10 O3 C3 51(2) 9_566 . ?
N11 O3 N10 93(4) 9_566 9_566 ?
N11 O3 C3 42(2) 9_566 . ?
Ca1 O4 Ca1 106.0(3) . 13_556 ?
Ca1 O4 H4 112(9) 13_556 . ?
Ca1 O4 H4 110(9) . . ?
Ca1 O5 H5A 130.0 . . ?
Ca1 O5 H5B 119.0 . . ?
H5A O5 H5B 108.2 . . ?
Ca1 O6 H6A 109.9 . . ?
Ca1 O6 H6B 109.5 . . ?
H6A O6 H6B 108.3 . . ?
H7A O7 H7B 112.5 . . ?
N1 C1 N4 106.6(12) . . ?
O1 C1 N1 128.9(13) . . ?
O1 C1 N4 124.5(12) . . ?
N5 C2 N8 105.6(12) . . ?
O2 C2 N5 125.5(13) . . ?
O2 C2 N8 128.9(12) . . ?
N9 C3 N9 114(3) 9_566 . ?
N9 C3 N12 10(2) 9_566 . ?
N9 C3 O3 116(3) 9_566 . ?
N9 C3 C3 54(3) . 9_566 ?
N9 C3 C3 60(2) 9_566 9_566 ?
N10 C3 N9 71(3) 9_566 9_566 ?
N10 C3 N9 176(3) 9_566 . ?
N10 C3 N12 80(2) 9_566 . ?
N10 C3 N12 169(5) 9_566 9_566 ?
N10 C3 O3 45(2) 9_566 . ?
N10 C3 C3 130(4) 9_566 9_566 ?
N11 C3 N9 89(3) 9_566 . ?
N11 C3 N9 157(5) 9_566 9_566 ?
N11 C3 N10 86(4) 9_566 9_566 ?
N11 C3 N12 167(3) 9_566 . ?
N11 C3 N12 83(4) 9_566 9_566 ?
N11 C3 O3 41(2) 9_566 . ?
N11 C3 C3 144(5) 9_566 9_566 ?
N12 C3 N9 7(2) 9_566 . ?
N12 C3 N9 120(3) 9_566 9_566 ?
N12 C3 N9 104(2) . . ?
N12 C3 N12 111(3) 9_566 . ?
N12 C3 O3 124(4) 9_566 . ?
N12 C3 C3 61(2) 9_566 9_566 ?
N12 C3 C3 50(3) . 9_566 ?
O3 C3 N9 130(2) . . ?
O3 C3 N12 126(2) . . ?
O3 C3 C3 175(4) . 9_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
Ca1 N2 N3 N4 180.0 . . . . ?
Ca1 N6 N7 Ca1 0.0 . . . 13_556 ?
Ca1 N6 N7 N8 180.0 . . . . ?
Ca1 N7 N8 C2 180.0 13_556 . . . ?
N1 N2 N3 N4 0.0 . . . . ?
N2 N1 C1 N4 0.0 . . . . ?
N2 N1 C1 O1 180.0 . . . . ?
N2 N3 N4 C1 0.0 . . . . ?
N3 N4 C1 N1 0.0 . . . . ?
N3 N4 C1 O1 180.0 . . . . ?
N5 N6 N7 Ca1 180.0 . . . 13_556 ?
N5 N6 N7 N8 0.0 . . . . ?
N6 N5 C2 N8 0.0 . . . . ?
N6 N5 C2 O2 180.0 . . . . ?
N6 N7 N8 C2 0.0 . . . . ?
N7 N8 C2 N5 0.0 . . . . ?
N7 N8 C2 O2 180.0 . . . . ?
N9 N10 N11 N9 0.0 . . . 9_566 ?
N9 N10 N11 N12 0.0 . . . . ?
N9 N10 N11 O3 180.0 . . . 9_566 ?
N9 N10 N11 C3 0.0 . . . 9_566 ?
N9 N11 N12 N10 0.0 9_566 . . 9_566 ?
N9 N11 N12 C3 0.0 9_566 . . . ?
N9 N11 N12 C3 0.0 9_566 . . 9_566 ?
N9 N12 C3 N9 180.0 9_566 . . . ?
N9 N12 C3 N10 0.0 9_566 . . 9_566 ?
N9 N12 C3 N11 0.0 9_566 . . 9_566 ?
N9 N12 C3 N12 180.0 9_566 . . 9_566 ?
N9 N12 C3 O3 0.0 9_566 . . . ?
N9 N12 C3 C3 180.0 9_566 . . 9_566 ?
N10 N9 C3 N9 0.0 . . . 9_566 ?
N10 N9 C3 N11 180.0 . . . 9_566 ?
N10 N9 C3 N12 180.0 . . . 9_566 ?
N10 N9 C3 N12 0.0 . . . . ?
N10 N9 C3 O3 180.0 . . . . ?
N10 N9 C3 C3 0.0 . . . 9_566 ?
N10 N11 N12 N10 0.0 . . . 9_566 ?
N10 N11 N12 C3 0.0 . . . . ?
N10 N11 N12 C3 0.0 . . . 9_566 ?
N10 N12 C3 N9 180.0 9_566 . . . ?
N10 N12 C3 N9 0.0 9_566 . . 9_566 ?
N10 N12 C3 N11 0.0 9_566 . . 9_566 ?
N10 N12 C3 N12 180.0 9_566 . . 9_566 ?
N10 N12 C3 O3 0.0 9_566 . . . ?
N10 N12 C3 C3 180.0 9_566 . . 9_566 ?
N10 O3 C3 N9 180.0 9_566 . . . ?
N10 O3 C3 N9 0.0 9_566 . . 9_566 ?
N10 O3 C3 N11 180.0 9_566 . . 9_566 ?
N10 O3 C3 N12 0.0 9_566 . . . ?
N10 O3 C3 N12 180.0 9_566 . . 9_566 ?
N11 N9 N10 N11 0.0 9_566 . . . ?
N11 N9 N10 N12 0.0 9_566 . . 9_566 ?
N11 N9 N10 O3 0.0 9_566 . . 9_566 ?
N11 N9 N10 C3 0.0 9_566 . . 9_566 ?
N11 N9 C3 N9 180.0 9_566 . . 9_566 ?
N11 N9 C3 N12 180.0 9_566 . . . ?
N11 N9 C3 N12 0.0 9_566 . . 9_566 ?
N11 N9 C3 O3 0.0 9_566 . . . ?
N11 N9 C3 C3 180.0 9_566 . . 9_566 ?
N11 N12 C3 N9 180.0 . . . 9_566 ?
N11 N12 C3 N9 0.0 . . . . ?
N11 N12 C3 N10 180.0 . . . 9_566 ?
N11 N12 C3 N11 180.0 . . . 9_566 ?
N11 N12 C3 N12 0.0 . . . 9_566 ?
N11 N12 C3 O3 180.0 . . . . ?
N11 N12 C3 C3 0.0 . . . 9_566 ?
N11 O3 C3 N9 180.0 9_566 . . 9_566 ?
N11 O3 C3 N9 0.0 9_566 . . . ?
N11 O3 C3 N10 180.0 9_566 . . 9_566 ?
N11 O3 C3 N12 0.0 9_566 . . 9_566 ?
N11 O3 C3 N12 180.0 9_566 . . . ?
N12 N9 N10 N11 0.0 9_566 . . . ?
N12 N9 N10 O3 0.0 9_566 . . 9_566 ?
N12 N9 N10 C3 0.0 9_566 . . 9_566 ?
N12 N9 C3 N9 180.0 9_566 . . 9_566 ?
N12 N9 C3 N11 0.0 9_566 . . 9_566 ?
N12 N9 C3 N12 180.0 9_566 . . . ?
N12 N9 C3 O3 0.0 9_566 . . . ?
N12 N9 C3 C3 180.0 9_566 . . 9_566 ?
N12 N10 N11 N9 0.0 9_566 . . 9_566 ?
N12 N10 N11 N12 0.0 9_566 . . . ?
N12 N10 N11 O3 180.0 9_566 . . 9_566 ?
N12 N10 N11 C3 0.0 9_566 . . 9_566 ?
O3 N10 N11 N9 180.0 9_566 . . 9_566 ?
O3 N10 N11 N12 180.0 9_566 . . . ?
O3 N10 N11 C3 180.0 9_566 . . 9_566 ?
O3 N11 N12 N10 0.0 9_566 . . 9_566 ?
O3 N11 N12 C3 0.0 9_566 . . 9_566 ?
O3 N11 N12 C3 0.0 9_566 . . . ?
C1 N1 N2 Ca1 180.0 . . . . ?
C1 N1 N2 N3 0.0 . . . . ?
C2 N5 N6 Ca1 180.0 . . . . ?
C2 N5 N6 N7 0.0 . . . . ?
C3 N9 N10 N11 0.0 . . . . ?
C3 N9 N10 N11 0.0 9_566 . . . ?
C3 N9 N10 N12 0.0 . . . 9_566 ?
C3 N9 N10 N12 0.0 9_566 . . 9_566 ?
C3 N9 N10 O3 0.0 . . . 9_566 ?
C3 N9 N10 O3 0.0 9_566 . . 9_566 ?
C3 N9 N10 C3 0.0 . . . 9_566 ?
C3 N9 C3 N9 0.0 9_566 . . 9_566 ?
C3 N9 C3 N11 180.0 9_566 . . 9_566 ?
C3 N9 C3 N12 0.0 9_566 . . . ?
C3 N9 C3 N12 180.0 9_566 . . 9_566 ?
C3 N9 C3 O3 180.0 9_566 . . . ?
C3 N10 N11 N9 0.0 9_566 . . 9_566 ?
C3 N10 N11 N12 0.0 9_566 . . . ?
C3 N10 N11 O3 180.0 9_566 . . 9_566 ?
C3 N11 N12 N10 0.0 9_566 . . 9_566 ?
C3 N11 N12 C3 0.0 9_566 . . . ?
C3 N12 C3 N9 0.0 9_566 . . . ?
C3 N12 C3 N9 180.0 9_566 . . 9_566 ?
C3 N12 C3 N10 180.0 9_566 . . 9_566 ?
C3 N12 C3 N11 180.0 9_566 . . 9_566 ?
C3 N12 C3 N12 0.0 9_566 . . 9_566 ?
C3 N12 C3 O3 180.0 9_566 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.889(9)
2 0.111(9)
####################################################################### 
# 
# 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_140612a
_database_code_depnum_ccdc_archive 'CCDC 1018902'
_audit_update_record             
;
2014-08-11 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C H3 Li N4 O2'
_chemical_formula_weight         110.01

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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'

_cell_length_a                   6.6019(4)
_cell_length_b                   5.0870(3)
_cell_length_c                   14.9308(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.846(2)
_cell_angle_gamma                90.00
_cell_volume                     494.05(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1077
_cell_measurement_theta_min      2.797
_cell_measurement_theta_max      28.107

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             224
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9479
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2272
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         25.02
_reflns_number_total             863
_reflns_number_gt                674
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0504P)²+0.3033P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.040(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         863
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_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
N2 N 0.7791(3) 0.4392(4) 0.52956(15) 0.0308(6) Uani 1 1 d . . .
O1 O 0.5913(3) 0.6707(4) 0.31204(13) 0.0339(6) Uani 1 1 d . . .
C1 C 0.6559(4) 0.5401(5) 0.38467(17) 0.0252(6) Uani 1 1 d . . .
O2 O 0.1083(3) 0.5583(4) 0.27379(13) 0.0376(6) Uani 1 1 d . . .
H2C H 0.1423 0.5616 0.3313 0.045 Uiso 1 1 d R . .
H2D H 0.0457 0.4148 0.2588 0.045 Uiso 0.50 1 d PR A 1
H2B H 0.0303 0.6877 0.2560 0.045 Uiso 0.50 1 d PR B 2
N1 N 0.7241(3) 0.6397(4) 0.46970(15) 0.0290(6) Uani 1 1 d . . .
H1 H 0.7313 0.8041 0.4833 0.035 Uiso 1 1 calc R . .
N3 N 0.7464(4) 0.2215(4) 0.48246(16) 0.0330(7) Uani 1 1 d . . .
N4 N 0.6719(3) 0.2741(4) 0.39262(15) 0.0307(6) Uani 1 1 d . . .
Li1 Li 0.3667(7) 0.5319(9) 0.2194(3) 0.0307(11) Uani 1 1 d . . .


_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. 
;

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 1.310(3) . ?
N2 N1 1.364(3) . ?
O1 C1 1.281(3) . ?
O1 Li1 1.928(5) 2_655 ?
O1 Li1 1.978(5) . ?
C1 N4 1.361(4) . ?
C1 N1 1.370(3) . ?
O2 Li1 2.015(5) . ?
O2 H2C 0.8500 . ?
O2 H2D 0.8500 . ?
O2 H2B 0.8500 . ?
N1 H1 0.8600 . ?
N3 N4 1.374(3) . ?
N4 Li1 2.057(5) 2_645 ?
Li1 O1 1.928(5) 2_645 ?
Li1 N4 2.057(5) 2_655 ?
Li1 Li1 3.139(5) 2_655 ?
Li1 Li1 3.139(5) 2_645 ?

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 106.2(2) . . ?
C1 O1 Li1 131.3(2) . 2_655 ?
C1 O1 Li1 120.5(2) . . ?
Li1 O1 Li1 106.98(17) 2_655 . ?
O1 C1 N4 126.8(2) . . ?
O1 C1 N1 127.0(2) . . ?
N4 C1 N1 106.2(2) . . ?
Li1 O2 H2C 108.3 . . ?
Li1 O2 H2D 104.1 . . ?
H2C O2 H2D 108.4 . . ?
Li1 O2 H2B 115.8 . . ?
H2C O2 H2B 110.0 . . ?
H2D O2 H2B 110.0 . . ?
N2 N1 C1 109.8(2) . . ?
N2 N1 H1 125.1 . . ?
C1 N1 H1 125.1 . . ?
N2 N3 N4 111.0(2) . . ?
C1 N4 N3 106.8(2) . . ?
C1 N4 Li1 121.9(2) . 2_645 ?
N3 N4 Li1 130.6(2) . 2_645 ?
O1 Li1 O1 112.9(2) 2_645 . ?
O1 Li1 O2 109.2(2) 2_645 . ?
O1 Li1 O2 106.2(2) . . ?
O1 Li1 N4 112.1(2) 2_645 2_655 ?
O1 Li1 N4 109.2(2) . 2_655 ?
O2 Li1 N4 107.0(2) . 2_655 ?
O1 Li1 Li1 138.3(3) 2_645 2_655 ?
O1 Li1 Li1 35.97(15) . 2_655 ?
O2 Li1 Li1 107.4(2) . 2_655 ?
N4 Li1 Li1 74.75(14) 2_655 2_655 ?
O1 Li1 Li1 37.05(6) 2_645 2_645 ?
O1 Li1 Li1 76.7(2) . 2_645 ?
O2 Li1 Li1 114.0(2) . 2_645 ?
N4 Li1 Li1 135.0(3) 2_655 2_645 ?
Li1 Li1 Li1 108.2(3) 2_655 2_645 ?

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
Li1 O1 C1 N4 -158.9(3) 2_655 . . . ?
Li1 O1 C1 N4 35.6(4) . . . . ?
Li1 O1 C1 N1 20.5(4) 2_655 . . . ?
Li1 O1 C1 N1 -145.0(3) . . . . ?
N3 N2 N1 C1 0.3(3) . . . . ?
O1 C1 N1 N2 179.7(2) . . . . ?
N4 C1 N1 N2 -0.8(3) . . . . ?
N1 N2 N3 N4 0.3(3) . . . . ?
O1 C1 N4 N3 -179.6(2) . . . . ?
N1 C1 N4 N3 0.9(3) . . . . ?
O1 C1 N4 Li1 9.6(4) . . . 2_645 ?
N1 C1 N4 Li1 -169.9(2) . . . 2_645 ?
N2 N3 N4 C1 -0.8(3) . . . . ?
N2 N3 N4 Li1 169.0(2) . . . 2_645 ?
C1 O1 Li1 O1 -48.4(3) . . . 2_645 ?
Li1 O1 Li1 O1 142.9(3) 2_655 . . 2_645 ?
C1 O1 Li1 O2 71.2(3) . . . . ?
Li1 O1 Li1 O2 -97.49(17) 2_655 . . . ?
C1 O1 Li1 N4 -173.8(2) . . . 2_655 ?
Li1 O1 Li1 N4 17.5(2) 2_655 . . 2_655 ?
C1 O1 Li1 Li1 168.7(3) . . . 2_655 ?
C1 O1 Li1 Li1 -40.4(3) . . . 2_645 ?
Li1 O1 Li1 Li1 151.0(2) 2_655 . . 2_645 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_140715c
_database_code_depnum_ccdc_archive 'CCDC 1018912'
_audit_update_record             
;
2017-05-25 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Barium 5-oxotetrazolate dehydrate'
_chemical_formula_moiety         '0.25(C8 H24 Ba4 N32 O16)'
_chemical_formula_sum            'C2 H6 Ba N8 O4'
_chemical_formula_weight         343.49
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   15.4882(13)
_cell_length_b                   6.3340(5)
_cell_length_c                   9.3181(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.545(2)
_cell_angle_gamma                90
_cell_volume                     871.60(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.208
_cell_measurement_theta_min      2.292
_shelx_estimated_absorpt_T_max   0.588
_shelx_estimated_absorpt_T_min   0.331
_exptl_absorpt_coefficient_mu    4.573
_exptl_absorpt_correction_T_max  0.5879
_exptl_absorpt_correction_T_min  0.3314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_min         2.759
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                728
_reflns_number_total             769
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.705
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         769
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²+2.0705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0931
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.563(4)
 0.437(4)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All O(H,H) groups
3.a Riding coordinates:
 O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Ba1 Ba 0.5000 0.64215(8) 0.2500 0.0151(2) Uani 1 2 d S T P . .
C1 C 0.1925(5) 0.5291(10) 0.3513(17) 0.0171(14) Uani 1 1 d . . . . .
N1 N 0.2443(5) 0.5966(11) 0.2702(7) 0.0206(17) Uani 1 1 d . . . . .
N2 N 0.3312(6) 0.5904(13) 0.3587(8) 0.0218(16) Uani 1 1 d . . . . .
N3 N 0.3355(5) 0.5221(11) 0.4943(8) 0.0171(16) Uani 1 1 d . . . . .
N4 N 0.2499(5) 0.4879(10) 0.4909(8) 0.0144(17) Uani 1 1 d . . . . .
H4 H 0.2333 0.4457 0.5663 0.017 Uiso 1 1 calc R . . . .
O1 O 0.1068(3) 0.5051(9) 0.3091(13) 0.0255(11) Uani 1 1 d . . . . .
O2 O 0.5107(4) 0.2562(9) 0.0682(6) 0.0256(13) Uani 1 1 d . . . . .
H2A H 0.5544 0.2023 0.1348 0.031 Uiso 1 1 d R . . . .
H2B H 0.4657 0.2023 0.0868 0.031 Uiso 1 1 d R . . . .


_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.
;
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
Ba1 N2 3.093(8) . ?
Ba1 N2 3.093(8) 2_655 ?
Ba1 N3 3.096(7) 5_666 ?
Ba1 N3 3.096(7) 6_565 ?
Ba1 O1 2.788(5) 4 ?
Ba1 O1 2.788(5) 3 ?
Ba1 O2 2.990(5) 6_566 ?
Ba1 O2 2.990(5) 5_665 ?
Ba1 O2 3.007(6) 2_655 ?
Ba1 O2 3.007(6) . ?
C1 N1 1.327(14) . ?
C1 N4 1.361(15) . ?
C1 O1 1.275(8) . ?
N1 N2 1.350(11) . ?
N2 N3 1.318(9) . ?
N3 Ba1 3.096(7) 5_666 ?
N3 N4 1.335(11) . ?
N4 H4 0.8600 . ?
O1 Ba1 2.788(5) 3_445 ?
O2 Ba1 2.990(5) 5_665 ?
O2 H2A 0.8401 . ?
O2 H2B 0.8400 . ?

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 Ba1 N2 167.8(3) 2_655 . ?
N2 Ba1 N3 68.64(17) . 6_565 ?
N2 Ba1 N3 68.64(17) 2_655 5_666 ?
N2 Ba1 N3 107.04(16) 2_655 6_565 ?
N2 Ba1 N3 107.04(16) . 5_666 ?
N3 Ba1 N3 140.7(3) 6_565 5_666 ?
O1 Ba1 N2 122.2(3) 3 . ?
O1 Ba1 N2 69.0(2) 3 2_655 ?
O1 Ba1 N2 122.2(3) 4 2_655 ?
O1 Ba1 N2 69.0(2) 4 . ?
O1 Ba1 N3 136.9(2) 4 5_666 ?
O1 Ba1 N3 79.8(2) 3 5_666 ?
O1 Ba1 N3 79.8(2) 4 6_565 ?
O1 Ba1 N3 136.9(2) 3 6_565 ?
O1 Ba1 O1 68.9(2) 3 4 ?
O1 Ba1 O2 82.6(3) 3 5_665 ?
O1 Ba1 O2 130.6(2) 4 2_655 ?
O1 Ba1 O2 130.6(2) 3 . ?
O1 Ba1 O2 77.0(3) 3 6_566 ?
O1 Ba1 O2 77.0(3) 4 5_665 ?
O1 Ba1 O2 82.6(3) 4 6_566 ?
O1 Ba1 O2 133.6(2) 4 . ?
O1 Ba1 O2 133.6(2) 3 2_655 ?
O2 Ba1 N2 123.22(18) 6_566 2_655 ?
O2 Ba1 N2 59.85(18) 5_665 2_655 ?
O2 Ba1 N2 59.86(18) 6_566 . ?
O2 Ba1 N2 107.09(19) 2_655 2_655 ?
O2 Ba1 N2 107.09(19) . . ?
O2 Ba1 N2 62.2(2) 2_655 . ?
O2 Ba1 N2 62.2(2) . 2_655 ?
O2 Ba1 N2 123.22(18) 5_665 . ?
O2 Ba1 N3 61.46(17) 6_566 5_666 ?
O2 Ba1 N3 61.46(17) 5_665 6_565 ?
O2 Ba1 N3 128.49(17) 6_566 6_565 ?
O2 Ba1 N3 128.49(17) 5_665 5_666 ?
O2 Ba1 N3 57.71(18) . 6_565 ?
O2 Ba1 N3 57.71(18) 2_655 5_666 ?
O2 Ba1 N3 89.31(17) . 5_666 ?
O2 Ba1 N3 89.31(17) 2_655 6_565 ?
O2 Ba1 O2 71.23(19) 2_655 . ?
O2 Ba1 O2 67.19(17) 5_665 . ?
O2 Ba1 O2 67.19(17) 6_566 2_655 ?
O2 Ba1 O2 137.54(11) 5_665 2_655 ?
O2 Ba1 O2 155.1(2) 6_566 5_665 ?
O2 Ba1 O2 137.54(11) 6_566 . ?
N1 C1 N4 105.9(6) . . ?
O1 C1 N1 127.9(14) . . ?
O1 C1 N4 126.2(14) . . ?
C1 N1 N2 107.8(7) . . ?
N1 N2 Ba1 125.6(5) . . ?
N3 N2 Ba1 123.0(6) . . ?
N3 N2 N1 110.4(8) . . ?
N2 N3 Ba1 129.8(6) . 5_666 ?
N2 N3 N4 105.5(8) . . ?
N4 N3 Ba1 123.0(5) . 5_666 ?
C1 N4 H4 124.8 . . ?
N3 N4 C1 110.5(7) . . ?
N3 N4 H4 124.8 . . ?
C1 O1 Ba1 131.3(5) . 3_445 ?
Ba1 O2 Ba1 112.81(17) 5_665 . ?
Ba1 O2 H2A 94.8 . . ?
Ba1 O2 H2A 127.7 5_665 . ?
Ba1 O2 H2B 119.4 5_665 . ?
Ba1 O2 H2B 91.4 . . ?
H2A O2 H2B 102.4 . . ?

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
Ba1 N2 N3 Ba1 -4.7(11) . . . 5_666 ?
Ba1 N2 N3 N4 -170.0(4) . . . . ?
Ba1 N3 N4 C1 -164.7(5) 5_666 . . . ?
C1 N1 N2 Ba1 168.3(5) . . . . ?
C1 N1 N2 N3 -0.5(10) . . . . ?
N1 C1 N4 N3 -2.2(9) . . . . ?
N1 C1 O1 Ba1 106.9(10) . . . 3_445 ?
N1 N2 N3 Ba1 164.5(5) . . . 5_666 ?
N1 N2 N3 N4 -0.8(10) . . . . ?
N2 N3 N4 C1 1.8(9) . . . . ?
N4 C1 N1 N2 1.6(9) . . . . ?
N4 C1 O1 Ba1 -72.6(17) . . . 3_445 ?
O1 C1 N1 N2 -177.9(9) . . . . ?
O1 C1 N4 N3 177.4(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.563(4)
2 0.437(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_140630a
_database_code_depnum_ccdc_archive 'CCDC 1018907'
_audit_update_record             
;
2017-05-25 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Rubidium 5-oxotetrazolate'
_chemical_formula_moiety         'C H N4 O Rb'
_chemical_formula_sum            'C H N4 O Rb'
_chemical_formula_weight         170.53
_chemical_melting_point          ?
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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.9480(3)
_cell_length_b                   7.1191(6)
_cell_length_c                   7.4189(7)
_cell_angle_alpha                67.2890(10)
_cell_angle_beta                 71.8880(10)
_cell_angle_gamma                89.451(2)
_cell_volume                     227.30(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    733
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.442
_cell_measurement_theta_min      3.148
_shelx_estimated_absorpt_T_max   0.359
_shelx_estimated_absorpt_T_min   0.079
_exptl_absorpt_coefficient_mu    10.755
_exptl_absorpt_correction_T_max  0.3585
_exptl_absorpt_correction_T_min  0.0789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             160
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1155
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.433
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                673
_reflns_number_total             786
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.839
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.532
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         786
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.1196
_refine_ls_restrained_S_all      1.334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2932
_refine_ls_wR_factor_ref         0.3052
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Rb1 Rb 0.8805(3) 1.0794(2) 0.2339(2) 0.0355(9) Uani 1 1 d . . . . .
N1 N 0.814(3) 0.4471(18) 0.747(2) 0.030(3) Uani 1 1 d . . . . .
H1 H 0.9914 0.4782 0.7257 0.036 Uiso 1 1 calc R . . . .
N2 N 0.676(3) 0.254(2) 0.819(2) 0.039(3) Uani 1 1 d . . . . .
N3 N 0.417(3) 0.2700(19) 0.821(2) 0.039(3) Uani 1 1 d . . . . .
N4 N 0.371(3) 0.4680(19) 0.761(2) 0.031(3) Uani 1 1 d . . . . .
O1 O 0.674(2) 0.7748(15) 0.6493(18) 0.037(3) Uani 1 1 d . . . . .
C1 C 0.617(3) 0.583(2) 0.713(2) 0.028(3) Uani 1 1 d . . . . .


_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.
;
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
Rb1 N1 3.668(14) 1_564 ?
Rb1 N2 3.317(15) 1_564 ?
Rb1 N2 3.268(15) 2_766 ?
Rb1 N3 3.120(14) 2_666 ?
Rb1 N3 3.173(15) 1_664 ?
Rb1 N4 3.634(13) 1_664 ?
Rb1 N4 3.454(12) 2_676 ?
Rb1 O1 2.936(11) 2_776 ?
Rb1 O1 2.858(11) . ?
Rb1 O1 2.918(11) 2_676 ?
Rb1 C1 3.463(15) 2_676 ?
Rb1 C1 3.681(16) 2_776 ?
N1 Rb1 3.668(14) 1_546 ?
N1 H1 0.8600 . ?
N1 N2 1.365(19) . ?
N1 C1 1.376(18) . ?
N2 Rb1 3.317(15) 1_546 ?
N2 Rb1 3.268(15) 2_766 ?
N2 N3 1.284(19) . ?
N3 Rb1 3.120(14) 2_666 ?
N3 Rb1 3.173(14) 1_446 ?
N3 N4 1.344(17) . ?
N4 Rb1 3.634(13) 1_446 ?
N4 Rb1 3.454(12) 2_676 ?
N4 C1 1.35(2) . ?
O1 Rb1 2.936(11) 2_776 ?
O1 Rb1 2.918(11) 2_676 ?
O1 C1 1.259(19) . ?
C1 Rb1 3.463(15) 2_676 ?
C1 Rb1 3.681(16) 2_776 ?

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 Rb1 C1 97.2(3) 1_564 2_776 ?
N2 Rb1 N1 114.5(3) 2_766 1_564 ?
N2 Rb1 N1 21.8(3) 1_564 1_564 ?
N2 Rb1 N2 107.5(3) 2_766 1_564 ?
N2 Rb1 N4 160.6(3) 2_766 2_676 ?
N2 Rb1 N4 77.6(3) 1_564 2_676 ?
N2 Rb1 N4 88.8(3) 2_766 1_664 ?
N2 Rb1 N4 62.3(3) 1_564 1_664 ?
N2 Rb1 C1 176.8(3) 2_766 2_676 ?
N2 Rb1 C1 95.5(4) 2_766 2_776 ?
N2 Rb1 C1 70.8(3) 1_564 2_676 ?
N2 Rb1 C1 118.9(4) 1_564 2_776 ?
N3 Rb1 N1 89.2(4) 2_666 1_564 ?
N3 Rb1 N1 58.1(3) 1_664 1_564 ?
N3 Rb1 N2 70.1(4) 2_666 2_766 ?
N3 Rb1 N2 68.8(4) 1_664 1_564 ?
N3 Rb1 N2 67.6(4) 2_666 1_564 ?
N3 Rb1 N2 67.6(3) 1_664 2_766 ?
N3 Rb1 N3 103.5(3) 2_666 1_664 ?
N3 Rb1 N4 21.4(3) 1_664 1_664 ?
N3 Rb1 N4 115.5(4) 2_666 1_664 ?
N3 Rb1 N4 98.2(3) 1_664 2_676 ?
N3 Rb1 N4 127.9(3) 2_666 2_676 ?
N3 Rb1 C1 165.7(3) 2_666 2_776 ?
N3 Rb1 C1 106.7(4) 2_666 2_676 ?
N3 Rb1 C1 69.7(3) 1_664 2_776 ?
N3 Rb1 C1 113.7(3) 1_664 2_676 ?
N4 Rb1 N1 45.1(3) 1_664 1_564 ?
N4 Rb1 N1 63.8(3) 2_676 1_564 ?
N4 Rb1 N4 76.9(3) 2_676 1_664 ?
N4 Rb1 C1 62.6(3) 1_664 2_776 ?
N4 Rb1 C1 66.3(3) 2_676 2_776 ?
N4 Rb1 C1 22.4(3) 2_676 2_676 ?
O1 Rb1 N1 113.2(3) 2_776 1_564 ?
O1 Rb1 N1 74.6(3) 2_676 1_564 ?
O1 Rb1 N1 155.3(3) . 1_564 ?
O1 Rb1 N2 138.3(3) . 1_564 ?
O1 Rb1 N2 72.6(3) 2_676 1_564 ?
O1 Rb1 N2 81.4(3) . 2_766 ?
O1 Rb1 N2 81.7(3) 2_776 2_766 ?
O1 Rb1 N2 134.2(3) 2_776 1_564 ?
O1 Rb1 N2 156.8(3) 2_676 2_766 ?
O1 Rb1 N3 89.3(3) 2_676 2_666 ?
O1 Rb1 N3 130.2(3) 2_676 1_664 ?
O1 Rb1 N3 74.5(4) 2_776 1_664 ?
O1 Rb1 N3 145.5(3) . 1_664 ?
O1 Rb1 N3 149.7(3) 2_776 2_666 ?
O1 Rb1 N3 78.3(4) . 2_666 ?
O1 Rb1 N4 81.6(3) 2_776 2_676 ?
O1 Rb1 N4 159.2(3) . 1_664 ?
O1 Rb1 N4 42.6(3) 2_676 2_676 ?
O1 Rb1 N4 107.7(3) . 2_676 ?
O1 Rb1 N4 73.5(3) 2_776 1_664 ?
O1 Rb1 N4 110.5(3) 2_676 1_664 ?
O1 Rb1 O1 86.9(3) . 2_776 ?
O1 Rb1 O1 84.0(3) . 2_676 ?
O1 Rb1 O1 115.4(4) 2_676 2_776 ?
O1 Rb1 C1 98.1(3) . 2_676 ?
O1 Rb1 C1 20.6(3) 2_676 2_676 ?
O1 Rb1 C1 101.4(3) 2_776 2_676 ?
O1 Rb1 C1 104.7(3) 2_676 2_776 ?
O1 Rb1 C1 100.0(3) . 2_776 ?
O1 Rb1 C1 17.8(3) 2_776 2_776 ?
C1 Rb1 N1 65.0(3) 2_676 1_564 ?
C1 Rb1 N4 92.7(3) 2_676 1_664 ?
C1 Rb1 C1 87.6(4) 2_676 2_776 ?
Rb1 N1 H1 79.6 1_546 . ?
N2 N1 Rb1 64.5(9) . 1_546 ?
N2 N1 H1 126.1 . . ?
N2 N1 C1 107.9(12) . . ?
C1 N1 Rb1 130.1(10) . 1_546 ?
C1 N1 H1 126.1 . . ?
Rb1 N2 Rb1 72.5(3) 2_766 1_546 ?
N1 N2 Rb1 93.7(10) . 1_546 ?
N1 N2 Rb1 112.6(9) . 2_766 ?
N3 N2 Rb1 125.5(11) . 1_546 ?
N3 N2 Rb1 134.2(11) . 2_766 ?
N3 N2 N1 107.9(12) . . ?
Rb1 N3 Rb1 76.5(3) 2_666 1_446 ?
N2 N3 Rb1 122.7(11) . 1_446 ?
N2 N3 Rb1 115.9(10) . 2_666 ?
N2 N3 N4 110.0(12) . . ?
N4 N3 Rb1 98.9(9) . 1_446 ?
N4 N3 Rb1 127.8(10) . 2_666 ?
Rb1 N4 Rb1 103.1(3) 2_676 1_446 ?
N3 N4 Rb1 59.6(8) . 1_446 ?
N3 N4 Rb1 162.0(10) . 2_676 ?
N3 N4 C1 108.7(12) . . ?
C1 N4 Rb1 134.7(10) . 1_446 ?
C1 N4 Rb1 79.2(8) . 2_676 ?
Rb1 O1 Rb1 115.4(4) 2_676 2_776 ?
Rb1 O1 Rb1 93.1(3) . 2_776 ?
Rb1 O1 Rb1 96.0(3) . 2_676 ?
C1 O1 Rb1 104.9(9) . 2_676 ?
C1 O1 Rb1 116.9(9) . 2_776 ?
C1 O1 Rb1 129.3(10) . . ?
Rb1 C1 Rb1 87.6(4) 2_676 2_776 ?
N1 C1 Rb1 83.4(8) . 2_776 ?
N1 C1 Rb1 163.3(11) . 2_676 ?
N4 C1 Rb1 78.4(8) . 2_676 ?
N4 C1 Rb1 157.6(10) . 2_776 ?
N4 C1 N1 105.4(13) . . ?
O1 C1 Rb1 54.5(7) . 2_676 ?
O1 C1 Rb1 45.3(7) . 2_776 ?
O1 C1 N1 124.0(13) . . ?
O1 C1 N4 130.5(13) . . ?

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
Rb1 N1 N2 Rb1 -72.6(6) 1_546 . . 2_766 ?
Rb1 N1 N2 N3 129.3(14) 1_546 . . . ?
Rb1 N1 C1 Rb1 86.1(9) 1_546 . . 2_776 ?
Rb1 N1 C1 Rb1 28(4) 1_546 . . 2_676 ?
Rb1 N1 C1 N4 -73.0(15) 1_546 . . . ?
Rb1 N1 C1 O1 107.3(15) 1_546 . . . ?
Rb1 N2 N3 Rb1 -100.0(12) 1_546 . . 2_666 ?
Rb1 N2 N3 Rb1 0.3(19) 2_766 . . 2_666 ?
Rb1 N2 N3 Rb1 -9.9(16) 1_546 . . 1_446 ?
Rb1 N2 N3 Rb1 90.5(16) 2_766 . . 1_446 ?
Rb1 N2 N3 N4 -154.1(11) 2_766 . . . ?
Rb1 N2 N3 N4 105.6(13) 1_546 . . . ?
Rb1 N3 N4 Rb1 97(3) 2_666 . . 2_676 ?
Rb1 N3 N4 Rb1 18(3) 1_446 . . 2_676 ?
Rb1 N3 N4 Rb1 79.8(9) 2_666 . . 1_446 ?
Rb1 N3 N4 C1 131.4(10) 1_446 . . . ?
Rb1 N3 N4 C1 -148.8(10) 2_666 . . . ?
Rb1 N4 C1 Rb1 -46(3) 1_446 . . 2_776 ?
Rb1 N4 C1 Rb1 52(3) 2_676 . . 2_776 ?
Rb1 N4 C1 Rb1 -97.9(10) 1_446 . . 2_676 ?
Rb1 N4 C1 N1 65.5(16) 1_446 . . . ?
Rb1 N4 C1 N1 163.3(11) 2_676 . . . ?
Rb1 N4 C1 O1 -17.0(16) 2_676 . . . ?
Rb1 N4 C1 O1 -114.9(17) 1_446 . . . ?
Rb1 O1 C1 Rb1 119.6(13) . . . 2_776 ?
Rb1 O1 C1 Rb1 -111.1(10) . . . 2_676 ?
Rb1 O1 C1 Rb1 -129.3(10) 2_676 . . 2_776 ?
Rb1 O1 C1 Rb1 129.3(10) 2_776 . . 2_676 ?
Rb1 O1 C1 N1 89.2(17) . . . . ?
Rb1 O1 C1 N1 -30(2) 2_776 . . . ?
Rb1 O1 C1 N1 -159.8(13) 2_676 . . . ?
Rb1 O1 C1 N4 -90.4(19) . . . . ?
Rb1 O1 C1 N4 21(2) 2_676 . . . ?
Rb1 O1 C1 N4 149.9(14) 2_776 . . . ?
N1 N2 N3 Rb1 -118.2(11) . . . 1_446 ?
N1 N2 N3 Rb1 151.6(11) . . . 2_666 ?
N1 N2 N3 N4 -3(2) . . . . ?
N2 N1 C1 Rb1 99(4) . . . 2_676 ?
N2 N1 C1 Rb1 157.4(12) . . . 2_776 ?
N2 N1 C1 N4 -1.6(16) . . . . ?
N2 N1 C1 O1 178.7(16) . . . . ?
N2 N3 N4 Rb1 -112(3) . . . 2_676 ?
N2 N3 N4 Rb1 -129.7(16) . . . 1_446 ?
N2 N3 N4 C1 2(2) . . . . ?
N3 N4 C1 Rb1 -163.3(12) . . . 2_676 ?
N3 N4 C1 Rb1 -111(3) . . . 2_776 ?
N3 N4 C1 N1 0.0(17) . . . . ?
N3 N4 C1 O1 179.7(16) . . . . ?
C1 N1 N2 Rb1 160.9(10) . . . 2_766 ?
C1 N1 N2 Rb1 -126.5(11) . . . 1_546 ?
C1 N1 N2 N3 2.7(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_140719i
_database_code_depnum_ccdc_archive 'CCDC 1018916'
_audit_update_record             
;
2014-08-11 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H12 N8 O7 Sr'
_chemical_formula_weight         347.82

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnnm

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

_cell_length_a                   11.2966(9)
_cell_length_b                   14.7871(13)
_cell_length_c                   6.9961(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1168.66(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2973
_cell_measurement_theta_min      2.284
_cell_measurement_theta_max      28.348

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    4.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2572
_exptl_absorpt_correction_T_max  0.5227
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5475
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1125
_reflns_number_gt                979
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0444P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1125
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Sr1 Sr 0.56124(3) 0.64003(2) 0.5000 0.0189(2) Uani 1 2 d S . .
N1 N 0.8404(3) 0.4882(2) 0.5000 0.0228(7) Uani 1 2 d S . .
H1 H 0.8854 0.5351 0.5000 0.027 Uiso 1 2 calc SR . .
N2 N 0.7198(3) 0.4896(2) 0.5000 0.0240(8) Uani 1 2 d S . .
N3 N 0.6864(3) 0.4049(2) 0.5000 0.0258(8) Uani 1 2 d S . .
N4 N 0.7809(3) 0.3475(2) 0.5000 0.0274(9) Uani 1 2 d S . .
N5 N 0.5982(3) 0.9058(2) 0.5000 0.0231(8) Uani 1 2 d S . .
H5 H 0.5223 0.9102 0.5000 0.028 Uiso 1 2 calc SR . .
N6 N 0.6594(3) 0.8268(2) 0.5000 0.0257(8) Uani 1 2 d S . .
N7 N 0.7702(3) 0.8493(2) 0.5000 0.0315(9) Uani 1 2 d S . .
N8 N 0.7851(3) 0.9419(2) 0.5000 0.0276(8) Uani 1 2 d S . .
O1 O 0.9879(3) 0.3759(2) 0.5000 0.0305(7) Uani 1 2 d S . .
O2 O 0.6450(2) 1.06035(19) 0.5000 0.0287(7) Uani 1 2 d S . .
O3 O 0.5000 0.5000 0.2542(3) 0.0265(7) Uani 1 2 d S . .
H3 H 0.5581 0.4852 0.1837 0.032 Uiso 1 1 d R . .
O4 O 0.45652(18) 0.73512(18) 0.2510(3) 0.0445(7) Uani 1 1 d . . .
H4C H 0.4030 0.7069 0.1898 0.053 Uiso 1 1 d R . .
H4D H 0.4789 0.7797 0.1835 0.053 Uiso 1 1 d R . .
O5 O 0.7155(2) 0.66574(15) 0.7606(3) 0.0441(6) Uani 1 1 d . . .
H5C H 0.7576 0.6300 0.8271 0.053 Uiso 1 1 d R . .
H5D H 0.7129 0.7165 0.8175 0.053 Uiso 1 1 d R . .
C1 C 0.8786(3) 0.4013(3) 0.5000 0.0210(9) Uani 1 2 d S . .
C2 C 0.6743(3) 0.9769(3) 0.5000 0.0197(9) Uani 1 2 d S . .


_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. 
;

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
Sr1 O4 2.532(2) . ?
Sr1 O4 2.532(2) 6_556 ?
Sr1 O5 2.551(2) . ?
Sr1 O5 2.551(2) 6_556 ?
Sr1 O3 2.7789(15) . ?
Sr1 O3 2.7789(15) 5_666 ?
Sr1 N2 2.856(3) . ?
Sr1 N3 2.875(3) 5_666 ?
Sr1 N6 2.977(4) . ?
Sr1 Sr1 4.3663(8) 5_666 ?
N1 C1 1.355(5) . ?
N1 N2 1.363(4) . ?
N1 H1 0.8600 . ?
N2 N3 1.308(5) . ?
N3 N4 1.364(5) . ?
N3 Sr1 2.875(3) 5_666 ?
N4 C1 1.360(5) . ?
N5 N6 1.357(5) . ?
N5 C2 1.358(5) . ?
N5 H5 0.8600 . ?
N6 N7 1.295(5) . ?
N7 N8 1.379(5) . ?
N8 C2 1.355(5) . ?
O1 C1 1.290(5) . ?
O2 C2 1.277(5) . ?
O3 Sr1 2.7789(15) 5_666 ?
O3 H3 0.8500 . ?
O4 H4C 0.8500 . ?
O4 H4D 0.8499 . ?
O5 H5C 0.8500 . ?
O5 H5D 0.8500 . ?

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
O4 Sr1 O4 86.93(12) . 6_556 ?
O4 Sr1 O5 136.74(8) . . ?
O4 Sr1 O5 75.21(7) 6_556 . ?
O4 Sr1 O5 75.21(7) . 6_556 ?
O4 Sr1 O5 136.74(8) 6_556 6_556 ?
O5 Sr1 O5 91.26(12) . 6_556 ?
O4 Sr1 O3 82.64(7) . . ?
O4 Sr1 O3 136.31(5) 6_556 . ?
O5 Sr1 O3 136.34(6) . . ?
O5 Sr1 O3 80.73(6) 6_556 . ?
O4 Sr1 O3 136.31(5) . 5_666 ?
O4 Sr1 O3 82.64(7) 6_556 5_666 ?
O5 Sr1 O3 80.73(6) . 5_666 ?
O5 Sr1 O3 136.34(6) 6_556 5_666 ?
O3 Sr1 O3 76.44(8) . 5_666 ?
O4 Sr1 N2 136.52(6) . . ?
O4 Sr1 N2 136.52(6) 6_556 . ?
O5 Sr1 N2 71.80(7) . . ?
O5 Sr1 N2 71.80(7) 6_556 . ?
O3 Sr1 N2 64.89(5) . . ?
O3 Sr1 N2 64.89(5) 5_666 . ?
O4 Sr1 N3 70.96(7) . 5_666 ?
O4 Sr1 N3 70.96(7) 6_556 5_666 ?
O5 Sr1 N3 134.36(6) . 5_666 ?
O5 Sr1 N3 134.36(6) 6_556 5_666 ?
O3 Sr1 N3 65.52(5) . 5_666 ?
O3 Sr1 N3 65.52(5) 5_666 5_666 ?
N2 Sr1 N3 115.47(9) . 5_666 ?
O4 Sr1 N6 70.05(7) . . ?
O4 Sr1 N6 70.05(7) 6_556 . ?
O5 Sr1 N6 66.86(7) . . ?
O5 Sr1 N6 66.86(7) 6_556 . ?
O3 Sr1 N6 141.65(4) . . ?
O3 Sr1 N6 141.65(4) 5_666 . ?
N2 Sr1 N6 119.28(9) . . ?
N3 Sr1 N6 125.25(9) 5_666 . ?
O4 Sr1 Sr1 112.25(6) . 5_666 ?
O4 Sr1 Sr1 112.25(6) 6_556 5_666 ?
O5 Sr1 Sr1 110.97(5) . 5_666 ?
O5 Sr1 Sr1 110.97(5) 6_556 5_666 ?
O3 Sr1 Sr1 38.22(4) . 5_666 ?
O3 Sr1 Sr1 38.22(4) 5_666 5_666 ?
N2 Sr1 Sr1 57.31(7) . 5_666 ?
N3 Sr1 Sr1 58.16(7) 5_666 5_666 ?
N6 Sr1 Sr1 176.59(7) . 5_666 ?
C1 N1 N2 109.4(3) . . ?
C1 N1 H1 125.3 . . ?
N2 N1 H1 125.3 . . ?
N3 N2 N1 105.9(3) . . ?
N3 N2 Sr1 124.4(2) . . ?
N1 N2 Sr1 129.7(3) . . ?
N2 N3 N4 111.7(3) . . ?
N2 N3 Sr1 120.1(2) . 5_666 ?
N4 N3 Sr1 128.1(2) . 5_666 ?
C1 N4 N3 105.7(3) . . ?
N6 N5 C2 110.1(3) . . ?
N6 N5 H5 124.9 . . ?
C2 N5 H5 124.9 . . ?
N7 N6 N5 105.7(3) . . ?
N7 N6 Sr1 126.8(3) . . ?
N5 N6 Sr1 127.5(2) . . ?
N6 N7 N8 111.9(3) . . ?
C2 N8 N7 105.5(3) . . ?
Sr1 O3 Sr1 103.56(8) . 5_666 ?
Sr1 O3 H3 111.1 . . ?
Sr1 O3 H3 111.0 5_666 . ?
Sr1 O4 H4C 114.0 . . ?
Sr1 O4 H4D 132.4 . . ?
H4C O4 H4D 108.2 . . ?
Sr1 O5 H5C 132.9 . . ?
Sr1 O5 H5D 116.3 . . ?
H5C O5 H5D 108.2 . . ?
O1 C1 N1 125.4(4) . . ?
O1 C1 N4 127.3(4) . . ?
N1 C1 N4 107.2(3) . . ?
O2 C2 N8 127.5(4) . . ?
O2 C2 N5 125.8(4) . . ?
N8 C2 N5 106.7(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 0.0 . . . . ?
C1 N1 N2 Sr1 180.0 . . . . ?
O4 Sr1 N2 N3 -88.70(10) . . . . ?
O4 Sr1 N2 N3 88.70(10) 6_556 . . . ?
O5 Sr1 N2 N3 131.19(6) . . . . ?
O5 Sr1 N2 N3 -131.19(6) 6_556 . . . ?
O3 Sr1 N2 N3 -43.10(5) . . . . ?
O3 Sr1 N2 N3 43.10(5) 5_666 . . . ?
N3 Sr1 N2 N3 0.0 5_666 . . . ?
N6 Sr1 N2 N3 180.0 . . . . ?
Sr1 Sr1 N2 N3 0.0 5_666 . . . ?
O4 Sr1 N2 N1 91.30(10) . . . . ?
O4 Sr1 N2 N1 -91.30(10) 6_556 . . . ?
O5 Sr1 N2 N1 -48.81(6) . . . . ?
O5 Sr1 N2 N1 48.81(6) 6_556 . . . ?
O3 Sr1 N2 N1 136.90(5) . . . . ?
O3 Sr1 N2 N1 -136.90(5) 5_666 . . . ?
N3 Sr1 N2 N1 180.0 5_666 . . . ?
N6 Sr1 N2 N1 0.0 . . . . ?
Sr1 Sr1 N2 N1 180.0 5_666 . . . ?
N1 N2 N3 N4 0.0 . . . . ?
Sr1 N2 N3 N4 180.0 . . . . ?
N1 N2 N3 Sr1 180.0 . . . 5_666 ?
Sr1 N2 N3 Sr1 0.0 . . . 5_666 ?
N2 N3 N4 C1 0.0 . . . . ?
Sr1 N3 N4 C1 180.0 5_666 . . . ?
C2 N5 N6 N7 0.0 . . . . ?
C2 N5 N6 Sr1 180.0 . . . . ?
O4 Sr1 N6 N7 -132.96(6) . . . . ?
O4 Sr1 N6 N7 132.96(6) 6_556 . . . ?
O5 Sr1 N6 N7 51.02(7) . . . . ?
O5 Sr1 N6 N7 -51.02(7) 6_556 . . . ?
O3 Sr1 N6 N7 -85.68(8) . . . . ?
O3 Sr1 N6 N7 85.68(8) 5_666 . . . ?
N2 Sr1 N6 N7 0.0 . . . . ?
N3 Sr1 N6 N7 180.0 5_666 . . . ?
Sr1 Sr1 N6 N7 0.0 5_666 . . . ?
O4 Sr1 N6 N5 47.04(6) . . . . ?
O4 Sr1 N6 N5 -47.04(6) 6_556 . . . ?
O5 Sr1 N6 N5 -128.98(7) . . . . ?
O5 Sr1 N6 N5 128.98(7) 6_556 . . . ?
O3 Sr1 N6 N5 94.32(8) . . . . ?
O3 Sr1 N6 N5 -94.32(8) 5_666 . . . ?
N2 Sr1 N6 N5 180.0 . . . . ?
N3 Sr1 N6 N5 0.0 5_666 . . . ?
Sr1 Sr1 N6 N5 180.0 5_666 . . . ?
N5 N6 N7 N8 0.0 . . . . ?
Sr1 N6 N7 N8 180.0 . . . . ?
N6 N7 N8 C2 0.0 . . . . ?
O4 Sr1 O3 Sr1 -141.37(5) . . . 5_666 ?
O4 Sr1 O3 Sr1 -63.69(9) 6_556 . . 5_666 ?
O5 Sr1 O3 Sr1 60.48(9) . . . 5_666 ?
O5 Sr1 O3 Sr1 142.50(6) 6_556 . . 5_666 ?
O3 Sr1 O3 Sr1 0.0 5_666 . . 5_666 ?
N2 Sr1 O3 Sr1 68.35(5) . . . 5_666 ?
N3 Sr1 O3 Sr1 -68.98(5) 5_666 . . 5_666 ?
N6 Sr1 O3 Sr1 174.50(11) . . . 5_666 ?
N2 N1 C1 O1 180.0 . . . . ?
N2 N1 C1 N4 0.0 . . . . ?
N3 N4 C1 O1 180.0 . . . . ?
N3 N4 C1 N1 0.0 . . . . ?
N7 N8 C2 O2 180.0 . . . . ?
N7 N8 C2 N5 0.0 . . . . ?
N6 N5 C2 O2 180.0 . . . . ?
N6 N5 C2 N8 0.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.119
####################################################################### 
# 
# 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_140714e
_database_code_depnum_ccdc_archive 'CCDC 1018911'
_audit_update_record             
;
2014-08-11 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C H K N4 O'
_chemical_formula_weight         124.16

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   4.1001(4)
_cell_length_b                   12.9476(11)
_cell_length_c                   8.1433(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.419(2)
_cell_angle_gamma                90.00
_cell_volume                     423.74(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    850
_cell_measurement_theta_min      2.998
_cell_measurement_theta_max      26.713

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             248
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7617
_exptl_absorpt_correction_T_max  0.8694
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2015
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             739
_reflns_number_gt                571
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0336P)²+0.0921P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         739
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0708
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
K1 K 0.18751(15) -0.00434(4) 0.77862(7) 0.0325(2) Uani 1 1 d . . .
N1 N 0.5979(6) 0.24028(16) 0.6868(3) 0.0327(6) Uani 1 1 d . . .
N2 N 0.6143(6) 0.14005(17) 0.6424(3) 0.0374(6) Uani 1 1 d . . .
N3 N 0.7438(6) 0.13113(16) 0.5110(3) 0.0352(6) Uani 1 1 d . . .
N4 N 0.8158(5) 0.22746(15) 0.4689(2) 0.0282(5) Uani 1 1 d . . .
H4 H 0.9065 0.2429 0.3855 0.034 Uiso 1 1 calc R . .
O1 O 0.7574(5) 0.39289(13) 0.5710(2) 0.0348(5) Uani 1 1 d . . .
C1 C 0.7259(6) 0.29673(19) 0.5757(3) 0.0248(6) Uani 1 1 d . . .


_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. 
;

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
K1 O1 2.7104(19) 2_646 ?
K1 O1 2.7352(18) 2_546 ?
K1 O1 2.7504(18) 4_566 ?
K1 N2 2.925(2) . ?
K1 N3 2.932(2) 3_656 ?
K1 N2 3.036(2) 1_455 ?
K1 N3 3.093(2) 1_455 ?
K1 C1 3.422(3) 2_546 ?
K1 K1 3.9901(12) 3_657 ?
K1 K1 4.1001(4) 1_655 ?
K1 K1 4.1001(4) 1_455 ?
K1 K1 4.1919(12) 3_557 ?
N1 C1 1.348(3) . ?
N1 N2 1.352(3) . ?
N2 N3 1.290(3) . ?
N2 K1 3.036(2) 1_655 ?
N3 N4 1.342(3) . ?
N3 K1 2.932(2) 3_656 ?
N3 K1 3.093(2) 1_655 ?
N4 C1 1.350(3) . ?
N4 H4 0.8600 . ?
O1 C1 1.253(3) . ?
O1 K1 2.7104(19) 2_656 ?
O1 K1 2.7352(18) 2_556 ?
O1 K1 2.7504(18) 4_665 ?
C1 K1 3.422(2) 2_556 ?

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
O1 K1 O1 97.69(6) 2_646 2_546 ?
O1 K1 O1 86.12(6) 2_646 4_566 ?
O1 K1 O1 80.33(6) 2_546 4_566 ?
O1 K1 N2 88.46(6) 2_646 . ?
O1 K1 N2 169.34(6) 2_546 . ?
O1 K1 N2 91.46(6) 4_566 . ?
O1 K1 N3 83.26(6) 2_646 3_656 ?
O1 K1 N3 105.45(6) 2_546 3_656 ?
O1 K1 N3 168.49(6) 4_566 3_656 ?
N2 K1 N3 83.85(6) . 3_656 ?
O1 K1 N2 170.92(6) 2_646 1_455 ?
O1 K1 N2 85.79(6) 2_546 1_455 ?
O1 K1 N2 86.20(6) 4_566 1_455 ?
N2 K1 N2 86.89(6) . 1_455 ?
N3 K1 N2 103.97(6) 3_656 1_455 ?
O1 K1 N3 157.05(6) 2_646 1_455 ?
O1 K1 N3 103.88(6) 2_546 1_455 ?
O1 K1 N3 104.98(6) 4_566 1_455 ?
N2 K1 N3 71.51(6) . 1_455 ?
N3 K1 N3 83.54(6) 3_656 1_455 ?
N2 K1 N3 24.28(5) 1_455 1_455 ?
O1 K1 C1 84.44(6) 2_646 2_546 ?
O1 K1 C1 19.72(5) 2_546 2_546 ?
O1 K1 C1 93.93(6) 4_566 2_546 ?
N2 K1 C1 170.77(6) . 2_546 ?
N3 K1 C1 89.45(6) 3_656 2_546 ?
N2 K1 C1 100.92(6) 1_455 2_546 ?
N3 K1 C1 114.11(6) 1_455 2_546 ?
O1 K1 K1 43.45(4) 2_646 3_657 ?
O1 K1 K1 88.57(4) 2_546 3_657 ?
O1 K1 K1 42.67(4) 4_566 3_657 ?
N2 K1 K1 89.96(5) . 3_657 ?
N3 K1 K1 126.57(5) 3_656 3_657 ?
N2 K1 K1 128.69(5) 1_455 3_657 ?
N3 K1 K1 143.49(5) 1_455 3_657 ?
C1 K1 K1 88.94(4) 2_546 3_657 ?
O1 K1 K1 41.38(4) 2_646 1_655 ?
O1 K1 K1 139.07(4) 2_546 1_655 ?
O1 K1 K1 93.86(4) 4_566 1_655 ?
N2 K1 K1 47.68(5) . 1_655 ?
N3 K1 K1 75.21(5) 3_656 1_655 ?
N2 K1 K1 134.57(4) 1_455 1_655 ?
N3 K1 K1 116.66(4) 1_455 1_655 ?
C1 K1 K1 124.33(4) 2_546 1_655 ?
K1 K1 K1 62.399(17) 3_657 1_655 ?
O1 K1 K1 138.62(4) 2_646 1_455 ?
O1 K1 K1 40.93(4) 2_546 1_455 ?
O1 K1 K1 86.14(4) 4_566 1_455 ?
N2 K1 K1 132.32(5) . 1_455 ?
N3 K1 K1 104.79(5) 3_656 1_455 ?
N2 K1 K1 45.43(4) 1_455 1_455 ?
N3 K1 K1 63.34(4) 1_455 1_455 ?
C1 K1 K1 55.67(4) 2_546 1_455 ?
K1 K1 K1 117.601(17) 3_657 1_455 ?
K1 K1 K1 180.00(3) 1_655 1_455 ?
O1 K1 K1 92.46(4) 2_646 3_557 ?
O1 K1 K1 40.30(4) 2_546 3_557 ?
O1 K1 K1 40.03(4) 4_566 3_557 ?
N2 K1 K1 131.14(5) . 3_557 ?
N3 K1 K1 144.76(5) 3_656 3_557 ?
N2 K1 K1 84.76(4) 1_455 3_557 ?
N3 K1 K1 109.04(5) 1_455 3_557 ?
C1 K1 K1 55.30(4) 2_546 3_557 ?
K1 K1 K1 60.087(17) 3_657 3_557 ?
K1 K1 K1 122.486(16) 1_655 3_557 ?
K1 K1 K1 57.514(16) 1_455 3_557 ?
C1 N1 N2 107.11(19) . . ?
N3 N2 N1 111.0(2) . . ?
N3 N2 K1 129.24(17) . . ?
N1 N2 K1 116.53(15) . . ?
N3 N2 K1 80.33(15) . 1_655 ?
N1 N2 K1 124.68(17) . 1_655 ?
K1 N2 K1 86.89(6) . 1_655 ?
N2 N3 N4 106.0(2) . . ?
N2 N3 K1 146.90(17) . 3_656 ?
N4 N3 K1 104.71(14) . 3_656 ?
N2 N3 K1 75.39(14) . 1_655 ?
N4 N3 K1 125.37(16) . 1_655 ?
K1 N3 K1 96.46(6) 3_656 1_655 ?
N3 N4 C1 110.54(19) . . ?
N3 N4 H4 124.7 . . ?
C1 N4 H4 124.7 . . ?
C1 O1 K1 123.81(17) . 2_656 ?
C1 O1 K1 112.83(16) . 2_556 ?
K1 O1 K1 97.69(6) 2_656 2_556 ?
C1 O1 K1 123.63(15) . 4_665 ?
K1 O1 K1 93.88(6) 2_656 4_665 ?
K1 O1 K1 99.67(6) 2_556 4_665 ?
O1 C1 N1 128.0(2) . . ?
O1 C1 N4 126.7(2) . . ?
N1 C1 N4 105.3(2) . . ?
O1 C1 K1 47.44(13) . 2_556 ?
N1 C1 K1 83.68(14) . 2_556 ?
N4 C1 K1 160.08(16) . 2_556 ?

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 -0.1(3) . . . . ?
C1 N1 N2 K1 -161.64(15) . . . . ?
C1 N1 N2 K1 92.6(2) . . . 1_655 ?
O1 K1 N2 N3 82.6(2) 2_646 . . . ?
O1 K1 N2 N3 -151.8(3) 2_546 . . . ?
O1 K1 N2 N3 168.7(2) 4_566 . . . ?
N3 K1 N2 N3 -0.7(2) 3_656 . . . ?
N2 K1 N2 N3 -105.2(2) 1_455 . . . ?
N3 K1 N2 N3 -86.0(2) 1_455 . . . ?
C1 K1 N2 N3 42.9(5) 2_546 . . . ?
K1 K1 N2 N3 126.1(2) 3_657 . . . ?
K1 K1 N2 N3 74.8(2) 1_655 . . . ?
K1 K1 N2 N3 -105.2(2) 1_455 . . . ?
K1 K1 N2 N3 174.56(19) 3_557 . . . ?
O1 K1 N2 N1 -119.76(19) 2_646 . . . ?
O1 K1 N2 N1 5.7(4) 2_546 . . . ?
O1 K1 N2 N1 -33.69(19) 4_566 . . . ?
N3 K1 N2 N1 156.85(19) 3_656 . . . ?
N2 K1 N2 N1 52.4(2) 1_455 . . . ?
N3 K1 N2 N1 71.62(19) 1_455 . . . ?
C1 K1 N2 N1 -159.5(3) 2_546 . . . ?
K1 K1 N2 N1 -76.33(18) 3_657 . . . ?
K1 K1 N2 N1 -127.6(2) 1_655 . . . ?
K1 K1 N2 N1 52.4(2) 1_455 . . . ?
K1 K1 N2 N1 -27.8(2) 3_557 . . . ?
O1 K1 N2 K1 7.81(6) 2_646 . . 1_655 ?
O1 K1 N2 K1 133.3(3) 2_546 . . 1_655 ?
O1 K1 N2 K1 93.88(6) 4_566 . . 1_655 ?
N3 K1 N2 K1 -75.58(6) 3_656 . . 1_655 ?
N2 K1 N2 K1 180.0 1_455 . . 1_655 ?
N3 K1 N2 K1 -160.80(7) 1_455 . . 1_655 ?
C1 K1 N2 K1 -31.9(4) 2_546 . . 1_655 ?
K1 K1 N2 K1 51.24(5) 3_657 . . 1_655 ?
K1 K1 N2 K1 180.0 1_455 . . 1_655 ?
K1 K1 N2 K1 99.73(6) 3_557 . . 1_655 ?
N1 N2 N3 N4 0.4(3) . . . . ?
K1 N2 N3 N4 158.94(17) . . . . ?
K1 N2 N3 N4 -123.19(18) 1_655 . . . ?
N1 N2 N3 K1 -157.2(2) . . . 3_656 ?
K1 N2 N3 K1 1.4(4) . . . 3_656 ?
K1 N2 N3 K1 79.2(3) 1_655 . . 3_656 ?
N1 N2 N3 K1 123.6(2) . . . 1_655 ?
K1 N2 N3 K1 -77.86(17) . . . 1_655 ?
N2 N3 N4 C1 -0.5(3) . . . . ?
K1 N3 N4 C1 167.04(15) 3_656 . . . ?
K1 N3 N4 C1 -83.8(2) 1_655 . . . ?
K1 O1 C1 N1 92.2(3) 2_656 . . . ?
K1 O1 C1 N1 -25.0(3) 2_556 . . . ?
K1 O1 C1 N1 -144.9(2) 4_665 . . . ?
K1 O1 C1 N4 -87.7(3) 2_656 . . . ?
K1 O1 C1 N4 155.2(2) 2_556 . . . ?
K1 O1 C1 N4 35.2(3) 4_665 . . . ?
K1 O1 C1 K1 117.17(18) 2_656 . . 2_556 ?
K1 O1 C1 K1 -119.9(2) 4_665 . . 2_556 ?
N2 N1 C1 O1 179.9(3) . . . . ?
N2 N1 C1 N4 -0.3(3) . . . . ?
N2 N1 C1 K1 161.64(19) . . . 2_556 ?
N3 N4 C1 O1 -179.7(3) . . . . ?
N3 N4 C1 N1 0.5(3) . . . . ?
N3 N4 C1 K1 -114.4(5) . . . 2_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_140703e
_database_code_depnum_ccdc_archive 'CCDC 1018908'
_audit_update_record             
;
2017-05-25 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Cesium 5-oxotetrazolate'
_chemical_formula_moiety         '0.13(C8 H8 Cs8 N32 O8)'
_chemical_formula_sum            'C H Cs N4 O'
_chemical_formula_weight         217.97
_chemical_melting_point          ?
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'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z'
'x-1/2, -y-1/2, z'

_cell_length_a                   6.9541(5)
_cell_length_b                   13.8119(12)
_cell_length_c                   4.9030(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     470.93(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1582
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.316
_cell_measurement_theta_min      2.95
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.162
_exptl_absorpt_coefficient_mu    7.732
_exptl_absorpt_correction_T_max  0.5767
_exptl_absorpt_correction_T_min  0.1621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    3.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2125
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         2.950
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                423
_reflns_number_total             471
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.266
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         471
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+11.0148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1213
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: N1(0.5) H1(0.5) N2(0.5) N3(0.5) N4(0.5)
4.a Riding coordinates:
 N1(H1)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cs1 Cs 0.12811(16) 0.15004(7) 0.0000 0.0323(4) Uani 1 2 d S TU P . .
N1 N 0.623(4) 0.1156(17) 0.766(5) 0.031(4) Uani 0.5 1 d . U . . .
H1 H 0.5760 0.1280 0.9225 0.037 Uiso 0.5 1 d R . . . .
N2 N 0.755(3) 0.0497(17) 0.691(5) 0.032(4) Uani 0.5 1 d . U . . .
N3 N 0.763(3) 0.0388(15) 0.434(4) 0.030(4) Uani 0.5 1 d . U . . .
N4 N 0.631(4) 0.1024(18) 0.327(5) 0.029(4) Uani 0.5 1 d . U . . .
O1 O 0.4186(16) 0.2158(9) 0.5000 0.033(3) Uani 1 2 d S TU P . .
C1 C 0.543(2) 0.1527(12) 0.5000 0.030(3) Uani 1 2 d S TU P . .


_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.
;
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
Cs1 N1 3.43(2) 3_456 ?
Cs1 N1 3.43(2) 8_564 ?
Cs1 N2 3.31(2) 6_456 ?
Cs1 N2 3.25(2) 5_656 ?
Cs1 N2 3.31(2) 1_454 ?
Cs1 N2 3.25(2) 2_654 ?
Cs1 N3 3.452(19) 2_655 ?
Cs1 N3 3.452(19) 5_655 ?
Cs1 O1 3.304(8) . ?
Cs1 O1 3.401(8) 3_456 ?
Cs1 O1 3.304(8) 1_554 ?
Cs1 O1 3.401(8) 3_455 ?
N1 Cs1 3.43(2) 3_556 ?
N1 Cs1 3.73(3) 1_656 ?
N1 Cs1 3.66(3) 1_556 ?
N1 N2 1.34(3) . ?
N1 N3 1.74(3) 6_556 ?
N1 N4 0.50(3) 6_556 ?
N1 C1 1.51(3) . ?
N2 Cs1 3.31(2) 1_656 ?
N2 Cs1 3.25(2) 5_656 ?
N2 N2 1.87(5) 6_556 ?
N2 N3 1.27(3) . ?
N2 N3 0.64(2) 6_556 ?
N2 N4 1.13(3) 6_556 ?
N3 Cs1 3.452(19) 5_655 ?
N3 Cs1 3.65(2) 1_655 ?
N3 N1 1.74(3) 6_556 ?
N3 N2 0.64(2) 6_556 ?
N3 N3 0.64(4) 6_556 ?
N3 N4 1.37(3) . ?
N3 N4 1.73(3) 6_556 ?
N4 Cs1 3.78(2) 3 ?
N4 N1 0.50(3) 6_556 ?
N4 N2 1.13(3) 6_556 ?
N4 N3 1.73(3) 6_556 ?
N4 N4 1.69(5) 6_556 ?
N4 C1 1.25(3) . ?
O1 Cs1 3.401(8) 3_556 ?
O1 Cs1 3.304(8) 1_556 ?
O1 Cs1 3.401(8) 3 ?
O1 C1 1.229(19) . ?
C1 Cs1 3.713(12) 3 ?
C1 Cs1 3.787(13) 1_556 ?
C1 Cs1 3.713(12) 3_556 ?
C1 N1 1.51(3) 6_556 ?
C1 N4 1.25(3) 6_556 ?

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 Cs1 N1 39.0(9) 3_456 8_564 ?
N1 Cs1 N3 120.6(6) 8_564 5_655 ?
N1 Cs1 N3 120.6(6) 3_456 2_655 ?
N1 Cs1 N3 157.0(6) 8_564 2_655 ?
N1 Cs1 N3 157.0(6) 3_456 5_655 ?
N2 Cs1 N1 103.5(6) 6_456 3_456 ?
N2 Cs1 N1 130.3(6) 2_654 8_564 ?
N2 Cs1 N1 163.4(6) 2_654 3_456 ?
N2 Cs1 N1 122.6(6) 6_456 8_564 ?
N2 Cs1 N1 130.3(6) 5_656 3_456 ?
N2 Cs1 N1 163.4(6) 5_656 8_564 ?
N2 Cs1 N1 122.6(6) 1_454 3_456 ?
N2 Cs1 N1 103.5(6) 1_454 8_564 ?
N2 Cs1 N2 68.1(7) 2_654 1_454 ?
N2 Cs1 N2 93.1(5) 2_654 6_456 ?
N2 Cs1 N2 93.1(5) 5_656 1_454 ?
N2 Cs1 N2 54.5(8) 1_454 6_456 ?
N2 Cs1 N2 55.5(8) 2_654 5_656 ?
N2 Cs1 N2 68.1(7) 5_656 6_456 ?
N2 Cs1 N3 10.3(4) 2_654 5_655 ?
N2 Cs1 N3 98.0(6) 6_456 5_655 ?
N2 Cs1 N3 65.9(6) 2_654 2_655 ?
N2 Cs1 N3 64.7(5) 6_456 2_655 ?
N2 Cs1 N3 10.3(4) 5_656 2_655 ?
N2 Cs1 N3 65.9(6) 5_656 5_655 ?
N2 Cs1 N3 64.7(5) 1_454 5_655 ?
N2 Cs1 N3 98.0(6) 1_454 2_655 ?
N2 Cs1 O1 74.6(4) 2_654 1_554 ?
N2 Cs1 O1 154.9(4) 5_656 3_455 ?
N2 Cs1 O1 64.0(4) 6_456 3_456 ?
N2 Cs1 O1 103.5(4) 2_654 3_455 ?
N2 Cs1 O1 103.5(4) 5_656 3_456 ?
N2 Cs1 O1 102.8(4) 1_454 3_456 ?
N2 Cs1 O1 74.6(4) 5_656 . ?
N2 Cs1 O1 115.2(5) 5_656 1_554 ?
N2 Cs1 O1 154.9(4) 2_654 3_456 ?
N2 Cs1 O1 102.8(4) 6_456 3_455 ?
N2 Cs1 O1 115.2(5) 2_654 . ?
N2 Cs1 O1 64.0(4) 1_454 3_455 ?
N3 Cs1 N3 76.2(6) 5_655 2_655 ?
O1 Cs1 N1 40.7(5) 3_456 3_456 ?
O1 Cs1 N1 60.0(5) . 3_456 ?
O1 Cs1 N1 89.7(5) . 8_564 ?
O1 Cs1 N1 60.0(5) 1_554 8_564 ?
O1 Cs1 N1 73.9(5) 3_455 3_456 ?
O1 Cs1 N1 89.7(5) 1_554 3_456 ?
O1 Cs1 N1 73.9(5) 3_456 8_564 ?
O1 Cs1 N1 40.7(5) 3_455 8_564 ?
O1 Cs1 N2 104.8(4) . 6_456 ?
O1 Cs1 N2 104.8(4) 1_554 1_454 ?
O1 Cs1 N2 159.1(4) 1_554 6_456 ?
O1 Cs1 N2 159.1(4) . 1_454 ?
O1 Cs1 N3 161.9(4) 3_455 2_655 ?
O1 Cs1 N3 122.1(4) . 5_655 ?
O1 Cs1 N3 67.4(4) . 2_655 ?
O1 Cs1 N3 93.5(3) 3_455 5_655 ?
O1 Cs1 N3 67.4(4) 1_554 5_655 ?
O1 Cs1 N3 93.5(3) 3_456 2_655 ?
O1 Cs1 N3 122.1(4) 1_554 2_655 ?
O1 Cs1 N3 161.9(4) 3_456 5_655 ?
O1 Cs1 O1 65.00(9) . 3_456 ?
O1 Cs1 O1 65.00(9) 1_554 3_455 ?
O1 Cs1 O1 130.32(9) . 3_455 ?
O1 Cs1 O1 92.2(3) 3_456 3_455 ?
O1 Cs1 O1 130.32(9) 1_554 3_456 ?
O1 Cs1 O1 95.8(3) 1_554 . ?
Cs1 N1 Cs1 140.7(7) 1_556 1_656 ?
Cs1 N1 Cs1 76.5(5) 3_556 1_656 ?
Cs1 N1 Cs1 77.4(5) 3_556 1_556 ?
N2 N1 Cs1 61.8(13) . 1_656 ?
N2 N1 Cs1 136.3(17) . 3_556 ?
N2 N1 Cs1 144.7(17) . 1_556 ?
N2 N1 N3 18.6(12) . 6_556 ?
N2 N1 C1 104.1(19) . . ?
N3 N1 Cs1 141.3(14) 6_556 1_556 ?
N3 N1 Cs1 74.1(11) 6_556 1_656 ?
N3 N1 Cs1 139.2(14) 6_556 3_556 ?
N4 N1 Cs1 116(6) 6_556 1_556 ?
N4 N1 Cs1 131(5) 6_556 3_556 ?
N4 N1 Cs1 103(6) 6_556 1_656 ?
N4 N1 N2 55(5) 6_556 . ?
N4 N1 N3 36(5) 6_556 6_556 ?
N4 N1 C1 51(5) 6_556 . ?
C1 N1 Cs1 124.7(15) . 1_656 ?
C1 N1 Cs1 88.4(11) . 3_556 ?
C1 N1 Cs1 83.2(12) . 1_556 ?
C1 N1 N3 85.6(15) . 6_556 ?
Cs1 N2 Cs1 86.9(5) 5_656 1_656 ?
N1 N2 Cs1 97.3(15) . 1_656 ?
N1 N2 Cs1 128.1(17) . 5_656 ?
N1 N2 N2 105.9(15) . 6_556 ?
N2 N2 Cs1 117.2(4) 6_556 1_656 ?
N2 N2 Cs1 117.8(4) 6_556 5_656 ?
N3 N2 Cs1 103(3) 6_556 5_656 ?
N3 N2 Cs1 110.5(18) . 5_656 ?
N3 N2 Cs1 118.1(19) . 1_656 ?
N3 N2 Cs1 118(4) 6_556 1_656 ?
N3 N2 N1 119(4) 6_556 . ?
N3 N2 N1 112(2) . . ?
N3 N2 N2 15(3) 6_556 6_556 ?
N3 N2 N2 7.3(17) . 6_556 ?
N3 N2 N3 7.4(17) 6_556 . ?
N3 N2 N4 98(4) 6_556 6_556 ?
N4 N2 Cs1 141(2) 6_556 5_656 ?
N4 N2 Cs1 111.4(18) 6_556 1_656 ?
N4 N2 N1 21.0(16) 6_556 . ?
N4 N2 N2 85.5(16) 6_556 6_556 ?
N4 N2 N3 92(2) 6_556 . ?
Cs1 N3 Cs1 78.8(4) 5_655 1_655 ?
N1 N3 Cs1 78.6(11) 6_556 1_655 ?
N1 N3 Cs1 103.5(11) 6_556 5_655 ?
N2 N3 Cs1 135.4(19) . 5_655 ?
N2 N3 Cs1 53(3) 6_556 1_655 ?
N2 N3 Cs1 123.9(19) . 1_655 ?
N2 N3 Cs1 67(3) 6_556 5_655 ?
N2 N3 N1 118(2) . 6_556 ?
N2 N3 N1 42(3) 6_556 6_556 ?
N2 N3 N2 158(5) 6_556 . ?
N2 N3 N3 165(3) 6_556 6_556 ?
N2 N3 N4 106(2) . . ?
N2 N3 N4 55(3) 6_556 . ?
N2 N3 N4 119(4) 6_556 6_556 ?
N2 N3 N4 41.0(16) . 6_556 ?
N3 N3 Cs1 128.1(3) 6_556 5_655 ?
N3 N3 Cs1 125.6(3) 6_556 1_655 ?
N3 N3 N1 124.4(11) 6_556 6_556 ?
N3 N3 N2 7.3(17) 6_556 . ?
N3 N3 N4 47.4(10) 6_556 6_556 ?
N3 N3 N4 112.5(13) 6_556 . ?
N4 N3 Cs1 156.8(13) 6_556 5_655 ?
N4 N3 Cs1 113.2(14) . 5_655 ?
N4 N3 Cs1 123.4(12) 6_556 1_655 ?
N4 N3 Cs1 88.4(14) . 1_655 ?
N4 N3 N1 77.1(12) 6_556 6_556 ?
N4 N3 N1 12.3(15) . 6_556 ?
N4 N3 N4 65.1(19) . 6_556 ?
N1 N4 Cs1 43(5) 6_556 3 ?
N1 N4 N2 104(6) 6_556 6_556 ?
N1 N4 N3 151(6) 6_556 6_556 ?
N1 N4 N3 132(6) 6_556 . ?
N1 N4 N4 157(5) 6_556 6_556 ?
N1 N4 C1 111(6) 6_556 . ?
N2 N4 Cs1 123.5(19) 6_556 3 ?
N2 N4 N3 27.2(13) 6_556 . ?
N2 N4 N3 47.3(17) 6_556 6_556 ?
N2 N4 N4 94.5(16) 6_556 6_556 ?
N2 N4 C1 141(2) 6_556 . ?
N3 N4 Cs1 138.7(13) 6_556 3 ?
N3 N4 Cs1 138.1(16) . 3 ?
N3 N4 N3 20.1(12) . 6_556 ?
N3 N4 N4 67.5(13) . 6_556 ?
N4 N4 Cs1 115.1(4) 6_556 3 ?
N4 N4 N3 47.4(10) 6_556 6_556 ?
C1 N4 Cs1 77.5(12) . 3 ?
C1 N4 N3 114.8(19) . . ?
C1 N4 N3 94.7(16) . 6_556 ?
C1 N4 N4 47.5(12) . 6_556 ?
Cs1 O1 Cs1 95.8(3) 1_556 . ?
Cs1 O1 Cs1 161.2(4) . 3_556 ?
Cs1 O1 Cs1 161.2(4) 1_556 3 ?
Cs1 O1 Cs1 82.92(6) . 3 ?
Cs1 O1 Cs1 82.92(6) 1_556 3_556 ?
Cs1 O1 Cs1 92.2(3) 3_556 3 ?
C1 O1 Cs1 94.8(7) . 3 ?
C1 O1 Cs1 103.7(7) . . ?
C1 O1 Cs1 103.7(6) . 1_556 ?
C1 O1 Cs1 94.8(7) . 3_556 ?
Cs1 C1 Cs1 123.8(4) 3 1_556 ?
Cs1 C1 Cs1 80.7(3) 1_556 . ?
Cs1 C1 Cs1 72.59(17) 3 . ?
Cs1 C1 Cs1 82.7(3) 3_556 3 ?
Cs1 C1 Cs1 72.59(17) 3_556 1_556 ?
Cs1 C1 Cs1 123.8(4) 3_556 . ?
N1 C1 Cs1 67.6(10) 6_556 3 ?
N1 C1 Cs1 73.5(11) . 1_556 ?
N1 C1 Cs1 146.9(13) 6_556 1_556 ?
N1 C1 Cs1 146.9(13) . . ?
N1 C1 Cs1 139.7(13) 6_556 3_556 ?
N1 C1 Cs1 139.7(13) . 3 ?
N1 C1 Cs1 67.6(10) . 3_556 ?
N1 C1 Cs1 73.5(11) 6_556 . ?
N1 C1 N1 120(2) 6_556 . ?
N4 C1 Cs1 85.9(12) 6_556 1_556 ?
N4 C1 Cs1 143.4(15) 6_556 . ?
N4 C1 Cs1 85.9(12) . . ?
N4 C1 Cs1 83.3(12) . 3 ?
N4 C1 Cs1 143.4(15) . 1_556 ?
N4 C1 Cs1 140.8(15) 6_556 3 ?
N4 C1 Cs1 83.3(12) 6_556 3_556 ?
N4 C1 Cs1 140.8(15) . 3_556 ?
N4 C1 N1 102.6(17) . . ?
N4 C1 N1 102.6(17) 6_556 6_556 ?
N4 C1 N1 17.8(14) . 6_556 ?
N4 C1 N1 17.8(14) 6_556 . ?
N4 C1 N4 85(2) 6_556 . ?
O1 C1 Cs1 65.9(6) . 3_556 ?
O1 C1 Cs1 58.0(6) . . ?
O1 C1 Cs1 65.9(6) . 3 ?
O1 C1 Cs1 58.0(6) . 1_556 ?
O1 C1 N1 120.0(11) . 6_556 ?
O1 C1 N1 120.0(11) . . ?
O1 C1 N4 137.4(12) . 6_556 ?
O1 C1 N4 137.4(12) . . ?

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 N1 N2 Cs1 -48(4) 1_556 . . 5_656 ?
Cs1 N1 N2 Cs1 -140(2) 1_556 . . 1_656 ?
Cs1 N1 N2 Cs1 111(2) 3_556 . . 5_656 ?
Cs1 N1 N2 Cs1 19(2) 3_556 . . 1_656 ?
Cs1 N1 N2 Cs1 91.8(16) 1_656 . . 5_656 ?
Cs1 N1 N2 N2 99(3) 1_556 . . 6_556 ?
Cs1 N1 N2 N2 -121.1(8) 1_656 . . 6_556 ?
Cs1 N1 N2 N2 -102(2) 3_556 . . 6_556 ?
Cs1 N1 N2 N3 92(5) 1_556 . . 6_556 ?
Cs1 N1 N2 N3 -128(5) 1_656 . . 6_556 ?
Cs1 N1 N2 N3 96(3) 1_556 . . . ?
Cs1 N1 N2 N3 -124(3) 1_656 . . . ?
Cs1 N1 N2 N3 -109(4) 3_556 . . 6_556 ?
Cs1 N1 N2 N3 -105(3) 3_556 . . . ?
Cs1 N1 N2 N4 -134(6) 1_656 . . 6_556 ?
Cs1 N1 N2 N4 -115(7) 3_556 . . 6_556 ?
Cs1 N1 N2 N4 86(6) 1_556 . . 6_556 ?
Cs1 N1 C1 Cs1 -72.4(11) 1_656 . . 3_556 ?
Cs1 N1 C1 Cs1 169.7(9) 1_656 . . . ?
Cs1 N1 C1 Cs1 -40.4(19) 1_556 . . . ?
Cs1 N1 C1 Cs1 -150.0(13) 1_656 . . 1_556 ?
Cs1 N1 C1 Cs1 -117.9(17) 3_556 . . . ?
Cs1 N1 C1 Cs1 123.2(14) 1_556 . . 3 ?
Cs1 N1 C1 Cs1 77.5(4) 1_556 . . 3_556 ?
Cs1 N1 C1 Cs1 45.6(17) 3_556 . . 3 ?
Cs1 N1 C1 Cs1 -77.5(4) 3_556 . . 1_556 ?
Cs1 N1 C1 Cs1 -27(2) 1_656 . . 3 ?
Cs1 N1 C1 N1 63(3) 1_656 . . 6_556 ?
Cs1 N1 C1 N1 -146.9(19) 1_556 . . 6_556 ?
Cs1 N1 C1 N1 135.6(18) 3_556 . . 6_556 ?
Cs1 N1 C1 N4 150(7) 3_556 . . 6_556 ?
Cs1 N1 C1 N4 78(6) 1_656 . . 6_556 ?
Cs1 N1 C1 N4 -142.4(16) 1_556 . . . ?
Cs1 N1 C1 N4 -132(7) 1_556 . . 6_556 ?
Cs1 N1 C1 N4 67.7(19) 1_656 . . . ?
Cs1 N1 C1 N4 140.1(16) 3_556 . . . ?
Cs1 N1 C1 O1 -114.0(17) 1_656 . . . ?
Cs1 N1 C1 O1 -41.6(17) 3_556 . . . ?
Cs1 N1 C1 O1 36.0(16) 1_556 . . . ?
Cs1 N2 N3 Cs1 -109.5(15) 5_656 . . 1_655 ?
Cs1 N2 N3 Cs1 -12(3) 1_656 . . 1_655 ?
Cs1 N2 N3 Cs1 1(3) 5_656 . . 5_655 ?
Cs1 N2 N3 Cs1 98(2) 1_656 . . 5_655 ?
Cs1 N2 N3 N1 155.7(14) 5_656 . . 6_556 ?
Cs1 N2 N3 N1 -107(2) 1_656 . . 6_556 ?
Cs1 N2 N3 N2 -85(13) 1_656 . . 6_556 ?
Cs1 N2 N3 N2 177(12) 5_656 . . 6_556 ?
Cs1 N2 N3 N3 95(13) 1_656 . . 6_556 ?
Cs1 N2 N3 N3 -3(12) 5_656 . . 6_556 ?
Cs1 N2 N3 N4 151.5(14) 5_656 . . . ?
Cs1 N2 N3 N4 -110.8(19) 1_656 . . . ?
Cs1 N2 N3 N4 -115(2) 1_656 . . 6_556 ?
Cs1 N2 N3 N4 147(3) 5_656 . . 6_556 ?
Cs1 N3 N4 Cs1 -25(2) 1_655 . . 3 ?
Cs1 N3 N4 Cs1 -102.2(19) 5_655 . . 3 ?
Cs1 N3 N4 N1 -40(8) 5_655 . . 6_556 ?
Cs1 N3 N4 N1 37(8) 1_655 . . 6_556 ?
Cs1 N3 N4 N2 -33(3) 5_655 . . 6_556 ?
Cs1 N3 N4 N2 44(4) 1_655 . . 6_556 ?
Cs1 N3 N4 N3 -128.3(7) 1_655 . . 6_556 ?
Cs1 N3 N4 N3 154.7(14) 5_655 . . 6_556 ?
Cs1 N3 N4 N4 -128.3(7) 1_655 . . 6_556 ?
Cs1 N3 N4 N4 154.7(14) 5_655 . . 6_556 ?
Cs1 N3 N4 C1 158.7(17) 5_655 . . . ?
Cs1 N3 N4 C1 -124(2) 1_655 . . . ?
Cs1 N4 C1 Cs1 72.93(19) 3 . . . ?
Cs1 N4 C1 Cs1 -69.6(16) 3 . . 3_556 ?
Cs1 N4 C1 Cs1 141.2(18) 3 . . 1_556 ?
Cs1 N4 C1 N1 28(6) 3 . . 6_556 ?
Cs1 N4 C1 N1 -139.5(14) 3 . . . ?
Cs1 N4 C1 N4 -142.5(13) 3 . . 6_556 ?
Cs1 N4 C1 O1 43(2) 3 . . . ?
Cs1 O1 C1 Cs1 -176.5(5) 1_556 . . 3 ?
Cs1 O1 C1 Cs1 83.88(13) 3_556 . . 1_556 ?
Cs1 O1 C1 Cs1 -92.7(4) 3_556 . . 3 ?
Cs1 O1 C1 Cs1 83.88(13) . . . 3 ?
Cs1 O1 C1 Cs1 92.7(4) 3 . . 3_556 ?
Cs1 O1 C1 Cs1 99.6(6) 1_556 . . . ?
Cs1 O1 C1 Cs1 -83.88(13) 3 . . . ?
Cs1 O1 C1 Cs1 -176.5(5) 3_556 . . . ?
Cs1 O1 C1 Cs1 -99.6(6) . . . 1_556 ?
Cs1 O1 C1 Cs1 176.5(5) . . . 3_556 ?
Cs1 O1 C1 Cs1 176.5(5) 3 . . 1_556 ?
Cs1 O1 C1 Cs1 -83.88(13) 1_556 . . 3_556 ?
Cs1 O1 C1 N1 141.2(16) 1_556 . . 6_556 ?
Cs1 O1 C1 N1 -134.9(16) 3_556 . . 6_556 ?
Cs1 O1 C1 N1 134.9(16) 3 . . . ?
Cs1 O1 C1 N1 -41.6(19) 1_556 . . . ?
Cs1 O1 C1 N1 -42.2(18) 3 . . 6_556 ?
Cs1 O1 C1 N1 41.6(19) . . . 6_556 ?
Cs1 O1 C1 N1 -141.2(16) . . . . ?
Cs1 O1 C1 N1 42.2(18) 3_556 . . . ?
Cs1 O1 C1 N4 -48(3) 3 . . . ?
Cs1 O1 C1 N4 -136(3) . . . 6_556 ?
Cs1 O1 C1 N4 136(3) 1_556 . . . ?
Cs1 O1 C1 N4 -36(3) 1_556 . . 6_556 ?
Cs1 O1 C1 N4 -140(3) 3_556 . . . ?
Cs1 O1 C1 N4 48(3) 3_556 . . 6_556 ?
Cs1 O1 C1 N4 36(3) . . . . ?
Cs1 O1 C1 N4 140(3) 3 . . 6_556 ?
N1 N2 N3 Cs1 100(2) . . . 1_655 ?
N1 N2 N3 Cs1 -149.4(18) . . . 5_655 ?
N1 N2 N3 N1 6(3) . . . 6_556 ?
N1 N2 N3 N2 27(15) . . . 6_556 ?
N1 N2 N3 N3 -153(15) . . . 6_556 ?
N1 N2 N3 N4 -3(2) . . . 6_556 ?
N1 N2 N3 N4 1(3) . . . . ?
N1 N3 N4 Cs1 -62(8) 6_556 . . 3 ?
N1 N3 N4 N2 7(8) 6_556 . . 6_556 ?
N1 N3 N4 N3 -165(8) 6_556 . . 6_556 ?
N1 N3 N4 N4 -165(8) 6_556 . . 6_556 ?
N1 N3 N4 C1 -161(10) 6_556 . . . ?
N1 N4 C1 Cs1 114(6) 6_556 . . 1_556 ?
N1 N4 C1 Cs1 -28(6) 6_556 . . 3 ?
N1 N4 C1 Cs1 45(6) 6_556 . . . ?
N1 N4 C1 Cs1 -97(6) 6_556 . . 3_556 ?
N1 N4 C1 N1 -167(7) 6_556 . . . ?
N1 N4 C1 N4 -170(5) 6_556 . . 6_556 ?
N1 N4 C1 O1 15(8) 6_556 . . . ?
N2 N1 C1 Cs1 -92(2) . . . 3 ?
N2 N1 C1 Cs1 104(2) . . . . ?
N2 N1 C1 Cs1 144.9(18) . . . 1_556 ?
N2 N1 C1 Cs1 -137.6(19) . . . 3_556 ?
N2 N1 C1 N1 -2(3) . . . 6_556 ?
N2 N1 C1 N4 13(5) . . . 6_556 ?
N2 N1 C1 N4 2.5(19) . . . . ?
N2 N1 C1 O1 -179.2(17) . . . . ?
N2 N2 N3 Cs1 74(13) 6_556 . . 1_655 ?
N2 N2 N3 Cs1 -176(15) 6_556 . . 5_655 ?
N2 N2 N3 N1 -21(12) 6_556 . . 6_556 ?
N2 N2 N3 N3 180.0(2) 6_556 . . 6_556 ?
N2 N2 N3 N4 -26(12) 6_556 . . . ?
N2 N2 N3 N4 -30(14) 6_556 . . 6_556 ?
N2 N3 N4 Cs1 100(3) . . . 3 ?
N2 N3 N4 Cs1 -69(4) 6_556 . . 3 ?
N2 N3 N4 N1 -7(8) 6_556 . . 6_556 ?
N2 N3 N4 N1 162(8) . . . 6_556 ?
N2 N3 N4 N2 169(6) . . . 6_556 ?
N2 N3 N4 N3 -172(4) 6_556 . . 6_556 ?
N2 N3 N4 N3 -3.4(17) . . . 6_556 ?
N2 N3 N4 N4 -172(4) 6_556 . . 6_556 ?
N2 N3 N4 N4 -3.4(17) . . . 6_556 ?
N2 N3 N4 C1 1(3) . . . . ?
N2 N3 N4 C1 -168(4) 6_556 . . . ?
N2 N4 C1 Cs1 -158(4) 6_556 . . . ?
N2 N4 C1 Cs1 -90(5) 6_556 . . 1_556 ?
N2 N4 C1 Cs1 129(4) 6_556 . . 3 ?
N2 N4 C1 Cs1 59(5) 6_556 . . 3_556 ?
N2 N4 C1 N1 156(10) 6_556 . . 6_556 ?
N2 N4 C1 N1 -11(4) 6_556 . . . ?
N2 N4 C1 N4 -14(5) 6_556 . . 6_556 ?
N2 N4 C1 O1 172(3) 6_556 . . . ?
N3 N1 N2 Cs1 -140(5) 6_556 . . 5_656 ?
N3 N1 N2 Cs1 128(5) 6_556 . . 1_656 ?
N3 N1 N2 N2 7(4) 6_556 . . 6_556 ?
N3 N1 N2 N3 4(2) 6_556 . . . ?
N3 N1 N2 N4 -6(7) 6_556 . . 6_556 ?
N3 N1 C1 Cs1 -139.6(14) 6_556 . . 3_556 ?
N3 N1 C1 Cs1 142.9(12) 6_556 . . 1_556 ?
N3 N1 C1 Cs1 103(2) 6_556 . . . ?
N3 N1 C1 Cs1 -93.9(17) 6_556 . . 3 ?
N3 N1 C1 N1 -4(3) 6_556 . . 6_556 ?
N3 N1 C1 N4 0.5(15) 6_556 . . . ?
N3 N1 C1 N4 11(6) 6_556 . . 6_556 ?
N3 N1 C1 O1 178.9(16) 6_556 . . . ?
N3 N2 N3 Cs1 4(15) 6_556 . . 5_655 ?
N3 N2 N3 Cs1 -106(13) 6_556 . . 1_655 ?
N3 N2 N3 N1 159(12) 6_556 . . 6_556 ?
N3 N2 N3 N2 -180.0(2) 6_556 . . 6_556 ?
N3 N2 N3 N4 155(12) 6_556 . . . ?
N3 N2 N3 N4 150(14) 6_556 . . 6_556 ?
N3 N3 N4 Cs1 103.1(18) 6_556 . . 3 ?
N3 N3 N4 N1 165(8) 6_556 . . 6_556 ?
N3 N3 N4 N2 172(4) 6_556 . . 6_556 ?
N3 N3 N4 N4 -0.002(9) 6_556 . . 6_556 ?
N3 N3 N4 C1 4(2) 6_556 . . . ?
N3 N4 C1 Cs1 138.9(12) 6_556 . . 3 ?
N3 N4 C1 Cs1 69(2) 6_556 . . 3_556 ?
N3 N4 C1 Cs1 -81(3) . . . 1_556 ?
N3 N4 C1 Cs1 -80(2) 6_556 . . 1_556 ?
N3 N4 C1 Cs1 68(3) . . . 3_556 ?
N3 N4 C1 Cs1 138(2) . . . 3 ?
N3 N4 C1 Cs1 -150(2) . . . . ?
N3 N4 C1 Cs1 -148.1(12) 6_556 . . . ?
N3 N4 C1 N1 165(8) . . . 6_556 ?
N3 N4 C1 N1 -0.5(15) 6_556 . . . ?
N3 N4 C1 N1 167(7) 6_556 . . 6_556 ?
N3 N4 C1 N1 -2(2) . . . . ?
N3 N4 C1 N4 -5(3) . . . 6_556 ?
N3 N4 C1 N4 -4(2) 6_556 . . 6_556 ?
N3 N4 C1 O1 -180(2) . . . . ?
N3 N4 C1 O1 -178(2) 6_556 . . . ?
N4 N1 N2 Cs1 -134(6) 6_556 . . 5_656 ?
N4 N1 N2 Cs1 134(6) 6_556 . . 1_656 ?
N4 N1 N2 N2 13(6) 6_556 . . 6_556 ?
N4 N1 N2 N3 6(7) 6_556 . . 6_556 ?
N4 N1 N2 N3 10(6) 6_556 . . . ?
N4 N1 C1 Cs1 -104(6) 6_556 . . 3 ?
N4 N1 C1 Cs1 132(7) 6_556 . . 1_556 ?
N4 N1 C1 Cs1 92(7) 6_556 . . . ?
N4 N1 C1 Cs1 -150(7) 6_556 . . 3_556 ?
N4 N1 C1 N1 -15(8) 6_556 . . 6_556 ?
N4 N1 C1 N4 -10(5) 6_556 . . . ?
N4 N1 C1 O1 168(6) 6_556 . . . ?
N4 N2 N3 Cs1 104(2) 6_556 . . 1_655 ?
N4 N2 N3 Cs1 -146(2) 6_556 . . 5_655 ?
N4 N2 N3 N1 9(3) 6_556 . . 6_556 ?
N4 N2 N3 N2 30(14) 6_556 . . 6_556 ?
N4 N2 N3 N3 -150(14) 6_556 . . 6_556 ?
N4 N2 N3 N4 5(2) 6_556 . . . ?
N4 N3 N4 Cs1 103.1(18) 6_556 . . 3 ?
N4 N3 N4 N1 165(8) 6_556 . . 6_556 ?
N4 N3 N4 N2 172(4) 6_556 . . 6_556 ?
N4 N3 N4 N3 0.002(15) 6_556 . . 6_556 ?
N4 N3 N4 C1 4(2) 6_556 . . . ?
N4 N4 C1 Cs1 73.0(17) 6_556 . . 3_556 ?
N4 N4 C1 Cs1 142.5(13) 6_556 . . 3 ?
N4 N4 C1 Cs1 -144.5(13) 6_556 . . . ?
N4 N4 C1 Cs1 -76.2(18) 6_556 . . 1_556 ?
N4 N4 C1 N1 3.1(17) 6_556 . . . ?
N4 N4 C1 N1 170(5) 6_556 . . 6_556 ?
N4 N4 C1 O1 -175(4) 6_556 . . . ?
C1 N1 N2 Cs1 -146.1(15) . . . 5_656 ?
C1 N1 N2 Cs1 122.1(15) . . . 1_656 ?
C1 N1 N2 N2 1.1(18) . . . 6_556 ?
C1 N1 N2 N3 -6(5) . . . 6_556 ?
C1 N1 N2 N3 -2(3) . . . . ?
C1 N1 N2 N4 -12(5) . . . 6_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
