#------------------------------------------------------------------------------
#$Date: 2024-11-09 14:07:10 +0200 (Sat, 09 Nov 2024) $
#$Revision: 295862 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/54/7245423.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7245423
loop_
_publ_author_name
'Stolar, Tomislav'
'Alić, Jasna'
'Lončarić, Ivor'
'Etter, Martin'
'Jung, Dahee'
'Farha, Omar K.'
'Đilović, Ivica'
'Meštrović, Ernest'
'Užarević, Krunoslav'
_publ_section_title
;
 Sustainable solid form screening: mechanochemical control over nucleobase
 hydrogen-bonded organic framework polymorphism
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00668E
_journal_year                    2022
_chemical_formula_moiety         'C5 H6 N6'
_chemical_formula_sum            'C5 H6 N6'
_chemical_formula_weight         150.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-23 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                109.619(3)
_cell_angle_beta                 108.625(3)
_cell_angle_gamma                107.919(3)
_cell_formula_units_Z            6
_cell_length_a                   10.7265(5)
_cell_length_b                   11.3448(2)
_cell_length_c                   11.6327(4)
_cell_measurement_reflns_used    16920
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.9580
_cell_measurement_theta_min      4.5660
_cell_volume                     1118.77(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -40.00   0.50    0.20    --  -46.91 -64.00-162.00  138
  2  ω    -57.00  11.00   0.50    0.20    --  -46.91  64.00 -26.00  136
  3  ω     64.00 101.00   0.50    0.20    --   46.91  64.00 -26.00   74
  4  ω     -2.00  62.00   0.50    0.20    --   46.91 -64.00-162.00  128
  5  ω   -154.00-108.00   0.50    0.80    --  -86.25 -64.00-162.00   92
  6  ω    -69.00 -44.00   0.50    0.80    --  -86.25  64.00 -26.00   50
  7  ω     35.00  75.00   0.50    0.80    --  107.75 -64.00-162.00   80
  8  ω     98.00 167.00   0.50    0.80    --  107.75  64.00 -26.00  138
  9  ω   -110.00 -75.00   0.50    0.20    --  -46.91-125.00  30.00   70
 10  ω   -116.00 -74.00   0.50    0.20    --  -46.91-125.00-150.00   84
 11  ω    -27.00  29.00   0.50    0.20    --  -46.91  19.00 -90.00  112
 12  ω    -25.00  27.00   0.50    0.20    --   46.91 -19.00  90.00  104
 13  ω     35.00  94.00   0.50    0.20    --   46.91-125.00  60.00  118
 14  ω    -47.00 -16.00   0.50    0.80    --  -86.25  45.00-180.00   62
 15  ω    -51.00 -14.00   0.50    0.80    --  -86.25  45.00 150.00   74
 16  ω     79.00 108.00   0.50    0.80    --  107.75-111.00 -58.68   58
 17  ω     36.00  62.00   0.50    0.80    --  107.75-111.00 -58.68   52
 18  ω     35.00 100.00   0.50    0.80    --  107.75 -95.00  90.00  130
 19  ω     35.00  71.00   0.50    0.80    --  107.75 -61.00 150.00   72
 20  ω     40.00  69.00   0.50    0.80    --  107.75-125.00   0.00   58
 21  ω     74.00 111.00   0.50    0.80    --  107.75-125.00   0.00   74
 22  ω     78.00 103.00   0.50    0.80    --  107.75 -95.00-150.00   50
 23  ω    117.00 176.00   0.50    0.80    --  107.75  38.00 -84.84  118
 24  ω     95.00 140.00   0.50    0.80    --  107.75 125.00 -90.00   90
 25  ω     42.00  97.00   0.50    0.80    --  107.75 -95.00   0.00  110
 26  ω     39.00  64.00   0.50    0.80    --  107.75-125.00-180.00   50
 27  ω     87.00 112.00   0.50    0.80    --  107.75-125.00-180.00   50
 28  ω    145.00 174.00   0.50    0.80    --  107.75 125.00 -90.00   58
 29  ω    105.00 177.00   0.50    0.80    --  107.75  26.00-119.12  144
 30  ω     37.00  63.00   0.50    0.80    --  107.75 -61.00 -90.00   52
 31  ω     95.00 178.00   0.50    0.80    --  107.75  45.00  90.00  166
 32  ω     39.00  80.00   0.50    0.80    --  107.75 -77.00-120.00   82
 33  ω     40.00 102.00   0.50    0.80    --  107.75 -95.00  60.00  124
 34  ω    117.00 174.00   0.50    0.80    --  107.75  30.00-180.00  114
 35  ω     41.00  66.00   0.50    0.80    --  107.75 -95.00 120.00   50
 36  ω     37.00  68.00   0.50    0.80    --  107.75 -95.00 -30.00   62
 37  ω     77.00 103.00   0.50    0.80    --  107.75 -95.00  30.00   52
 38  ω     98.00 127.00   0.50    0.80    --  107.75 125.00  60.00   58
 39  ω     36.00 103.00   0.50    0.80    --  107.75 -95.00 150.00  134
 40  ω    123.00 176.00   0.50    0.80    --  107.75  77.00-180.00  106
 41  ω     76.00 108.00   0.50    0.80    --  107.75-109.00  50.89   64
 42  ω     35.00  60.00   0.50    0.80    --  107.75 -95.00  30.00   50
 43  ω     63.00 112.00   0.50    0.80    --  107.75-125.00-150.00   98
 44  ω     39.00  90.00   0.50    0.80    --  107.75-125.00  30.00  102
 45  ω     61.00 107.00   0.50    0.80    --  107.75-106.00-110.40   92
 46  ω    150.00 175.00   0.50    0.80    --  107.75 125.00  60.00   50
 47  ω     35.00  62.00   0.50    0.80    --  107.75 -61.00  90.00   54
 48  ω     52.00  78.00   0.50    0.80    --  107.75-125.00 150.00   52
 49  ω     86.00 112.00   0.50    0.80    --  107.75-125.00 150.00   52
 50  ω     43.00  69.00   0.50    0.80    --  107.75 -77.00 120.00   52
 51  ω     38.00  64.00   0.50    0.80    --  107.75 -77.00 150.00   52
 52  ω     43.00  70.00   0.50    0.80    --  107.75 -95.00 -90.00   54
 53  ω     64.00 112.00   0.50    0.80    --  107.75-125.00  60.00   96
 54  ω    104.00 129.00   0.50    0.80    --  107.75  91.00  39.20   50
 55  ω    137.00 178.00   0.50    0.80    --  107.75  91.00  39.20   82
 56  ω    105.00 172.00   0.50    0.80    --  107.75  30.00  30.00  134
 57  ω    126.00 158.00   0.50    0.80    --  107.75  -3.00  94.12   64
 58  ω     75.00 111.00   0.50    0.80    --  107.75-124.00 -45.82   72
 59  ω     42.00 112.00   0.50    0.80    --  107.75-125.00-120.00  140
 60  ω     36.00  67.00   0.50    0.80    --  107.75 -61.00   0.00   62
 61  ω     44.00  83.00   0.50    0.80    --  107.75-141.00 109.00   78
 62  ω    -79.00 -35.00   0.50    0.20    --  -46.91 130.00  -5.00   88
 63  ω    -13.00  15.00   0.50    0.20    --   46.91 -19.00 -30.00   56
 64  ω    145.00 171.00   0.50    0.80    --  107.75  15.00 -30.00   52
 65  ω     61.00  87.00   0.50    0.80    --  107.75-135.00  17.98   52
 66  ω     38.00  65.00   0.50    0.80    --  107.75 -77.00   0.00   54
 67  ω     67.00  93.00   0.50    0.80    --  107.75 -77.00   0.00   52
 68  ω     80.00 105.00   0.50    0.80    --  107.75 -95.00  60.00   50
 69  ω     43.00  69.00   0.50    0.80    --  107.75 -61.00-180.00   52
 70  ω     37.00  75.00   0.50    0.80    --  107.75 -77.00-180.00   76
 71  ω     94.00 119.00   0.50    0.80    --  107.75-135.00  17.98   50
 72  ω    116.00 173.00   0.50    0.80    --  107.75  45.00 150.00  114
 73  ω     94.00 147.00   0.50    0.80    --  107.75  77.00  60.00  106
 74  ω     47.00  73.00   0.50    0.80    --  107.75 -77.00 -60.00   52
 75  ω     80.00 105.00   0.50    0.80    --  107.75 -77.00 -60.00   50
 76  ω     50.00  88.00   0.50    0.80    --  107.75-125.00 150.00   76
 77  ω    146.00 172.00   0.50    0.80    --  107.75 125.00  90.00   52
 78  ω    107.00 139.00   0.50    0.80    --  107.75  15.00 -30.00   64
 79  ω     96.00 122.00   0.50    0.80    --  107.75-141.00 109.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299184000
_diffrn_orient_matrix_UB_12      -0.1219036000
_diffrn_orient_matrix_UB_13      0.0088048000
_diffrn_orient_matrix_UB_21      0.1587386000
_diffrn_orient_matrix_UB_22      0.1076000000
_diffrn_orient_matrix_UB_23      0.1176734000
_diffrn_orient_matrix_UB_31      -0.0566252000
_diffrn_orient_matrix_UB_32      0.0084621000
_diffrn_orient_matrix_UB_33      0.1072286000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7318
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.995
_diffrn_reflns_theta_max         65.995
_diffrn_reflns_theta_min         4.674
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method isopropanol
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1757P)²+0.4101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6644
_reflns_number_total             7318
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 118.3424° 
around [0.90 -0.30 -0.31] (reciprocal) or [1.00 -0.01 0.00] (direct)
;
_cod_data_source_file            d2ce00668e2.cif
_cod_data_source_block           manu_2_comp_twin1_hklf4
_cod_depositor_comments
;

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C15 H18 N18'
_cod_original_formula_weight         450.47
_cod_original_formula_moiety         '3(C5 H6 N6)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1118.77(8)
_cod_database_code               7245423
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         '(C5 H6 N6)3 OH2'
_chemical_oxdiff_usercomment     'C5 H6 N6'
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7487(18)
 0.2513(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
3.a Rotating group:
 N36(H36A), N26(H26A)
3.b Aromatic/amide H refined with riding coordinates:
 N33(H33), N13(H13), N23(H23), C35(H35), C25(H25), C15(H15)
3.c X=CH2 refined with riding coordinates:
 N35(H35A,H35B), N15(H15A,H15B), N25(H25A,H25B), N16(H16A,H16B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'Mounted in cryo mesh'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.739
_oxdiff_exptl_absorpt_empirical_full_min 0.603
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
N31 N 1.1084(2) 0.8092(2) 0.9483(2) 0.0236(5) Uani 1 1 d . . . . .
N21 N 1.3327(2) 0.9356(2) 0.6344(2) 0.0238(5) Uani 1 1 d . . . . .
N35 N 1.2490(3) 0.8763(2) 0.8451(2) 0.0252(5) Uani 1 1 d . . . . .
H35A H 1.315352 0.857479 0.892153 0.030 Uiso 1 1 calc R U . . .
H35B H 1.262864 0.907496 0.788219 0.030 Uiso 1 1 calc R U . . .
N11 N 1.2015(2) 0.3622(2) 0.8057(2) 0.0238(5) Uani 1 1 d . . . . .
N32 N 0.8673(3) 0.8028(3) 0.8915(3) 0.0294(6) Uani 1 1 d . . . . .
N15 N 1.1351(3) 0.5365(2) 0.8867(2) 0.0262(5) Uani 1 1 d . . . . .
H15A H 1.048835 0.471020 0.864974 0.031 Uiso 1 1 calc R U . . .
H15B H 1.155529 0.626051 0.923981 0.031 Uiso 1 1 calc R U . . .
N24 N 1.1907(3) 0.6911(3) 0.2634(2) 0.0302(6) Uani 1 1 d . . . . .
N25 N 1.0909(3) 0.8349(2) 0.4650(2) 0.0258(5) Uani 1 1 d . . . . .
H25A H 1.069465 0.879076 0.528167 0.031 Uiso 1 1 calc R U . . .
H25B H 1.021370 0.780050 0.378228 0.031 Uiso 1 1 calc R U . . .
N34 N 1.0023(3) 0.9330(2) 0.6914(3) 0.0287(5) Uani 1 1 d . . . . .
N14 N 1.4409(3) 0.7446(2) 0.9491(3) 0.0294(5) Uani 1 1 d . . . . .
N33 N 0.8005(3) 0.8830(3) 0.7211(3) 0.0323(6) Uani 1 1 d . . . . .
H33 H 0.712324 0.873680 0.710279 0.039 Uiso 1 1 calc R U . . .
N22 N 1.5213(3) 0.8839(2) 0.5909(2) 0.0287(5) Uani 1 1 d . . . . .
N36 N 0.9712(3) 0.7355(3) 1.0483(3) 0.0360(6) Uani 1 1 d . . . . .
H36A H 0.893594 0.734397 1.060075 0.043 Uiso 1 1 d R U . . .
N16 N 1.2565(3) 0.1836(3) 0.7183(3) 0.0329(6) Uani 1 1 d . . . . .
H16A H 1.313583 0.150945 0.693706 0.039 Uiso 1 1 calc R U . . .
H16B H 1.170708 0.124798 0.704652 0.039 Uiso 1 1 calc R U . . .
N12 N 1.4325(3) 0.4088(2) 0.7954(3) 0.0286(5) Uani 1 1 d . . . . .
N13 N 1.5858(3) 0.6613(2) 0.8878(3) 0.0331(6) Uani 1 1 d . . . . .
H13 H 1.662741 0.661722 0.875634 0.040 Uiso 1 1 calc R U . . .
N23 N 1.4232(3) 0.7211(3) 0.3460(3) 0.0320(6) Uani 1 1 d . . . . .
H23 H 1.501822 0.711619 0.346708 0.038 Uiso 1 1 calc R U . . .
N26 N 1.5693(3) 1.0360(3) 0.8084(3) 0.0348(6) Uani 1 1 d . . . . .
H26A H 1.661547 1.061733 0.821729 0.042 Uiso 1 1 d R U . . .
C34 C 1.0169(3) 0.8860(3) 0.7890(3) 0.0247(6) Uani 1 1 d . . . . .
C31 C 1.1268(3) 0.8573(3) 0.8602(3) 0.0220(6) Uani 1 1 d . . . . .
C33 C 0.8923(3) 0.8546(3) 0.8082(3) 0.0267(6) Uani 1 1 d . . . . .
C21 C 1.2289(3) 0.8511(3) 0.5010(3) 0.0228(6) Uani 1 1 d . . . . .
C11 C 1.2358(3) 0.4999(3) 0.8629(3) 0.0222(6) Uani 1 1 d . . . . .
C32 C 0.9820(3) 0.7857(3) 0.9600(3) 0.0254(6) Uani 1 1 d . . . . .
C22 C 1.4724(3) 0.9496(3) 0.6722(3) 0.0254(6) Uani 1 1 d . . . . .
C14 C 1.3751(3) 0.5986(3) 0.8942(3) 0.0252(6) Uani 1 1 d . . . . .
C12 C 1.3004(3) 0.3238(3) 0.7769(3) 0.0250(6) Uani 1 1 d . . . . .
C24 C 1.2704(3) 0.7832(3) 0.4046(3) 0.0246(6) Uani 1 1 d . . . . .
C13 C 1.4640(3) 0.5451(3) 0.8555(3) 0.0260(6) Uani 1 1 d . . . . .
C23 C 1.4147(3) 0.8034(3) 0.4577(3) 0.0264(6) Uani 1 1 d . . . . .
C35 C 0.8713(3) 0.9284(3) 0.6545(3) 0.0319(6) Uani 1 1 d . . . . .
H35 H 0.829863 0.954237 0.587633 0.038 Uiso 1 1 calc R U . . .
C25 C 1.2875(3) 0.6570(3) 0.2343(3) 0.0326(7) Uani 1 1 d . . . . .
H25 H 1.264773 0.593664 0.143846 0.039 Uiso 1 1 calc R U . . .
C15 C 1.5651(3) 0.7760(3) 0.9422(3) 0.0330(7) Uani 1 1 d . . . . .
H15 H 1.634382 0.869642 0.972251 0.040 Uiso 1 1 calc R U . . .
H36B H 1.049(5) 0.733(4) 1.106(4) 0.040(9) Uiso 1 1 d . . . . .
H26B H 1.553(4) 1.094(4) 0.862(4) 0.039(10) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 N31 C32 118.6(2) . . ?
C21 N21 C22 118.9(2) . . ?
H35A N35 H35B 120.0 . . ?
C31 N35 H35A 120.0 . . ?
C31 N35 H35B 120.0 . . ?
C11 N11 C12 119.1(2) . . ?
C33 N32 C32 111.8(2) . . ?
H15A N15 H15B 120.0 . . ?
C11 N15 H15A 120.0 . . ?
C11 N15 H15B 120.0 . . ?
C25 N24 C24 103.5(2) . . ?
H25A N25 H25B 120.0 . . ?
C21 N25 H25A 120.0 . . ?
C21 N25 H25B 120.0 . . ?
C35 N34 C34 103.7(2) . . ?
C15 N14 C14 103.9(2) . . ?
C33 N33 H33 126.5 . . ?
C35 N33 H33 126.5 . . ?
C35 N33 C33 107.0(2) . . ?
C22 N22 C23 111.6(2) . . ?
H36A N36 H36B 125.8 . . ?
C32 N36 H36A 109.9 . . ?
C32 N36 H36B 121(3) . . ?
H16A N16 H16B 120.0 . . ?
C12 N16 H16A 120.0 . . ?
C12 N16 H16B 120.0 . . ?
C13 N12 C12 111.8(2) . . ?
C13 N13 H13 126.5 . . ?
C15 N13 H13 126.5 . . ?
C15 N13 C13 107.1(2) . . ?
C23 N23 H23 126.5 . . ?
C25 N23 H23 126.5 . . ?
C25 N23 C23 107.1(2) . . ?
H26A N26 H26B 118.0 . . ?
C22 N26 H26A 110.0 . . ?
C22 N26 H26B 123(3) . . ?
N34 C34 C31 132.0(2) . . ?
C33 C34 N34 110.7(2) . . ?
C33 C34 C31 117.2(2) . . ?
N31 C31 C34 118.3(2) . . ?
N35 C31 N31 118.7(2) . . ?
N35 C31 C34 123.0(2) . . ?
N32 C33 N33 128.5(2) . . ?
N32 C33 C34 126.4(2) . . ?
N33 C33 C34 105.1(2) . . ?
N21 C21 C24 118.6(2) . . ?
N25 C21 N21 118.7(2) . . ?
N25 C21 C24 122.8(2) . . ?
N11 C11 C14 118.3(2) . . ?
N15 C11 N11 118.7(2) . . ?
N15 C11 C14 123.0(2) . . ?
N32 C32 N31 127.6(2) . . ?
N32 C32 N36 117.6(2) . . ?
N36 C32 N31 114.8(2) . . ?
N22 C22 N21 127.3(3) . . ?
N22 C22 N26 117.8(2) . . ?
N26 C22 N21 114.9(2) . . ?
N14 C14 C11 132.1(2) . . ?
C13 C14 N14 110.9(2) . . ?
C13 C14 C11 116.9(2) . . ?
N16 C12 N11 115.2(2) . . ?
N12 C12 N11 127.2(2) . . ?
N12 C12 N16 117.5(2) . . ?
N24 C24 C21 132.2(2) . . ?
C23 C24 N24 111.3(2) . . ?
C23 C24 C21 116.4(2) . . ?
N12 C13 N13 128.6(2) . . ?
N12 C13 C14 126.6(3) . . ?
N13 C13 C14 104.7(2) . . ?
N22 C23 N23 128.2(2) . . ?
N22 C23 C24 127.0(2) . . ?
N23 C23 C24 104.7(2) . . ?
N34 C35 N33 113.6(3) . . ?
N34 C35 H35 123.2 . . ?
N33 C35 H35 123.2 . . ?
N24 C25 N23 113.4(3) . . ?
N24 C25 H25 123.3 . . ?
N23 C25 H25 123.3 . . ?
N14 C15 N13 113.5(2) . . ?
N14 C15 H15 123.3 . . ?
N13 C15 H15 123.3 . . ?
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
N31 C31 1.351(3) . ?
N31 C32 1.359(4) . ?
N21 C21 1.344(4) . ?
N21 C22 1.360(4) . ?
N35 H35A 0.8800 . ?
N35 H35B 0.8800 . ?
N35 C31 1.339(4) . ?
N11 C11 1.345(3) . ?
N11 C12 1.357(3) . ?
N32 C33 1.344(4) . ?
N32 C32 1.345(4) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N15 C11 1.344(3) . ?
N24 C24 1.386(4) . ?
N24 C25 1.314(4) . ?
N25 H25A 0.8800 . ?
N25 H25B 0.8800 . ?
N25 C21 1.337(4) . ?
N34 C34 1.394(3) . ?
N34 C35 1.310(4) . ?
N14 C14 1.390(3) . ?
N14 C15 1.306(4) . ?
N33 H33 0.8800 . ?
N33 C33 1.371(4) . ?
N33 C35 1.358(4) . ?
N22 C22 1.344(4) . ?
N22 C23 1.348(4) . ?
N36 H36A 0.8831 . ?
N36 C32 1.350(4) . ?
N36 H36B 0.91(4) . ?
N16 H16A 0.8800 . ?
N16 H16B 0.8800 . ?
N16 C12 1.350(4) . ?
N12 C12 1.345(4) . ?
N12 C13 1.340(4) . ?
N13 H13 0.8800 . ?
N13 C13 1.371(4) . ?
N13 C15 1.363(4) . ?
N23 H23 0.8800 . ?
N23 C23 1.373(4) . ?
N23 C25 1.357(4) . ?
N26 H26A 0.8840 . ?
N26 C22 1.353(4) . ?
N26 H26B 0.85(4) . ?
C34 C31 1.405(4) . ?
C34 C33 1.383(4) . ?
C21 C24 1.414(4) . ?
C11 C14 1.403(4) . ?
C14 C13 1.388(4) . ?
C24 C23 1.380(4) . ?
C35 H35 0.9500 . ?
C25 H25 0.9500 . ?
C15 H15 0.9500 . ?
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
N21 C21 C24 N24 179.5(3) . . . . ?
N21 C21 C24 C23 3.5(4) . . . . ?
N11 C11 C14 N14 178.1(3) . . . . ?
N11 C11 C14 C13 3.9(4) . . . . ?
N15 C11 C14 N14 -1.5(5) . . . . ?
N15 C11 C14 C13 -175.8(2) . . . . ?
N24 C24 C23 N22 -178.7(3) . . . . ?
N24 C24 C23 N23 -0.2(3) . . . . ?
N25 C21 C24 N24 -0.6(5) . . . . ?
N25 C21 C24 C23 -176.5(2) . . . . ?
N34 C34 C31 N31 -178.6(2) . . . . ?
N34 C34 C31 N35 1.8(5) . . . . ?
N34 C34 C33 N32 177.9(3) . . . . ?
N34 C34 C33 N33 0.0(3) . . . . ?
N14 C14 C13 N12 -177.8(3) . . . . ?
N14 C14 C13 N13 0.0(3) . . . . ?
C34 N34 C35 N33 0.4(3) . . . . ?
C31 N31 C32 N32 1.0(4) . . . . ?
C31 N31 C32 N36 178.9(2) . . . . ?
C31 C34 C33 N32 2.0(4) . . . . ?
C31 C34 C33 N33 -175.9(2) . . . . ?
C33 N32 C32 N31 -2.8(4) . . . . ?
C33 N32 C32 N36 179.4(2) . . . . ?
C33 N33 C35 N34 -0.4(4) . . . . ?
C33 C34 C31 N31 -3.8(4) . . . . ?
C33 C34 C31 N35 176.6(2) . . . . ?
C21 N21 C22 N22 -2.2(4) . . . . ?
C21 N21 C22 N26 -179.7(2) . . . . ?
C21 C24 C23 N22 -1.9(4) . . . . ?
C21 C24 C23 N23 176.6(2) . . . . ?
C11 N11 C12 N16 -179.3(2) . . . . ?
C11 N11 C12 N12 -2.1(4) . . . . ?
C11 C14 C13 N12 -2.4(4) . . . . ?
C11 C14 C13 N13 175.4(2) . . . . ?
C32 N31 C31 N35 -177.9(2) . . . . ?
C32 N31 C31 C34 2.5(4) . . . . ?
C32 N32 C33 N33 178.6(3) . . . . ?
C32 N32 C33 C34 1.2(4) . . . . ?
C22 N21 C21 N25 178.3(2) . . . . ?
C22 N21 C21 C24 -1.7(4) . . . . ?
C22 N22 C23 N23 -179.6(3) . . . . ?
C22 N22 C23 C24 -1.5(4) . . . . ?
C14 N14 C15 N13 -0.5(3) . . . . ?
C12 N11 C11 N15 177.8(2) . . . . ?
C12 N11 C11 C14 -1.9(4) . . . . ?
C12 N12 C13 N13 -178.4(3) . . . . ?
C12 N12 C13 C14 -1.1(4) . . . . ?
C24 N24 C25 N23 -0.4(3) . . . . ?
C13 N12 C12 N11 3.5(4) . . . . ?
C13 N12 C12 N16 -179.4(2) . . . . ?
C13 N13 C15 N14 0.5(4) . . . . ?
C23 N22 C22 N21 3.7(4) . . . . ?
C23 N22 C22 N26 -178.8(2) . . . . ?
C23 N23 C25 N24 0.3(4) . . . . ?
C35 N34 C34 C31 174.9(3) . . . . ?
C35 N34 C34 C33 -0.2(3) . . . . ?
C35 N33 C33 N32 -177.6(3) . . . . ?
C35 N33 C33 C34 0.3(3) . . . . ?
C25 N24 C24 C21 -175.7(3) . . . . ?
C25 N24 C24 C23 0.4(3) . . . . ?
C25 N23 C23 N22 178.4(3) . . . . ?
C25 N23 C23 C24 -0.1(3) . . . . ?
C15 N14 C14 C11 -174.2(3) . . . . ?
C15 N14 C14 C13 0.3(3) . . . . ?
C15 N13 C13 N12 177.5(3) . . . . ?
C15 N13 C13 C14 -0.2(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7487(18) 19106 4559 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2513(18) 18590 4559 nmt 0.9958 -0.0133 -0.0026 -0.9838 -0.9523 -0.9847
0.0056 1.0290 0.0108
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.268 0.500 0.500 208.7 53.1 '2 H2O'
