# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2361132'
loop_
_audit_author_name
_audit_author_address
'Andrei Churakov'
;Institute of General and Inorganic Chemistry RAS
Russia
;
_audit_update_record             
;
2024-06-06 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'N O3, 0.5(H2 O2), K'
_chemical_formula_sum            'H K N O4'
_chemical_formula_weight         118.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.9591(9)
_cell_length_b                   6.8466(8)
_cell_length_c                   8.0046(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.264(4)
_cell_angle_gamma                90
_cell_volume                     344.91(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3341
_cell_measurement_theta_min      3.237
_cell_measurement_theta_max      30.528

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_F_000             236
_exptl_transmission_factor_min   0.6662
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.392
_shelx_estimated_absorpt_T_min   0.606
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4042
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.237
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             991
_reflns_number_gt                964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0149P)²+0.0856P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.059(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         991
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0149
_refine_ls_wR_factor_ref         0.0369
_refine_ls_wR_factor_gt          0.0366
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_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_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
K1 K 0.72689(3) 0.63306(2) 0.88524(2) 0.01006(8) Uani 1 1 d . . . . .
N1 N 0.14562(11) 0.61678(10) 0.68819(9) 0.00926(14) Uani 1 1 d . . . . .
O11 O 0.17013(10) 0.73339(9) 0.57579(8) 0.01393(13) Uani 1 1 d . . . . .
O12 O 0.29931(9) 0.51345(9) 0.79248(8) 0.01296(13) Uani 1 1 d . . . . .
O13 O -0.03031(10) 0.60508(9) 0.69154(9) 0.01591(14) Uani 1 1 d . . . . .
O1 O 0.47619(10) 0.60174(9) 0.46982(10) 0.01534(14) Uani 1 1 d . . . . .
H1 H 0.373(2) 0.6240(18) 0.500(2) 0.027(3) Uiso 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 O13 2.7444(7) 1_655 ?
K1 O1 2.7941(7) 4_576 ?
K1 O11 2.8121(7) 2_646 ?
K1 O12 2.8454(7) 3_667 ?
K1 O12 2.8618(7) . ?
K1 O13 2.9231(7) 4_676 ?
K1 O12 2.9357(7) 2_656 ?
K1 O11 2.9430(7) 4_676 ?
K1 O1 3.0323(8) . ?
K1 O1 3.0382(8) 3_666 ?
K1 N1 3.3576(8) 4_676 ?
K1 K1 3.8966(5) 3_767 ?
K1 H1 3.016(14) . ?
N1 O13 1.2385(9) . ?
N1 O12 1.2567(9) . ?
N1 O11 1.2676(9) . ?
O1 O1 1.4655(12) 3_666 ?
O1 H1 0.868(15) . ?

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
O13 K1 O1 141.34(2) 1_655 4_576 ?
O13 K1 O11 78.789(19) 1_655 2_646 ?
O1 K1 O11 139.58(2) 4_576 2_646 ?
O13 K1 O12 141.33(2) 1_655 3_667 ?
O1 K1 O12 73.81(2) 4_576 3_667 ?
O11 K1 O12 70.627(18) 2_646 3_667 ?
O13 K1 O12 131.01(2) 1_655 . ?
O1 K1 O12 63.97(2) 4_576 . ?
O11 K1 O12 86.437(19) 2_646 . ?
O12 K1 O12 70.88(2) 3_667 . ?
O13 K1 O13 103.99(2) 1_655 4_676 ?
O1 K1 O13 66.13(2) 4_576 4_676 ?
O11 K1 O13 118.36(2) 2_646 4_676 ?
O12 K1 O13 72.15(2) 3_667 4_676 ?
O12 K1 O13 123.913(19) . 4_676 ?
O13 K1 O12 73.384(19) 1_655 2_656 ?
O1 K1 O12 67.97(2) 4_576 2_656 ?
O11 K1 O12 151.307(18) 2_646 2_656 ?
O12 K1 O12 137.503(17) 3_667 2_656 ?
O12 K1 O12 106.587(15) . 2_656 ?
O13 K1 O12 75.90(2) 4_676 2_656 ?
O13 K1 O11 63.43(2) 1_655 4_676 ?
O1 K1 O11 107.29(2) 4_576 4_676 ?
O11 K1 O11 94.804(18) 2_646 4_676 ?
O12 K1 O11 95.634(19) 3_667 4_676 ?
O12 K1 O11 165.261(18) . 4_676 ?
O13 K1 O11 43.274(17) 4_676 4_676 ?
O12 K1 O11 79.053(18) 2_656 4_676 ?
O13 K1 O1 65.19(2) 1_655 . ?
O1 K1 O1 100.67(2) 4_576 . ?
O11 K1 O1 93.035(18) 2_646 . ?
O12 K1 O1 137.715(19) 3_667 . ?
O12 K1 O1 69.351(18) . . ?
O13 K1 O1 145.010(18) 4_676 . ?
O12 K1 O1 69.126(17) 2_656 . ?
O11 K1 O1 125.137(18) 4_676 . ?
O13 K1 O1 65.63(2) 1_655 3_666 ?
O1 K1 O1 118.767(14) 4_576 3_666 ?
O11 K1 O1 65.396(18) 2_646 3_666 ?
O12 K1 O1 118.51(2) 3_667 3_666 ?
O12 K1 O1 65.723(18) . 3_666 ?
O13 K1 O1 168.741(19) 4_676 3_666 ?
O12 K1 O1 96.214(19) 2_656 3_666 ?
O11 K1 O1 127.983(18) 4_676 3_666 ?
O1 K1 O1 27.94(2) . 3_666 ?
O13 K1 N1 83.67(2) 1_655 4_676 ?
O1 K1 N1 86.14(2) 4_576 4_676 ?
O11 K1 N1 108.345(19) 2_646 4_676 ?
O12 K1 N1 84.070(19) 3_667 4_676 ?
O12 K1 N1 144.997(18) . 4_676 ?
O13 K1 N1 21.335(17) 4_676 4_676 ?
O12 K1 N1 75.682(18) 2_656 4_676 ?
O11 K1 N1 21.969(16) 4_676 4_676 ?
O1 K1 N1 138.062(18) . 4_676 ?
O1 K1 N1 149.244(18) 3_666 4_676 ?
O13 K1 K1 61.432(17) 1_655 3_767 ?
O1 K1 K1 140.710(17) 4_576 3_767 ?
O11 K1 K1 48.819(14) 2_646 3_767 ?
O12 K1 K1 80.489(14) 3_667 3_767 ?
O12 K1 K1 133.281(16) . 3_767 ?
O13 K1 K1 78.049(15) 4_676 3_767 ?
O12 K1 K1 119.317(15) 2_656 3_767 ?
O11 K1 K1 45.985(14) 4_676 3_767 ?
O1 K1 K1 118.223(14) . 3_767 ?
O1 K1 K1 99.460(15) 3_666 3_767 ?
N1 K1 K1 61.751(14) 4_676 3_767 ?
O13 K1 H1 81.6(3) 1_655 . ?
O1 K1 H1 86.5(3) 4_576 . ?
O11 K1 H1 98.7(2) 2_646 . ?
O12 K1 H1 125.3(3) 3_667 . ?
O12 K1 H1 54.7(3) . . ?
O13 K1 H1 142.9(2) 4_676 . ?
O12 K1 H1 70.6(2) 2_656 . ?
O11 K1 H1 139.0(3) 4_676 . ?
O1 K1 H1 16.5(3) . . ?
O1 K1 H1 35.1(3) 3_666 . ?
N1 K1 H1 145.9(3) 4_676 . ?
K1 K1 H1 132.8(3) 3_767 . ?
O13 N1 O12 121.21(7) . . ?
O13 N1 O11 119.33(7) . . ?
O12 N1 O11 119.46(7) . . ?
O13 N1 K1 59.17(4) . 4_475 ?
O12 N1 K1 175.71(5) . 4_475 ?
O11 N1 K1 60.29(4) . 4_475 ?
N1 O11 K1 129.73(5) . 2_656 ?
N1 O11 K1 97.74(5) . 4_475 ?
K1 O11 K1 85.196(18) 2_656 4_475 ?
N1 O12 K1 115.79(5) . 3_667 ?
N1 O12 K1 120.48(5) . . ?
K1 O12 K1 109.12(2) 3_667 . ?
N1 O12 K1 108.56(4) . 2_646 ?
K1 O12 K1 96.420(19) 3_667 2_646 ?
K1 O12 K1 102.842(19) . 2_646 ?
N1 O13 K1 149.35(5) . 1_455 ?
N1 O13 K1 99.50(5) . 4_475 ?
K1 O13 K1 98.99(2) 1_455 4_475 ?
O1 O1 K1 128.39(6) 3_666 4_575 ?
O1 O1 K1 76.25(5) 3_666 . ?
K1 O1 K1 95.35(2) 4_575 . ?
O1 O1 K1 75.81(5) 3_666 3_666 ?
K1 O1 K1 101.91(2) 4_575 3_666 ?
K1 O1 K1 152.06(2) . 3_666 ?
O1 O1 H1 99.9(9) 3_666 . ?
K1 O1 H1 129.3(9) 4_575 . ?
K1 O1 H1 80.7(9) . . ?
K1 O1 H1 104.2(9) 3_666 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O11 0.868(15) 1.907(15) 2.7587(9) 166.6(12) .

_refine_diff_density_max         0.249
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.043



####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2364418'
loop_
_audit_author_name
_audit_author_address
'Alexander Medvedev'
;Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2024-06-21 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H2 O2, 2(N O3), H2 O, 2(Rb)'
_chemical_formula_sum            'H4 N2 O9 Rb2'
_chemical_formula_weight         346.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.1429(11)
_cell_length_b                   12.8212(11)
_cell_length_c                   10.9801(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1709.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2630
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      30.42

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.697
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    11.482
_shelx_estimated_absorpt_T_min   0.161
_shelx_estimated_absorpt_T_max   0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2810
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9574
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.310
_diffrn_reflns_theta_max         28.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1199
_reflns_number_gt                817
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+19.4292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1199
_refine_ls_number_parameters     88
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.078
_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_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 0.66288(4) 0.500000 0.250000 0.01120(14) Uani 1 2 d S T P A .
Rb2 Rb 1.000000 0.33283(4) 0.750000 0.01684(15) Uani 1 2 d S T P . .
O1 O 0.721(3) 0.7124(14) 0.2114(8) 0.022(5) Uani 0.70(9) 1 d . . P A 1
O2 O 0.770(6) 0.7052(18) 0.218(2) 0.015(8) Uani 0.30(9) 1 d . . P A 2
H1 H 0.748(6) 0.733(4) 0.149(5) 0.029(16) Uiso 1 1 d . . . . .
O4 O 0.4890(3) 0.3672(2) 0.4012(3) 0.0216(8) Uani 1 1 d . . . . .
O5 O 0.6334(4) 0.4172(4) 0.500000 0.0183(11) Uani 1 2 d S T P A .
O6 O 0.8629(3) 0.5091(3) 0.4011(3) 0.0258(8) Uani 1 1 d . . . . .
O7 O 0.9197(4) 0.3734(3) 0.500000 0.0169(10) Uani 1 2 d S T P . .
N1 N 0.5381(5) 0.3849(4) 0.500000 0.0136(11) Uani 1 2 d S T P . .
N2 N 0.8817(5) 0.4638(4) 0.500000 0.0127(11) Uani 1 2 d S T P . .
O3 O 0.7659(4) 0.8107(4) 0.000000 0.0136(9) Uani 1 2 d DS T P . .
H31 H 0.833(4) 0.825(6) 0.000000 0.02(2) Uiso 1 2 d DS . P . .
H32 H 0.733(7) 0.869(5) 0.000000 0.04(3) Uiso 1 2 d DS . 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
Rb1 O1 2.846(10) . ?
Rb1 O1 2.846(10) 8_455 ?
Rb1 O6 2.943(3) 8_455 ?
Rb1 O6 2.943(3) . ?
Rb1 O2 2.96(4) 8_455 ?
Rb1 O2 2.96(4) . ?
Rb1 O5 2.9651(18) . ?
Rb1 O5 2.9651(18) 15_564 ?
Rb1 O4 3.010(3) 7_545 ?
Rb1 O4 3.010(3) 2_665 ?
Rb1 O4 3.180(4) 8_455 ?
Rb1 O4 3.180(4) . ?
Rb2 O2 2.85(7) 15_565 ?
Rb2 O2 2.85(7) 9_766 ?
Rb2 O7 2.9592(18) 7_646 ?
Rb2 O7 2.9592(18) . ?
Rb2 O4 3.058(3) 4_556 ?
Rb2 O4 3.058(3) 6_655 ?
Rb2 O6 3.104(3) 15_565 ?
Rb2 O6 3.104(3) 9_766 ?
Rb2 O1 3.13(4) 3_646 ?
Rb2 O1 3.13(4) 5_545 ?
Rb2 O6 3.261(4) 16_755 ?
Rb2 O6 3.261(4) 10_556 ?
O1 O1 1.46(3) 13_665 ?
O1 H1 0.80(6) . ?
O2 O2 1.43(4) 13_665 ?
O2 H1 0.89(7) . ?
O4 N1 1.258(4) . ?
O5 N1 1.229(7) . ?
O6 N2 1.253(4) . ?
O7 N2 1.247(7) . ?
O3 H31 0.84(5) . ?
O3 H32 0.84(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Rb1 O1 151.2(18) . 8_455 ?
O1 Rb1 O6 75.4(7) . 8_455 ?
O1 Rb1 O6 80.8(7) 8_455 8_455 ?
O1 Rb1 O6 80.8(7) . . ?
O1 Rb1 O6 75.4(7) 8_455 . ?
O6 Rb1 O6 68.81(15) 8_455 . ?
O1 Rb1 O2 139(2) . 8_455 ?
O1 Rb1 O2 11.9(4) 8_455 8_455 ?
O6 Rb1 O2 70.5(12) 8_455 8_455 ?
O6 Rb1 O2 66.7(8) . 8_455 ?
O6 Rb1 O2 66.7(8) 8_455 . ?
O6 Rb1 O2 70.5(12) . . ?
O2 Rb1 O2 128(2) 8_455 . ?
O1 Rb1 O5 120.72(19) . . ?
O1 Rb1 O5 63.2(3) 8_455 . ?
O6 Rb1 O5 127.40(12) 8_455 . ?
O6 Rb1 O5 65.92(11) . . ?
O2 Rb1 O5 68.0(8) 8_455 . ?
O2 Rb1 O5 118.7(6) . . ?
O1 Rb1 O5 63.2(3) . 15_564 ?
O1 Rb1 O5 120.72(19) 8_455 15_564 ?
O6 Rb1 O5 65.93(11) 8_455 15_564 ?
O6 Rb1 O5 127.40(12) . 15_564 ?
O5 Rb1 O5 166.12(19) . 15_564 ?
O1 Rb1 O4 127.7(5) . 7_545 ?
O1 Rb1 O4 72.1(7) 8_455 7_545 ?
O6 Rb1 O4 99.92(10) 8_455 7_545 ?
O6 Rb1 O4 147.03(10) . 7_545 ?
O5 Rb1 O4 103.53(11) . 7_545 ?
O5 Rb1 O4 67.53(11) 15_564 7_545 ?
O1 Rb1 O4 72.1(7) . 2_665 ?
O1 Rb1 O4 127.7(5) 8_455 2_665 ?
O6 Rb1 O4 147.03(10) 8_455 2_665 ?
O6 Rb1 O4 99.92(10) . 2_665 ?
O5 Rb1 O4 67.53(11) . 2_665 ?
O5 Rb1 O4 103.53(11) 15_564 2_665 ?
O4 Rb1 O4 104.41(15) 7_545 2_665 ?
O1 Rb1 O4 64.8(8) . 8_455 ?
O1 Rb1 O4 139.1(7) 8_455 8_455 ?
O6 Rb1 O4 105.94(9) 8_455 8_455 ?
O6 Rb1 O4 145.17(9) . 8_455 ?
O5 Rb1 O4 126.51(11) . 8_455 ?
O5 Rb1 O4 40.94(11) 15_564 8_455 ?
O4 Rb1 O4 66.93(10) 7_545 8_455 ?
O4 Rb1 O4 65.06(11) 2_665 8_455 ?
O1 Rb1 O4 139.1(7) . . ?
O1 Rb1 O4 64.8(8) 8_455 . ?
O6 Rb1 O4 145.17(9) 8_455 . ?
O6 Rb1 O4 105.94(9) . . ?
O2 Rb1 O4 75.8(12) 8_455 . ?
O2 Rb1 O4 146.2(5) . . ?
O5 Rb1 O4 40.94(11) . . ?
O5 Rb1 O4 126.51(11) 15_564 . ?
O4 Rb1 O4 65.06(11) 7_545 . ?
O4 Rb1 O4 66.93(10) 2_665 . ?
O4 Rb1 O4 96.82(13) 8_455 . ?
O2 Rb2 O7 66.1(5) 15_565 . ?
O2 Rb2 O7 117.7(4) 9_766 . ?
O7 Rb2 O7 159.77(17) 7_646 . ?
O7 Rb2 O4 131.71(11) 7_646 4_556 ?
O7 Rb2 O4 68.24(10) . 4_556 ?
O7 Rb2 O4 68.23(10) 7_646 6_655 ?
O7 Rb2 O4 131.71(11) . 6_655 ?
O4 Rb2 O4 66.02(13) 4_556 6_655 ?
O7 Rb2 O6 64.30(11) 7_646 15_565 ?
O7 Rb2 O6 101.78(10) . 15_565 ?
O4 Rb2 O6 144.54(9) 4_556 15_565 ?
O4 Rb2 O6 106.31(10) 6_655 15_565 ?
O7 Rb2 O6 101.78(10) 7_646 9_766 ?
O7 Rb2 O6 64.30(11) . 9_766 ?
O4 Rb2 O6 106.31(10) 4_556 9_766 ?
O4 Rb2 O6 144.54(9) 6_655 9_766 ?
O6 Rb2 O6 98.45(15) 15_565 9_766 ?
O7 Rb2 O1 104.1(2) 7_646 3_646 ?
O7 Rb2 O1 86.0(3) . 3_646 ?
O4 Rb2 O1 67.80(17) 4_556 3_646 ?
O4 Rb2 O1 63.2(2) 6_655 3_646 ?
O6 Rb2 O1 77.82(17) 15_565 3_646 ?
O6 Rb2 O1 148.9(2) 9_766 3_646 ?
O7 Rb2 O1 86.0(3) 7_646 5_545 ?
O7 Rb2 O1 104.1(2) . 5_545 ?
O4 Rb2 O1 63.2(2) 4_556 5_545 ?
O4 Rb2 O1 67.80(17) 6_655 5_545 ?
O6 Rb2 O1 148.9(2) 15_565 5_545 ?
O6 Rb2 O1 77.82(17) 9_766 5_545 ?
O1 Rb2 O1 120.8(4) 3_646 5_545 ?
O7 Rb2 O6 40.36(10) 7_646 16_755 ?
O7 Rb2 O6 121.24(11) . 16_755 ?
O4 Rb2 O6 151.61(9) 4_556 16_755 ?
O4 Rb2 O6 106.42(9) 6_655 16_755 ?
O6 Rb2 O6 63.23(10) 15_565 16_755 ?
O6 Rb2 O6 62.95(11) 9_766 16_755 ?
O1 Rb2 O6 135.39(17) 3_646 16_755 ?
O1 Rb2 O6 88.4(2) 5_545 16_755 ?
O7 Rb2 O6 121.24(11) 7_646 10_556 ?
O7 Rb2 O6 40.35(10) . 10_556 ?
O4 Rb2 O6 106.42(9) 4_556 10_556 ?
O4 Rb2 O6 151.61(9) 6_655 10_556 ?
O6 Rb2 O6 62.95(11) 15_565 10_556 ?
O6 Rb2 O6 63.23(10) 9_766 10_556 ?
O1 Rb2 O6 88.4(2) 3_646 10_556 ?
O1 Rb2 O6 135.39(17) 5_545 10_556 ?
O6 Rb2 O6 92.26(12) 16_755 10_556 ?
O1 O1 Rb1 131.6(18) 13_665 . ?
O1 O1 Rb2 90(3) 13_665 5_454 ?
Rb1 O1 Rb2 103.8(10) . 5_454 ?
O1 O1 Rb2 65(3) 13_665 9_766 ?
Rb1 O1 Rb2 93.7(10) . 9_766 ?
Rb2 O1 Rb2 155.0(3) 5_454 9_766 ?
O1 O1 H1 95(5) 13_665 . ?
Rb1 O1 H1 123(4) . . ?
Rb2 O1 H1 107(6) 5_454 . ?
Rb2 O1 H1 76(6) 9_766 . ?
O2 O2 Rb1 120(5) 13_665 . ?
Rb2 O2 Rb1 105.4(9) 9_766 . ?
O2 O2 H1 89(5) 13_665 . ?
Rb2 O2 H1 118(6) 9_766 . ?
Rb1 O2 H1 109(6) . . ?
N1 O4 Rb1 131.6(3) . 2_665 ?
N1 O4 Rb2 126.8(3) . 6_654 ?
Rb1 O4 Rb2 101.63(9) 2_665 6_654 ?
N1 O4 Rb1 92.2(3) . . ?
Rb1 O4 Rb1 79.38(8) 2_665 . ?
Rb2 O4 Rb1 97.85(10) 6_654 . ?
N1 O5 Rb1 103.55(14) . 10_556 ?
N1 O5 Rb1 103.55(14) . . ?
Rb1 O5 Rb1 135.57(17) 10_556 . ?
N2 O6 Rb1 128.4(3) . . ?
N2 O6 Rb2 131.9(3) . 9_766 ?
Rb1 O6 Rb2 99.63(9) . 9_766 ?
N2 O6 Rb2 91.5(3) . 10_556 ?
Rb1 O6 Rb2 96.16(10) . 10_556 ?
Rb2 O6 Rb2 84.64(9) 9_766 10_556 ?
N2 O7 Rb2 106.56(12) . 10_556 ?
N2 O7 Rb2 106.56(12) . . ?
Rb2 O7 Rb2 136.13(17) 10_556 . ?
O5 N1 O4 120.5(3) . 10_556 ?
O5 N1 O4 120.5(3) . . ?
O4 N1 O4 119.1(6) 10_556 . ?
O5 N1 Rb1 56.29(12) . 10_556 ?
O4 N1 Rb1 66.5(2) 10_556 10_556 ?
O4 N1 Rb1 165.2(4) . 10_556 ?
O5 N1 Rb1 56.29(12) . . ?
O4 N1 Rb1 165.2(4) 10_556 . ?
O4 N1 Rb1 66.5(2) . . ?
Rb1 N1 Rb1 104.77(15) 10_556 . ?
O7 N2 O6 119.9(3) . . ?
O7 N2 O6 119.9(3) . 10_556 ?
O6 N2 O6 120.2(6) . 10_556 ?
O7 N2 Rb2 53.60(11) . 10_556 ?
O6 N2 Rb2 67.7(2) . 10_556 ?
O6 N2 Rb2 166.1(4) 10_556 10_556 ?
O7 N2 Rb2 53.60(11) . . ?
O6 N2 Rb2 166.1(4) . . ?
O6 N2 Rb2 67.7(2) 10_556 . ?
Rb2 N2 Rb2 102.34(14) 10_556 . ?
H31 O3 H32 106(8) . . ?

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 O5 N1 O4 -18.5(6) 10_556 . . 10_556 ?
Rb1 O5 N1 O4 -163.0(4) . . . 10_556 ?
Rb1 O5 N1 O4 163.0(4) 10_556 . . . ?
Rb1 O5 N1 O4 18.5(6) . . . . ?
Rb1 O5 N1 Rb1 -144.5(3) . . . 10_556 ?
Rb1 O5 N1 Rb1 144.5(3) 10_556 . . . ?
Rb1 O4 N1 O5 -94.5(6) 2_665 . . . ?
Rb2 O4 N1 O5 84.8(6) 6_654 . . . ?
Rb1 O4 N1 O5 -16.7(5) . . . . ?
Rb1 O4 N1 O4 86.9(6) 2_665 . . 10_556 ?
Rb2 O4 N1 O4 -93.8(6) 6_654 . . 10_556 ?
Rb1 O4 N1 O4 164.7(4) . . . 10_556 ?
Rb1 O4 N1 Rb1 -21.7(17) 2_665 . . 10_556 ?
Rb2 O4 N1 Rb1 157.6(11) 6_654 . . 10_556 ?
Rb1 O4 N1 Rb1 56.1(14) . . . 10_556 ?
Rb1 O4 N1 Rb1 -77.8(3) 2_665 . . . ?
Rb2 O4 N1 Rb1 101.5(3) 6_654 . . . ?
Rb2 O7 N2 O6 14.5(6) 10_556 . . . ?
Rb2 O7 N2 O6 165.3(4) . . . . ?
Rb2 O7 N2 O6 -165.3(4) 10_556 . . 10_556 ?
Rb2 O7 N2 O6 -14.5(6) . . . 10_556 ?
Rb2 O7 N2 Rb2 150.8(4) . . . 10_556 ?
Rb2 O7 N2 Rb2 -150.8(4) 10_556 . . . ?
Rb1 O6 N2 O7 86.5(6) . . . . ?
Rb2 O6 N2 O7 -96.7(6) 9_766 . . . ?
Rb2 O6 N2 O7 -12.5(5) 10_556 . . . ?
Rb1 O6 N2 O6 -93.7(6) . . . 10_556 ?
Rb2 O6 N2 O6 83.0(7) 9_766 . . 10_556 ?
Rb2 O6 N2 O6 167.2(5) 10_556 . . 10_556 ?
Rb1 O6 N2 Rb2 99.1(3) . . . 10_556 ?
Rb2 O6 N2 Rb2 -84.2(3) 9_766 . . 10_556 ?
Rb1 O6 N2 Rb2 144.8(12) . . . . ?
Rb2 O6 N2 Rb2 -38.4(16) 9_766 . . . ?
Rb2 O6 N2 Rb2 45.7(14) 10_556 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1^a H1 O3 0.80(6) 1.93(6) 2.696(9) 160(7) . yes
O2^b H1 O3 0.89(7) 1.93(6) 2.75(2) 155(8) . yes
O3 H31 O4 0.84(5) 2.25(4) 3.007(6) 150.9(10) 5_554 yes
O3 H31 O4 0.84(5) 2.25(4) 3.007(6) 150.9(10) 14 yes
O3 H32 O6 0.84(5) 2.24(5) 2.994(6) 150(2) 6_664 yes
O3 H32 O6 0.84(5) 2.24(5) 2.994(6) 150(2) 13_665 yes

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.152



####################################################################### 
# 
# 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_z
_database_code_depnum_ccdc_archive 'CCDC 2361133'
loop_
_audit_author_name
_audit_author_address
'Andrei Churakov'
;Institute of General and Inorganic Chemistry RAS
Russia
;
_audit_update_record             
;
2024-06-06 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'N O3, 0.5(H2 O2), Rb'
_chemical_formula_sum            'H N O4 Rb'
_chemical_formula_weight         164.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.7050(3)
_cell_length_b                   8.1533(3)
_cell_length_c                   7.2160(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.7189(13)
_cell_angle_gamma                90
_cell_volume                     394.04(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4656
_cell_measurement_theta_min      3.938
_cell_measurement_theta_max      30.496

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.773
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   0.5477
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    12.436
_shelx_estimated_absorpt_T_min   0.436
_shelx_estimated_absorpt_T_max   0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6218
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.773
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1150
_reflns_number_gt                1068
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0141P)²+0.0585P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0370(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1150
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0145
_refine_ls_wR_factor_ref         0.0309
_refine_ls_wR_factor_gt          0.0303
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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_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 0.13552(2) 0.27696(2) 0.35417(2) 0.01367(6) Uani 1 1 d . . . . .
N1 N 0.63536(15) 0.09122(15) 0.35202(14) 0.0111(2) Uani 1 1 d . . . . .
O11 O 0.71420(15) 0.20396(12) 0.44942(14) 0.0173(2) Uani 1 1 d . . . . .
O12 O 0.50638(14) 0.12565(12) 0.22606(13) 0.0162(2) Uani 1 1 d . . . . .
O13 O 0.68473(16) -0.05397(12) 0.38064(13) 0.0177(2) Uani 1 1 d . . . . .
O1 O 0.53635(18) 0.50791(14) 0.40610(14) 0.0238(2) Uani 1 1 d . . . . .
H1 H 0.594(3) 0.418(3) 0.395(2) 0.033(6) Uiso 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 O13 2.8638(10) 3_656 ?
Rb1 O12 2.9628(10) . ?
Rb1 O12 2.9669(9) 4_566 ?
Rb1 O11 2.9965(10) 4_565 ?
Rb1 O11 2.9985(11) 1_455 ?
Rb1 O13 3.0061(10) 2 ?
Rb1 O12 3.0447(10) 2 ?
Rb1 O1 3.0761(11) 2_545 ?
Rb1 O1 3.2479(12) 3_666 ?
Rb1 O1 3.2884(12) . ?
Rb1 N1 3.4382(11) 2 ?
Rb1 N1 3.6784(11) . ?
Rb1 H1 3.282(19) . ?
N1 O13 1.2438(16) . ?
N1 O12 1.2562(13) . ?
N1 O11 1.2583(15) . ?
O1 O1 1.467(2) 3_666 ?
O1 H1 0.83(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Rb1 O12 67.13(3) 3_656 . ?
O13 Rb1 O12 72.37(3) 3_656 4_566 ?
O12 Rb1 O12 132.76(3) . 4_566 ?
O13 Rb1 O11 126.61(3) 3_656 4_565 ?
O12 Rb1 O11 61.86(3) . 4_565 ?
O12 Rb1 O11 160.08(3) 4_566 4_565 ?
O13 Rb1 O11 95.28(3) 3_656 1_455 ?
O12 Rb1 O11 143.38(3) . 1_455 ?
O12 Rb1 O11 61.79(3) 4_566 1_455 ?
O11 Rb1 O11 116.43(3) 4_565 1_455 ?
O13 Rb1 O13 159.14(4) 3_656 2 ?
O12 Rb1 O13 127.07(3) . 2 ?
O12 Rb1 O13 98.96(3) 4_566 2 ?
O11 Rb1 O13 65.22(3) 4_565 2 ?
O11 Rb1 O13 64.20(3) 1_455 2 ?
O13 Rb1 O12 146.89(3) 3_656 2 ?
O12 Rb1 O12 126.07(2) . 2 ?
O12 Rb1 O12 79.64(3) 4_566 2 ?
O11 Rb1 O12 80.45(3) 4_565 2 ?
O11 Rb1 O12 86.54(3) 1_455 2 ?
O13 Rb1 O12 41.95(3) 2 2 ?
O13 Rb1 O1 95.10(3) 3_656 2_545 ?
O12 Rb1 O1 78.94(3) . 2_545 ?
O12 Rb1 O1 128.77(3) 4_566 2_545 ?
O11 Rb1 O1 61.32(3) 4_565 2_545 ?
O11 Rb1 O1 70.65(3) 1_455 2_545 ?
O13 Rb1 O1 75.28(3) 2 2_545 ?
O12 Rb1 O1 116.43(3) 2 2_545 ?
O13 Rb1 O1 74.57(3) 3_656 3_666 ?
O12 Rb1 O1 80.43(3) . 3_666 ?
O12 Rb1 O1 65.99(3) 4_566 3_666 ?
O11 Rb1 O1 110.18(3) 4_565 3_666 ?
O11 Rb1 O1 127.36(3) 1_455 3_666 ?
O13 Rb1 O1 120.02(3) 2 3_666 ?
O12 Rb1 O1 78.15(3) 2 3_666 ?
O1 Rb1 O1 159.23(4) 2_545 3_666 ?
O13 Rb1 O1 88.37(3) 3_656 . ?
O12 Rb1 O1 65.20(3) . . ?
O12 Rb1 O1 90.90(3) 4_566 . ?
O11 Rb1 O1 84.30(3) 4_565 . ?
O11 Rb1 O1 149.46(3) 1_455 . ?
O13 Rb1 O1 111.08(3) 2 . ?
O12 Rb1 O1 74.53(3) 2 . ?
O1 Rb1 O1 139.325(15) 2_545 . ?
O1 Rb1 O1 25.94(3) 3_666 . ?
O13 Rb1 N1 163.58(3) 3_656 2 ?
O12 Rb1 N1 127.54(3) . 2 ?
O12 Rb1 N1 91.21(3) 4_566 2 ?
O11 Rb1 N1 69.72(2) 4_565 2 ?
O11 Rb1 N1 76.29(3) 1_455 2 ?
O13 Rb1 N1 20.90(3) 2 2 ?
O12 Rb1 N1 21.25(2) 2 2 ?
O1 Rb1 N1 95.30(3) 2_545 2 ?
O1 Rb1 N1 99.13(3) 3_666 2 ?
O1 Rb1 N1 91.99(3) . 2 ?
O13 Rb1 N1 52.18(3) 3_656 . ?
O12 Rb1 N1 17.99(2) . . ?
O12 Rb1 N1 114.78(2) 4_566 . ?
O11 Rb1 N1 79.32(2) 4_565 . ?
O11 Rb1 N1 141.97(3) 1_455 . ?
O13 Rb1 N1 144.39(3) 2 . ?
O12 Rb1 N1 131.31(3) 2 . ?
O1 Rb1 N1 91.08(3) 2_545 . ?
O1 Rb1 N1 68.30(3) 3_666 . ?
O1 Rb1 N1 59.76(3) . . ?
N1 Rb1 N1 140.15(2) 2 . ?
O13 Rb1 H1 78.5(3) 3_656 . ?
O12 Rb1 H1 51.5(4) . . ?
O12 Rb1 H1 97.9(3) 4_566 . ?
O11 Rb1 H1 82.0(3) 4_565 . ?
O11 Rb1 H1 159.6(3) 1_455 . ?
O13 Rb1 H1 122.0(4) 2 . ?
O12 Rb1 H1 88.4(4) 2 . ?
O1 Rb1 H1 128.8(4) 2_545 . ?
O1 Rb1 H1 32.3(3) 3_666 . ?
O1 Rb1 H1 14.6(4) . . ?
N1 Rb1 H1 104.5(4) 2 . ?
N1 Rb1 H1 45.2(4) . . ?
O13 N1 O12 120.10(11) . . ?
O13 N1 O11 120.07(11) . . ?
O12 N1 O11 119.83(11) . . ?
O13 N1 Rb1 59.57(7) . 2_545 ?
O12 N1 Rb1 61.45(7) . 2_545 ?
O11 N1 Rb1 170.22(8) . 2_545 ?
O13 N1 Rb1 128.79(8) . . ?
O12 N1 Rb1 46.76(6) . . ?
O11 N1 Rb1 93.19(7) . . ?
Rb1 N1 Rb1 81.14(2) 2_545 . ?
O13 N1 Rb1 98.96(7) . 1_655 ?
O12 N1 Rb1 120.47(8) . 1_655 ?
O11 N1 Rb1 48.56(6) . 1_655 ?
Rb1 N1 Rb1 140.47(3) 2_545 1_655 ?
Rb1 N1 Rb1 131.38(3) . 1_655 ?
N1 O11 Rb1 119.58(8) . 4_666 ?
N1 O11 Rb1 113.10(8) . 1_655 ?
Rb1 O11 Rb1 115.12(3) 4_666 1_655 ?
N1 O12 Rb1 115.24(7) . . ?
N1 O12 Rb1 119.59(7) . 4_665 ?
Rb1 O12 Rb1 117.13(3) . 4_665 ?
N1 O12 Rb1 97.30(7) . 2_545 ?
Rb1 O12 Rb1 100.88(3) . 2_545 ?
Rb1 O12 Rb1 100.36(3) 4_665 2_545 ?
N1 O13 Rb1 144.63(8) . 3_656 ?
N1 O13 Rb1 99.52(7) . 2_545 ?
Rb1 O13 Rb1 110.62(3) 3_656 2_545 ?
O1 O1 Rb1 119.69(10) 3_666 2 ?
O1 O1 Rb1 78.57(9) 3_666 3_666 ?
Rb1 O1 Rb1 99.48(3) 2 3_666 ?
O1 O1 Rb1 75.49(9) 3_666 . ?
Rb1 O1 Rb1 93.34(3) 2 . ?
Rb1 O1 Rb1 154.06(3) 3_666 . ?
O1 O1 H1 100.9(13) 3_666 . ?
Rb1 O1 H1 136.8(12) 2 . ?
Rb1 O1 H1 102.8(12) 3_666 . ?
Rb1 O1 H1 82.2(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O11 0.83(2) 1.96(2) 2.7615(15) 162.4(18) . yes

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.087



####################################################################### 
# 
# 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_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2361134'
loop_
_audit_author_name
_audit_author_address
'Andrei Churakov'
;Institute of General and Inorganic Chemistry RAS
Russia
;
_audit_update_record             
;
2024-06-06 deposited with the CCDC.	2025-02-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H20 N, N O3, 2(H2 O2)'
_chemical_formula_sum            'C8 H24 N2 O7'
_chemical_formula_weight         260.29

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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.3185(4)
_cell_length_b                   14.6896(5)
_cell_length_c                   15.1162(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2735.33(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.695
_cell_measurement_theta_max      30.349

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             1136
_exptl_transmission_factor_min   0.8481
_exptl_transmission_factor_max   0.9281
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.109
_shelx_estimated_absorpt_T_min   0.973
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33352
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.544
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2988
_reflns_number_gt                2599
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0376P)²+1.1500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2988
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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_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
N1 N 0.47903(7) 0.40212(6) 0.74221(6) 0.0157(2) Uani 1 1 d . . . . .
C1 C 0.39799(10) 0.46059(8) 0.69231(8) 0.0227(3) Uani 1 1 d . . . . .
C2 C 0.44724(14) 0.52182(11) 0.62319(10) 0.0372(3) Uani 1 1 d . . . . .
C3 C 0.54412(9) 0.34309(8) 0.67866(8) 0.0191(2) Uani 1 1 d . . . . .
C4 C 0.47676(11) 0.28190(9) 0.61969(9) 0.0277(3) Uani 1 1 d . . . . .
C5 C 0.41318(9) 0.34420(8) 0.80591(8) 0.0197(2) Uani 1 1 d . . . . .
C6 C 0.47928(11) 0.28331(9) 0.86558(9) 0.0281(3) Uani 1 1 d . . . . .
C7 C 0.56064(9) 0.46055(8) 0.79172(8) 0.0200(2) Uani 1 1 d . . . . .
C8 C 0.51240(11) 0.52335(9) 0.86050(9) 0.0283(3) Uani 1 1 d . . . . .
H11 H 0.3598(12) 0.4958(9) 0.7366(9) 0.026(3) Uiso 1 1 d . . . . .
H12 H 0.3475(12) 0.4176(9) 0.6659(9) 0.027(4) Uiso 1 1 d . . . . .
H21 H 0.3910(15) 0.5552(12) 0.5965(11) 0.047(5) Uiso 1 1 d . . . . .
H22 H 0.4822(15) 0.4881(12) 0.5779(12) 0.046(5) Uiso 1 1 d . . . . .
H23 H 0.4966(15) 0.5662(11) 0.6470(11) 0.046(5) Uiso 1 1 d . . . . .
H31 H 0.5880(11) 0.3859(9) 0.6448(9) 0.024(3) Uiso 1 1 d . . . . .
H32 H 0.5924(11) 0.3064(9) 0.7164(8) 0.019(3) Uiso 1 1 d . . . . .
H41 H 0.4328(14) 0.3169(11) 0.5776(11) 0.038(4) Uiso 1 1 d . . . . .
H42 H 0.5258(12) 0.2464(11) 0.5854(10) 0.032(4) Uiso 1 1 d . . . . .
H43 H 0.4334(12) 0.2391(11) 0.6521(10) 0.036(4) Uiso 1 1 d . . . . .
H51 H 0.3701(11) 0.3875(9) 0.8397(9) 0.022(3) Uiso 1 1 d . . . . .
H52 H 0.3656(12) 0.3079(9) 0.7689(9) 0.023(3) Uiso 1 1 d . . . . .
H61 H 0.5261(14) 0.3186(11) 0.9058(11) 0.040(4) Uiso 1 1 d . . . . .
H62 H 0.5209(13) 0.2385(11) 0.8319(10) 0.036(4) Uiso 1 1 d . . . . .
H63 H 0.4288(12) 0.2495(11) 0.9010(10) 0.033(4) Uiso 1 1 d . . . . .
H71 H 0.6110(11) 0.4176(8) 0.8187(9) 0.019(3) Uiso 1 1 d . . . . .
H72 H 0.5996(11) 0.4939(9) 0.7469(9) 0.023(3) Uiso 1 1 d . . . . .
H81 H 0.5706(13) 0.5566(11) 0.8866(10) 0.037(4) Uiso 1 1 d . . . . .
H82 H 0.4769(13) 0.4902(10) 0.9093(10) 0.033(4) Uiso 1 1 d . . . . .
H83 H 0.4632(13) 0.5681(10) 0.8354(10) 0.032(4) Uiso 1 1 d . . . . .
N2 N 0.75956(8) 0.58578(7) 0.54531(6) 0.0198(2) Uani 1 1 d . . . . .
O11 O 0.75885(8) 0.66092(6) 0.58627(6) 0.0292(2) Uani 1 1 d . . . . .
O12 O 0.73504(7) 0.51454(6) 0.58645(6) 0.0263(2) Uani 1 1 d . . . . .
O13 O 0.78482(8) 0.58382(6) 0.46631(6) 0.0315(2) Uani 1 1 d . . . . .
O1 O 0.71202(8) 0.63710(6) 0.76311(6) 0.0305(2) Uani 1 1 d . . . . .
O2 O 0.77810(8) 0.71235(7) 0.79663(6) 0.0321(2) Uani 1 1 d . . . . .
H1 H 0.7308(14) 0.6421(11) 0.7070(13) 0.045(5) Uiso 1 1 d . . . . .
H2 H 0.7780(15) 0.6983(13) 0.8529(14) 0.055(5) Uiso 1 1 d . . . . .
O3 O 0.80162(8) 0.80872(6) 0.48018(6) 0.0306(2) Uani 1 1 d . . . . .
O4 O 0.70349(8) 0.86189(6) 0.48820(7) 0.0303(2) Uani 1 1 d . . . . .
H3 H 0.7848(14) 0.7627(13) 0.5170(12) 0.046(5) Uiso 1 1 d . . . . .
H4 H 0.7318(15) 0.9143(12) 0.5152(13) 0.052(5) Uiso 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
N1 C1 1.5177(14) . ?
N1 C7 1.5191(14) . ?
N1 C5 1.5196(14) . ?
N1 C3 1.5224(13) . ?
C1 C2 1.5062(19) . ?
C1 H11 0.968(14) . ?
C1 H12 0.972(15) . ?
C2 H21 0.939(18) . ?
C2 H22 0.948(18) . ?
C2 H23 0.961(18) . ?
C3 C4 1.5137(17) . ?
C3 H31 0.975(14) . ?
C3 H32 0.984(13) . ?
C4 H41 0.981(17) . ?
C4 H42 0.952(16) . ?
C4 H43 0.960(16) . ?
C5 C6 1.5089(17) . ?
C5 H51 0.973(14) . ?
C5 H52 0.970(14) . ?
C6 H61 0.986(17) . ?
C6 H62 0.977(16) . ?
C6 H63 0.959(16) . ?
C7 C8 1.5116(17) . ?
C7 H71 0.974(13) . ?
C7 H72 0.964(14) . ?
C8 H81 0.953(17) . ?
C8 H82 0.986(16) . ?
C8 H83 0.971(16) . ?
N2 O13 1.2343(13) . ?
N2 O12 1.2543(13) . ?
N2 O11 1.2655(13) . ?
O1 O2 1.4634(13) . ?
O1 H1 0.882(19) . ?
O2 H2 0.88(2) . ?
O3 O4 1.4443(13) . ?
O3 H3 0.899(19) . ?
O4 H4 0.939(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C7 111.13(8) . . ?
C1 N1 C5 106.30(9) . . ?
C7 N1 C5 110.94(8) . . ?
C1 N1 C3 110.80(8) . . ?
C7 N1 C3 106.50(8) . . ?
C5 N1 C3 111.23(8) . . ?
C2 C1 N1 114.69(10) . . ?
C2 C1 H11 110.9(8) . . ?
N1 C1 H11 106.1(8) . . ?
C2 C1 H12 111.2(8) . . ?
N1 C1 H12 104.9(8) . . ?
H11 C1 H12 108.6(12) . . ?
C1 C2 H21 108.1(11) . . ?
C1 C2 H22 111.9(10) . . ?
H21 C2 H22 107.3(15) . . ?
C1 C2 H23 113.6(10) . . ?
H21 C2 H23 105.9(14) . . ?
H22 C2 H23 109.7(15) . . ?
C4 C3 N1 114.90(9) . . ?
C4 C3 H31 112.2(8) . . ?
N1 C3 H31 104.9(8) . . ?
C4 C3 H32 110.3(7) . . ?
N1 C3 H32 105.3(7) . . ?
H31 C3 H32 108.8(11) . . ?
C3 C4 H41 111.9(9) . . ?
C3 C4 H42 107.3(9) . . ?
H41 C4 H42 106.6(13) . . ?
C3 C4 H43 113.1(9) . . ?
H41 C4 H43 111.5(13) . . ?
H42 C4 H43 105.9(13) . . ?
C6 C5 N1 115.00(9) . . ?
C6 C5 H51 111.6(8) . . ?
N1 C5 H51 105.0(8) . . ?
C6 C5 H52 110.2(8) . . ?
N1 C5 H52 105.4(8) . . ?
H51 C5 H52 109.4(12) . . ?
C5 C6 H61 111.8(9) . . ?
C5 C6 H62 111.8(9) . . ?
H61 C6 H62 111.6(13) . . ?
C5 C6 H63 106.9(9) . . ?
H61 C6 H63 107.9(13) . . ?
H62 C6 H63 106.4(13) . . ?
C8 C7 N1 115.05(9) . . ?
C8 C7 H71 110.9(8) . . ?
N1 C7 H71 105.2(8) . . ?
C8 C7 H72 111.6(8) . . ?
N1 C7 H72 105.7(8) . . ?
H71 C7 H72 107.9(11) . . ?
C7 C8 H81 107.6(10) . . ?
C7 C8 H82 112.8(9) . . ?
H81 C8 H82 106.1(13) . . ?
C7 C8 H83 112.9(9) . . ?
H81 C8 H83 106.5(12) . . ?
H82 C8 H83 110.5(13) . . ?
O13 N2 O12 121.40(10) . . ?
O13 N2 O11 119.69(10) . . ?
O12 N2 O11 118.91(9) . . ?
O2 O1 H1 97.1(11) . . ?
O1 O2 H2 99.1(12) . . ?
O4 O3 H3 99.3(11) . . ?
O3 O4 H4 99.7(11) . . ?

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
C7 N1 C1 C2 60.85(13) . . . . ?
C5 N1 C1 C2 -178.33(11) . . . . ?
C3 N1 C1 C2 -57.35(13) . . . . ?
C1 N1 C3 C4 -56.60(13) . . . . ?
C7 N1 C3 C4 -177.58(10) . . . . ?
C5 N1 C3 C4 61.42(12) . . . . ?
C1 N1 C5 C6 -177.38(10) . . . . ?
C7 N1 C5 C6 -56.45(13) . . . . ?
C3 N1 C5 C6 61.91(13) . . . . ?
C1 N1 C7 C8 60.60(13) . . . . ?
C5 N1 C7 C8 -57.44(13) . . . . ?
C3 N1 C7 C8 -178.62(10) . . . . ?
H1 O1 O2 H2 -162.6(17) . . . . ?
H3 O3 O4 H4 114.6(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O11 0.882(19) 1.878(19) 2.7570(13) 174.2(17) . yes
O3 H3 O11 0.899(19) 1.854(19) 2.7501(13) 174.5(17) . yes
O2 H2 O3 0.88(2) 1.95(2) 2.8068(14) 166.4(18) 7_576 yes
O4 H4 O12 0.939(19) 1.87(2) 2.7941(13) 167.9(18) 8_765 yes

_refine_diff_density_max         0.243
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.036



