# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_0_2_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262338'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_0_2_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.695 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_0_2_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        270 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         C6H16Cd0.5N3O3
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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   9.7210(7)
_cell_length_b                   9.7210(7)
_cell_length_c                   21.012(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1985.6(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1844
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2920
_cell_measurement_theta_min      4.1510
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.764
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -3 -18 0.1147
13 1 7 0.0497
3 -5 -26 0.1428
-14 -1 -3 0.1012
-8 5 22 0.0738
1 12 -13 0.0197
-1 -12 14 0.0270

_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-10.2698 -3.4297 -18.1515 0.0254 0.9912 -0.1301
13.2844 1.2442 6.7310 -0.0245 -0.9405 -0.3389
3.4930 -5.0637 -26.4638 0.0071 0.3288 -0.9444
-13.6133 -0.5536 -3.1193 0.0233 0.8867 0.4618
-7.6560 5.0094 22.0442 0.0537 -0.0002 0.9986
0.7312 12.2257 -13.3279 0.9954 -0.0255 -0.0924
-1.1416 -11.9122 14.4697 -0.9890 0.0254 0.1459

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.695
_diffrn_reflns_Laue_measured_fraction_max 0.662
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4280
_diffrn_reflns_point_group_measured_fraction_full 0.695
_diffrn_reflns_point_group_measured_fraction_max 0.662
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.303
_diffrn_reflns_theta_min         4.193
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.695
_diffrn_measured_fraction_theta_max 0.662
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.20(2) GPa
 (200000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0013920000
_diffrn_orient_matrix_UB_12      0.0670280000
_diffrn_orient_matrix_UB_13      -0.0132771000
_diffrn_orient_matrix_UB_21      -0.0605118000
_diffrn_orient_matrix_UB_22      -0.0171418000
_diffrn_orient_matrix_UB_23      -0.0171303000
_diffrn_orient_matrix_UB_31      -0.0407911000
_diffrn_orient_matrix_UB_32      0.0231009000
_diffrn_orient_matrix_UB_33      0.0258816000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                398
_reflns_number_total             671
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         671
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0771
_refine_ls_restrained_S_all      1.164
_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)+(0.1045P)²+10.8920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.2479
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Rigid body (RIGU) restrains
 C2, C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, C2, C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2BC,H2BD), C2(H2AA,H2AB), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.0708(9) Uani 1 4 d S T P . .
N1 N 0.8203(14) 0.5957(12) 0.3608(5) 0.084(4) Uani 1 1 d . . . . .
H1A H 0.799505 0.561929 0.398976 0.101 Uiso 1 1 calc R U . . .
H1B H 0.747691 0.644230 0.347994 0.101 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.5252(9) 0.105(8) Uani 1 2 d S T P . .
O1 O 1.0641(15) 0.8342(12) 0.4943(6) 0.124(4) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.5822(9) 0.166(10) Uani 1 2 d S T P . .
C1 C 0.8333(18) 0.4799(17) 0.3179(7) 0.102(5) Uani 1 1 d . . . . .
H1C H 0.917511 0.431248 0.328276 0.122 Uiso 1 1 calc R U . . .
H1D H 0.842890 0.515023 0.274954 0.122 Uiso 1 1 calc R U . . .
C2 C 0.7148(18) 0.3769(17) 0.3188(8) 0.099(5) Uani 1 1 d . . . . .
H2BC H 0.634090 0.419643 0.300233 0.119 Uiso 0.79(4) 1 calc R U P A 2
H2BD H 0.693305 0.353922 0.362580 0.119 Uiso 0.79(4) 1 calc R U P A 2
H2AA H 0.634852 0.421966 0.336834 0.119 Uiso 0.21(4) 1 calc R U P A 1
H2AB H 0.739575 0.301953 0.347038 0.119 Uiso 0.21(4) 1 calc R U P A 1
C3B C 0.748(3) 0.241(2) 0.2813(9) 0.104(10) Uani 0.79(4) 1 d . . P A 2
H3BA H 0.835653 0.204816 0.295604 0.125 Uiso 0.79(4) 1 calc R U P A 2
H3BB H 0.677959 0.172492 0.291114 0.125 Uiso 0.79(4) 1 calc R U P A 2
C3A C 0.674(5) 0.316(5) 0.255(3) 0.056(17) Uani 0.21(4) 1 d . . P A 1
H3AA H 0.585368 0.270690 0.256810 0.067 Uiso 0.21(4) 1 calc R U P A 1
H3AB H 0.673699 0.384638 0.221482 0.067 Uiso 0.21(4) 1 calc R U 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
Cd1 N1 2.322(13) . ?
Cd1 N1 2.322(13) 10_676 ?
Cd1 N1 2.322(13) 12_756 ?
Cd1 N1 2.322(13) 3_765 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.448(18) . ?
N2 O1 1.216(14) 3_765 ?
N2 O1 1.216(14) . ?
N2 O2 1.20(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.53(2) . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 C3B 1.57(3) . ?
C2 C3A 1.52(6) . ?
C3B C3B 1.33(4) 13_655 ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3A C3A 1.97(10) 13_655 ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?

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 Cd1 N1 165.2(6) . 3_765 ?
N1 Cd1 N1 165.2(6) 10_676 12_756 ?
N1 Cd1 N1 90.95(7) . 12_756 ?
N1 Cd1 N1 90.95(7) . 10_676 ?
N1 Cd1 N1 90.95(7) 3_765 10_676 ?
N1 Cd1 N1 90.95(7) 3_765 12_756 ?
Cd1 N1 H1A 107.1 . . ?
Cd1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C1 N1 Cd1 121.1(10) . . ?
C1 N1 H1A 107.1 . . ?
C1 N1 H1B 107.1 . . ?
O1 N2 O1 115(2) 3_765 . ?
O2 N2 O1 122.3(11) . . ?
O2 N2 O1 122.3(11) . 3_765 ?
N1 C1 H1C 108.3 . . ?
N1 C1 H1D 108.3 . . ?
N1 C1 C2 115.9(14) . . ?
H1C C1 H1D 107.4 . . ?
C2 C1 H1C 108.3 . . ?
C2 C1 H1D 108.3 . . ?
C1 C2 H2BC 108.9 . . ?
C1 C2 H2BD 108.9 . . ?
C1 C2 H2AA 108.2 . . ?
C1 C2 H2AB 108.2 . . ?
C1 C2 C3B 113.2(14) . . ?
C1 C2 C3A 116(2) . . ?
H2BC C2 H2BD 107.8 . . ?
H2AA C2 H2AB 107.4 . . ?
C3B C2 H2BC 108.9 . . ?
C3B C2 H2BD 108.9 . . ?
C3A C2 H2AA 108.2 . . ?
C3A C2 H2AB 108.2 . . ?
C2 C3B H3BA 109.1 . . ?
C2 C3B H3BB 109.1 . . ?
C3B C3B C2 113(3) 13_655 . ?
C3B C3B H3BA 109.1 13_655 . ?
C3B C3B H3BB 109.1 13_655 . ?
H3BA C3B H3BB 107.8 . . ?
C2 C3A H3AA 112.0 . . ?
C2 C3A H3AB 112.0 . . ?
C3A C3A C2 99(4) 13_655 . ?
C3A C3A H3AA 112.0 13_655 . ?
C3A C3A H3AB 112.0 13_655 . ?
H3AA C3A H3AB 109.7 . . ?

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
Cd1 N1 C1 C2 173.0(10) . . . . ?
N1 C1 C2 C3B -169.1(17) . . . . ?
N1 C1 C2 C3A 142(3) . . . . ?
C1 C2 C3B C3B -71(3) . . . 13_655 ?
C1 C2 C3A C3A 77(4) . . . 13_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   238
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.647
_oxdiff_exptl_absorpt_empirical_full_min 0.520
####################################################################### 
# 
# 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_0_5_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262339'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_0_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.628 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_0_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        304 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C5.99 H15.98 Cd0.50 N3 O3'
_chemical_formula_weight         234.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'CdC6 N2 H16 N2 O6'
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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   9.6225(8)
_cell_length_b                   9.6225(8)
_cell_length_c                   20.790(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1925.0(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1713
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0940
_cell_measurement_theta_min      3.5390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             967
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -6 -26 0.0309
6 -2 26 0.0716
-8 -10 8 0.0197
-6 1 -26 0.1896
8 10 -8 0.0246
-2 6 26 0.0414

_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.3592 -5.9312 -26.2116 -0.1292 0.6888 -0.7134
5.7046 -1.5355 26.4146 0.0929 0.0136 0.9956
-8.2888 -9.9968 8.4066 0.9834 0.1813 -0.0084
-5.8704 1.3477 -26.2930 -0.0743 -0.0102 -0.9972
8.2888 9.9968 -8.4066 -0.9834 -0.1813 0.0084
-1.9848 5.9933 25.9463 0.1561 -0.7131 0.6831

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.628
_diffrn_reflns_Laue_measured_fraction_max 0.588
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            2434
_diffrn_reflns_point_group_measured_fraction_full 0.628
_diffrn_reflns_point_group_measured_fraction_max 0.588
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.425
_diffrn_reflns_theta_min         3.579
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.628
_diffrn_measured_fraction_theta_max 0.588
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.50(2) GPa
 (500000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   32.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   32.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   32.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   32.00   0.00  30.00   0.00    --    73
  5  ω      4.40  23.90   0.75   32.00    --   30.00  39.46 -16.00   26
  6  ω      4.40  23.90   0.75   32.00    --   30.00  39.46 164.00   26
  7  ω    -50.00  10.00   0.75   32.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   32.00    --  -30.00  39.46 -12.90   80
  9  ω    -63.00  -8.25   0.75   32.00    --  -30.00  81.40 -33.00   73
 10  ω    -63.00 -37.50   0.75   32.00    --  -30.00  81.40 147.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525308000
_diffrn_orient_matrix_UB_12      -0.0444933000
_diffrn_orient_matrix_UB_13      0.0122746000
_diffrn_orient_matrix_UB_21      0.0377166000
_diffrn_orient_matrix_UB_22      -0.0586928000
_diffrn_orient_matrix_UB_23      -0.0110408000
_diffrn_orient_matrix_UB_31      0.0354448000
_diffrn_orient_matrix_UB_32      -0.0034548000
_diffrn_orient_matrix_UB_33      0.0298350000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                459
_reflns_number_total             586
_reflns_odcompleteness_completeness 58.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.040
_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)+(0.0337P)²+0.1185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0693
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2AA,H2AB), C2(H2BC,H2BD), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.0464(3) Uani 1 4 d S T P . .
N1 N 0.8161(4) 0.5960(4) 0.36097(17) 0.0559(10) Uani 1 1 d . . . . .
H1A H 0.795681 0.561202 0.399484 0.067 Uiso 1 1 calc R U . . .
H1B H 0.742926 0.645887 0.348561 0.067 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.5258(3) 0.0645(16) Uani 1 2 d S T P . .
O1 O 1.0692(4) 0.8356(4) 0.49488(18) 0.0902(12) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.5840(3) 0.134(3) Uani 1 2 d S T P . .
C1 C 0.8279(5) 0.4801(5) 0.3170(2) 0.0701(15) Uani 1 1 d . . . . .
H1C H 0.913916 0.431219 0.325985 0.084 Uiso 1 1 calc R U . . .
H1D H 0.833692 0.515877 0.273498 0.084 Uiso 1 1 calc R U . . .
C2 C 0.7095(6) 0.3777(6) 0.3204(2) 0.0746(16) Uani 1 1 d . . . . .
H2AA H 0.625021 0.428324 0.330423 0.090 Uiso 0.40(4) 1 calc R U P A 1
H2AB H 0.727024 0.314261 0.355769 0.090 Uiso 0.40(4) 1 calc R U P A 1
H2BC H 0.626840 0.419475 0.301986 0.090 Uiso 0.60(4) 1 calc R U P A 2
H2BD H 0.689963 0.356250 0.365115 0.090 Uiso 0.60(4) 1 calc R U P A 2
C3B C 0.744(2) 0.2414(16) 0.2839(9) 0.062(5) Uani 0.60(4) 1 d . . P A 2
H3BA H 0.829864 0.203710 0.300529 0.074 Uiso 0.60(4) 1 calc R U P A 2
H3BB H 0.670781 0.174090 0.292424 0.074 Uiso 0.60(4) 1 calc R U P A 2
C3A C 0.683(4) 0.288(2) 0.2566(17) 0.085(9) Uani 0.40(4) 1 d . . P A 1
H3AA H 0.607775 0.222315 0.263218 0.102 Uiso 0.40(4) 1 calc R U P A 1
H3AB H 0.659264 0.347930 0.220774 0.102 Uiso 0.40(4) 1 calc R U 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
Cd1 N1 2.326(4) 3_765 ?
Cd1 N1 2.326(4) 10_676 ?
Cd1 N1 2.326(4) . ?
Cd1 N1 2.326(4) 12_756 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.447(6) . ?
N2 O1 1.239(4) 3_765 ?
N2 O1 1.239(4) . ?
N2 O2 1.209(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.508(6) . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 C3B 1.551(16) . ?
C2 C3A 1.60(3) . ?
C3B C3B 1.42(4) 13_655 ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3A C3A 1.51(7) 13_655 ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?

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 Cd1 N1 90.90(2) 3_765 12_756 ?
N1 Cd1 N1 90.90(2) 10_676 . ?
N1 Cd1 N1 165.59(17) 3_765 . ?
N1 Cd1 N1 90.90(2) 3_765 10_676 ?
N1 Cd1 N1 165.59(17) 12_756 10_676 ?
N1 Cd1 N1 90.90(2) 12_756 . ?
Cd1 N1 H1A 107.1 . . ?
Cd1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C1 N1 Cd1 120.7(3) . . ?
C1 N1 H1A 107.1 . . ?
C1 N1 H1B 107.1 . . ?
O1 N2 O1 117.5(6) 3_765 . ?
O2 N2 O1 121.3(3) . . ?
O2 N2 O1 121.3(3) . 3_765 ?
N1 C1 H1C 108.6 . . ?
N1 C1 H1D 108.6 . . ?
N1 C1 C2 114.5(4) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.6 . . ?
C2 C1 H1D 108.6 . . ?
C1 C2 H2AA 108.4 . . ?
C1 C2 H2AB 108.4 . . ?
C1 C2 H2BC 109.3 . . ?
C1 C2 H2BD 109.3 . . ?
C1 C2 C3B 111.7(7) . . ?
C1 C2 C3A 115.7(11) . . ?
H2AA C2 H2AB 107.4 . . ?
H2BC C2 H2BD 107.9 . . ?
C3B C2 H2BC 109.3 . . ?
C3B C2 H2BD 109.3 . . ?
C3A C2 H2AA 108.4 . . ?
C3A C2 H2AB 108.4 . . ?
C2 C3B H3BA 108.8 . . ?
C2 C3B H3BB 108.8 . . ?
C3B C3B C2 114(2) 13_655 . ?
C3B C3B H3BA 108.8 13_655 . ?
C3B C3B H3BB 108.8 13_655 . ?
H3BA C3B H3BB 107.7 . . ?
C2 C3A H3AA 110.5 . . ?
C2 C3A H3AB 110.5 . . ?
C3A C3A C2 106(3) 13_655 . ?
C3A C3A H3AA 110.5 13_655 . ?
C3A C3A H3AB 110.5 13_655 . ?
H3AA C3A H3AB 108.7 . . ?

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
Cd1 N1 C1 C2 171.2(4) . . . . ?
N1 C1 C2 C3B -167.4(10) . . . . ?
N1 C1 C2 C3A 155.5(15) . . . . ?
C1 C2 C3B C3B -67(2) . . . 13_655 ?
C1 C2 C3A C3A 58(3) . . . 13_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1283
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.633
_oxdiff_exptl_absorpt_empirical_full_min 0.574
####################################################################### 
# 
# 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_0_85_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262340'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form
_audit_creation_date             2023-05-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C5.93 H15.73 Cd0.50 N3 O3'
_chemical_formula_weight         233.32
_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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   9.5693(6)
_cell_length_b                   9.5693(6)
_cell_length_c                   20.504(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1877.5(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    184
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.8160
_cell_measurement_theta_min      3.8420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             963
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.640
_diffrn_reflns_Laue_measured_fraction_max 0.499
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3228
_diffrn_reflns_point_group_measured_fraction_full 0.640
_diffrn_reflns_point_group_measured_fraction_max 0.499
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         3.608
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.640
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       
;
Data were collected at room temperature and pressure of 0.85(2) GPa
 (850000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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                460
_reflns_number_total             687
_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       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         687
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0669
_refine_ls_restrained_S_all      1.162
_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)+(0.0036P)²+45.0774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1731
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C3A) = Uanis(C3B)
2. Others
 Sof(H2AA)=Sof(H2AB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2BC)=Sof(H2BD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2BC,H2BD), C2(H2AA,H2AB), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.0531(6) Uani 1 4 d S T P . .
N1 N 0.8142(10) 0.5989(11) 0.3601(5) 0.063(3) Uani 1 1 d . . . . .
H1A H 0.790330 0.566775 0.399313 0.076 Uiso 1 1 calc R U . . .
H1B H 0.742559 0.649706 0.345808 0.076 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.5260(9) 0.067(4) Uani 1 2 d S T P . .
O1 O 1.0684(12) 0.8363(12) 0.4966(5) 0.097(4) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.5855(8) 0.124(7) Uani 1 2 d S T P . .
C1 C 0.8265(15) 0.4794(14) 0.3174(7) 0.078(4) Uani 1 1 d . . . . .
H1C H 0.912162 0.430061 0.327869 0.094 Uiso 1 1 calc R U . . .
H1D H 0.834361 0.512450 0.272808 0.094 Uiso 1 1 calc R U . . .
C2 C 0.7101(16) 0.3813(17) 0.3212(8) 0.087(5) Uani 1 1 d . . . . .
H2BC H 0.628606 0.419200 0.299381 0.104 Uiso 0.45(3) 1 calc R U P A 2
H2BD H 0.686249 0.362852 0.366378 0.104 Uiso 0.45(3) 1 calc R U P A 2
H2AA H 0.624543 0.434582 0.326007 0.104 Uiso 0.55(3) 1 calc R U P A 1
H2AB H 0.721454 0.325839 0.360469 0.104 Uiso 0.55(3) 1 calc R U P A 1
C3B C 0.760(3) 0.241(3) 0.2861(19) 0.070(6) Uani 0.55(3) 1 d . . P A 2
H3BA H 0.857975 0.223549 0.295668 0.084 Uiso 0.55(3) 1 calc R U P A 2
H3BB H 0.705917 0.162253 0.301739 0.084 Uiso 0.55(3) 1 calc R U P A 2
C3A C 0.692(4) 0.283(4) 0.265(2) 0.070(6) Uani 0.45(3) 1 d . . P A 1
H3AA H 0.629052 0.210404 0.279019 0.084 Uiso 0.45(3) 1 calc R U P A 1
H3AB H 0.644488 0.335105 0.230833 0.084 Uiso 0.45(3) 1 calc R U 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
Cd1 N1 2.312(10) 3_765 ?
Cd1 N1 2.312(10) 12_756 ?
Cd1 N1 2.312(10) 10_676 ?
Cd1 N1 2.312(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.446(15) . ?
N2 O1 1.214(11) . ?
N2 O1 1.214(11) 3_765 ?
N2 O2 1.220(19) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.459(18) . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 C3B 1.60(3) . ?
C2 C3A 1.50(4) . ?
C3B C3B 1.50(8) 13_655 ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3A C3A 1.41(9) 13_655 ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?

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 Cd1 N1 91.00(7) 3_765 12_756 ?
N1 Cd1 N1 90.99(7) 10_676 . ?
N1 Cd1 N1 91.00(7) 3_765 10_676 ?
N1 Cd1 N1 91.00(7) 12_756 . ?
N1 Cd1 N1 164.8(5) 3_765 . ?
N1 Cd1 N1 164.8(5) 12_756 10_676 ?
Cd1 N1 H1A 107.1 . . ?
Cd1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C1 N1 Cd1 120.8(8) . . ?
C1 N1 H1A 107.1 . . ?
C1 N1 H1B 107.1 . . ?
O1 N2 O1 120.5(19) 3_765 . ?
O1 N2 O2 119.8(10) . . ?
O1 N2 O2 119.8(10) 3_765 . ?
N1 C1 H1C 108.6 . . ?
N1 C1 H1D 108.6 . . ?
N1 C1 C2 114.5(13) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.6 . . ?
C2 C1 H1D 108.6 . . ?
C1 C2 H2BC 110.4 . . ?
C1 C2 H2BD 110.4 . . ?
C1 C2 H2AA 108.1 . . ?
C1 C2 H2AB 108.1 . . ?
C1 C2 C3B 106.7(16) . . ?
C1 C2 C3A 116.6(19) . . ?
H2BC C2 H2BD 108.6 . . ?
H2AA C2 H2AB 107.3 . . ?
C3B C2 H2BC 110.4 . . ?
C3B C2 H2BD 110.4 . . ?
C3A C2 H2AA 108.1 . . ?
C3A C2 H2AB 108.1 . . ?
C2 C3B H3BA 110.1 . . ?
C2 C3B H3BB 110.1 . . ?
C3B C3B C2 108(3) 13_655 . ?
C3B C3B H3BA 110.1 13_655 . ?
C3B C3B H3BB 110.1 13_655 . ?
H3BA C3B H3BB 108.4 . . ?
C2 C3A H3AA 106.9 . . ?
C2 C3A H3AB 106.9 . . ?
C3A C3A C2 122(3) 13_655 . ?
C3A C3A H3AA 106.9 13_655 . ?
C3A C3A H3AB 106.9 13_655 . ?
H3AA C3A H3AB 106.7 . . ?

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
Cd1 N1 C1 C2 170.2(11) . . . . ?
N1 C1 C2 C3B -165.4(17) . . . . ?
N1 C1 C2 C3A 161(2) . . . . ?
C1 C2 C3B C3B -83(3) . . . 13_655 ?
C1 C2 C3A C3A 42(6) . . . 13_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT029_0_85_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.640 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_0_85_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        307 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
####################################################################### 
# 
# 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_1_1_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262341'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.356 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.77 Note
RESPONSE: The data/parameter ratio is affected by the access limits of 
the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT084_1_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT342_1_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.07167 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_1_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2084 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2022-08-04
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H24 Cd N6 O6'
_chemical_formula_sum            'C12 H24 Cd N6 O6'
_chemical_formula_weight         460.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12 N6 O6 H32'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.350(2)
_cell_length_b                   9.7253(18)
_cell_length_c                   11.181(5)
_cell_angle_alpha                110.90(3)
_cell_angle_beta                 105.07(3)
_cell_angle_gamma                95.909(17)
_cell_volume                     895.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7140
_cell_measurement_theta_min      2.2730
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.045
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             468
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 9 0.0485
2 13 -4 0.0555
9 -9 -4 0.0737
8 10 -7 0.0399
-10 -7 9 0.0309
10 7 -9 0.0309
-1 -13 3 0.0820

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.3945 -2.1635 8.5440 -0.0181 0.8138 -0.5809
2.1742 12.9992 -4.0976 0.0208 -0.8368 -0.5471
9.1583 -9.4991 -4.0280 -0.0022 0.0091 1.0000
8.4042 9.6062 -7.4434 0.0254 -0.9994 -0.0254
-10.1655 -7.4584 8.5362 0.0012 0.9811 -0.1932
10.1655 7.4584 -8.5362 -0.0012 -0.9811 0.1932
-0.7895 -13.2003 2.9057 -0.0414 0.7692 0.6431

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1353
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.356
_diffrn_reflns_Laue_measured_fraction_max 0.218
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5566
_diffrn_reflns_point_group_measured_fraction_full 0.356
_diffrn_reflns_point_group_measured_fraction_max 0.218
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.021
_diffrn_reflns_theta_min         2.296
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.356
_diffrn_measured_fraction_theta_max 0.218
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.10(2) GPa
 (1100000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  15.00   0.75   12.50    --  -24.60 -77.00-150.00   36
  2  ω   -109.00 -73.00   0.75   12.50    --  -24.60 178.00  90.00   48
  3  ω    -14.00  22.00   0.75   12.50    --  -24.60 -38.00-180.00   48
  4  ω    -30.00  45.00   0.75   12.50    --  -24.60 -26.00   8.00  100
  5  ω   -108.00 -72.00   0.75   12.50    --  -24.60-178.00  90.00   48
  6  ω    -59.00  13.00   0.75   12.50    --  -24.60  67.00 157.00   96
  7  ω     -2.00  25.00   0.75   12.50    --  -24.60 -97.00  35.00   36
  8  ω    -59.00  13.00   0.75   12.50    --  -24.60  67.00 -23.00   96
  9  ω    -37.00   6.50   0.75   12.50    --   25.46   0.00-150.00   58
 10  ω    -12.50  55.00   0.75   12.50    --   25.46 -53.00  17.00   90
 11  ω     63.75 108.00   0.75   12.50    --   25.46 178.00 -90.00   59
 12  ω     72.00 108.00   0.75   12.50    --   25.46-178.00  90.00   48
 13  ω     20.00  47.00   0.75   12.50    --  -24.60-135.00-123.00   36
 14  ω    -20.00   8.50   0.75   12.50    --  -24.60 -53.00  17.00   38
 15  ω    -25.00  50.00   0.75   12.50    --  -24.60 -19.00-180.00  100
 16  ω    -14.00  22.00   0.75   12.50    --  -24.60 -38.00-150.00   48
 17  ω    -35.00 -12.50   0.75   12.50    --  -24.60  77.00 -60.00   30
 18  ω     20.00  47.00   0.75   12.50    --  -24.60-135.00  57.00   36
 19  ω     -2.00  25.00   0.75   12.50    --  -24.60 -97.00-143.00   36
 20  ω     34.00  61.00   0.75   12.50    --   25.46 -99.00  30.00   36
 21  ω    -21.00  24.00   0.75   12.50    --   25.46  39.00 -12.00   60
 22  ω     34.00  67.00   0.75   12.50    --   25.46 -99.00-150.00   44
 23  ω    -25.00  21.50   0.75   12.50    --  -24.60 -39.00  12.00   62
 24  ω    -57.00 -37.50   0.75   12.50    --  -24.60  57.00-150.00   26
 25  ω    -35.00 -12.50   0.75   12.50    --  -24.60  77.00 150.00   30
 26  ω     12.00  34.50   0.75   12.50    --   25.46 -77.00  30.00   30
 27  ω    -17.50  38.75   0.75   12.50    --   25.46 -39.00-167.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449418000
_diffrn_orient_matrix_UB_12      0.0151795000
_diffrn_orient_matrix_UB_13      0.0669206000
_diffrn_orient_matrix_UB_21      -0.0540286000
_diffrn_orient_matrix_UB_22      -0.0543599000
_diffrn_orient_matrix_UB_23      0.0031027000
_diffrn_orient_matrix_UB_31      0.0392201000
_diffrn_orient_matrix_UB_32      -0.0566667000
_diffrn_orient_matrix_UB_33      -0.0254436000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                579
_reflns_number_total             852
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.675
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         852
_refine_ls_number_restraints     400
_refine_ls_R_factor_all          0.1691
_refine_ls_R_factor_gt           0.1154
_refine_ls_restrained_S_all      1.387
_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          0.3078
_refine_ls_wR_factor_ref         0.3855
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 H6B_$4-H10B
 2.1 with sigma of 0.02
 C2-C1 \\sim C3-C2 \\sim C3-C3_$1 \\sim C12-C11 \\sim C11-C10 \\sim C12-C12_$2
\\sim C12-C11 \\sim C11-C10
 \\sim C8-C7 \\sim C9-C8 \\sim C9-C9_$3 \\sim C9-C8 \\sim C8-C7
 with sigma of 0.02
 N3-C7 \\sim N1-C1 \\sim N4-C10 \\sim N2-C4
 with sigma of 0.02
 O2-N5 \\sim O3-N5 \\sim O1-N5 \\sim O6-N6 \\sim O4-N6 \\sim O5-N6
 with sigma of 0.02
 O6-O4 \\sim O5-O4 \\sim O5-O6 \\sim O3-O2 \\sim O2-O1 \\sim O3-O1
 with sigma of 0.02
3. Rigid bond restraints
 O6, N6, O5, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, N6, O5, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, N3, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C8, C7, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O6 \\sim N6 \\sim O4 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O4 \\sim N6 \\sim O5 \\sim O6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C12 \\sim C11 \\sim C10 \\sim N4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O6) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O6, N6, O5, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O1, O3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C1(H1A,H1B), C4(H4A,H4B), C7(H7A,H7B),
 C12(H12A,H12B), C2(H2A,H2B), C5(H5A,H5B), C8(H8A,H8B), C3(H3A,H3B), C6(H6A,
 H6B), C9(H9A,H9B)
;
_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
N2 N 0.689(6) 0.740(3) 0.221(8) 0.037(7) Uani 1 1 d D U . . .
N4 N 0.765(5) 0.480(3) 0.366(7) 0.049(9) Uani 1 1 d D U . . .
Cd1 Cd 0.8691(6) 0.5971(3) 0.2454(9) 0.056(5) Uani 1 1 d . U . . .
C10 C 0.606(5) 0.385(3) 0.277(6) 0.045(9) Uani 1 1 d D U . . .
H10A H 0.541853 0.448867 0.250688 0.054 Uiso 1 1 calc R U . . .
H10B H 0.610994 0.307312 0.196360 0.054 Uiso 1 1 calc DR U . . .
N1 N 1.049(5) 0.451(3) 0.255(8) 0.026(7) Uani 1 1 d D U . . .
O1 O 0.661(4) 0.410(3) 0.025(5) 0.071(8) Uani 1 1 d D U . . .
O2 O 0.861(3) 0.536(3) -0.003(5) 0.069(8) Uani 1 1 d D U . . .
N3 N 1.041(5) 0.793(3) 0.257(7) 0.026(5) Uani 1 1 d D U . . .
C11 C 0.540(6) 0.316(4) 0.355(7) 0.042(11) Uani 1 1 d D U . . .
H11A H 0.603419 0.250958 0.378520 0.050 Uiso 1 1 calc R U . . .
H11B H 0.440280 0.254635 0.297999 0.050 Uiso 1 1 calc R U . . .
C1 C 0.986(5) 0.282(3) 0.166(8) 0.030(7) Uani 1 1 d D U . . .
H1A H 0.917852 0.242056 0.203343 0.036 Uiso 1 1 calc R U . . .
H1B H 0.927262 0.271318 0.076613 0.036 Uiso 1 1 calc R U . . .
N5 N 0.724(4) 0.444(4) -0.056(5) 0.061(9) Uani 1 1 d D U . . .
C4 C 0.675(6) 0.791(3) 0.104(8) 0.034(7) Uani 1 1 d D U . . .
H4A H 0.773636 0.836479 0.106645 0.040 Uiso 1 1 calc R U . . .
H4B H 0.628168 0.706218 0.017625 0.040 Uiso 1 1 calc R U . . .
C7 C 1.203(5) 0.830(3) 0.352(7) 0.028(6) Uani 1 1 d D U . . .
H7A H 1.200972 0.878566 0.443194 0.034 Uiso 1 1 calc R U . . .
H7B H 1.232388 0.734839 0.343379 0.034 Uiso 1 1 calc R U . . .
C12 C 0.528(7) 0.430(3) 0.479(8) 0.059(10) Uani 1 1 d D U . . .
H12A H 0.473739 0.368832 0.512323 0.071 Uiso 1 1 calc R U . . .
H12B H 0.631416 0.460937 0.539889 0.071 Uiso 1 1 calc R U . . .
C2 C 1.100(6) 0.188(3) 0.151(9) 0.045(8) Uani 1 1 d D U . . .
H2A H 1.162662 0.203769 0.240549 0.054 Uiso 1 1 calc R U . . .
H2B H 1.164826 0.225028 0.108955 0.054 Uiso 1 1 calc R U . . .
O3 O 0.641(4) 0.424(3) -0.180(5) 0.070(7) Uani 1 1 d D U . . .
C5 C 0.582(8) 0.898(4) 0.122(12) 0.044(7) Uani 1 1 d . U . . .
H5A H 0.625847 0.979066 0.211575 0.053 Uiso 1 1 calc R U . . .
H5B H 0.481876 0.850682 0.115383 0.053 Uiso 1 1 calc R U . . .
C8 C 1.326(3) 0.924(3) 0.337(6) 0.032(7) Uani 1 1 d D U . . .
H8A H 1.298915 1.020762 0.348995 0.038 Uiso 1 1 calc R U . . .
H8B H 1.326362 0.877497 0.245002 0.038 Uiso 1 1 calc R U . . .
C3 C 1.043(4) 0.025(4) 0.0723(16) 0.042(8) Uani 1 1 d D U . . .
H3A H 0.977690 -0.011865 0.114252 0.051 Uiso 1 1 calc R U . . .
H3B H 1.128581 -0.023071 0.079473 0.051 Uiso 1 1 calc R U . . .
C6 C 0.568(5) 0.966(3) 0.011(8) 0.037(7) Uani 1 1 d . U . . .
H6A H 0.658475 1.041653 0.037227 0.045 Uiso 1 1 calc R U . . .
H6B H 0.561198 0.885730 -0.074019 0.045 Uiso 1 1 calc R U . . .
C9 C 1.483(3) 0.954(3) 0.4273(17) 0.036(7) Uani 1 1 d D U . . .
H9A H 1.508554 0.857620 0.418027 0.043 Uiso 1 1 calc R U . . .
H9B H 1.549337 1.003381 0.394290 0.043 Uiso 1 1 calc R U . . .
N6 N 0.990(4) 0.801(2) 0.541(6) 0.050(6) Uani 1 1 d D U . . .
O5 O 0.859(5) 0.829(3) 0.484(6) 0.079(9) Uani 1 1 d D U . . .
O4 O 1.020(4) 0.667(2) 0.485(6) 0.037(6) Uani 1 1 d D U . . .
O6 O 1.093(4) 0.911(3) 0.646(6) 0.057(7) Uani 1 1 d D U . . .


_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 Cd1 2.31(4) . ?
N2 C4 1.54(4) . ?
N4 Cd1 2.37(5) . ?
N4 C10 1.53(4) . ?
Cd1 N1 2.32(4) . ?
Cd1 O1 2.60(5) . ?
Cd1 O2 2.61(5) . ?
Cd1 N3 2.30(2) . ?
Cd1 O4 2.48(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.47(3) . ?
N1 C1 1.54(4) . ?
O1 N5 1.32(2) . ?
O2 N5 1.33(2) . ?
N3 C7 1.53(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.48(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.47(3) . ?
N5 O3 1.33(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.42(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.47(3) . ?
C12 C12 1.47(3) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.47(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.59(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.48(3) . ?
C3 C3 1.47(3) 2_755 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C6 C6 1.49(10) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.47(3) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N6 O5 1.33(2) . ?
N6 O4 1.33(2) . ?
N6 O6 1.33(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
C4 N2 Cd1 115.0(19) . . ?
C10 N4 Cd1 109(4) . . ?
N2 Cd1 N4 96.7(14) . . ?
N2 Cd1 N1 176(2) . . ?
N2 Cd1 O1 78.5(17) . . ?
N2 Cd1 O2 89.4(18) . . ?
N2 Cd1 O4 113.0(18) . . ?
N4 Cd1 O1 88.6(18) . . ?
N4 Cd1 O2 137.9(15) . . ?
N4 Cd1 O4 63.4(17) . . ?
N1 Cd1 N4 86.4(15) . . ?
N1 Cd1 O1 99.1(17) . . ?
N1 Cd1 O2 86.7(19) . . ?
N1 Cd1 O4 70.6(18) . . ?
O1 Cd1 O2 51.9(11) . . ?
N3 Cd1 N2 86.7(11) . . ?
N3 Cd1 N4 147(2) . . ?
N3 Cd1 N1 92.1(10) . . ?
N3 Cd1 O1 124(2) . . ?
N3 Cd1 O2 74.8(18) . . ?
N3 Cd1 O4 84.9(19) . . ?
O4 Cd1 O1 150.1(9) . . ?
O4 Cd1 O2 149.0(9) . . ?
N4 C10 H10A 109.9 . . ?
N4 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 N4 109(3) . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C1 N1 Cd1 114(3) . . ?
N5 O1 Cd1 95.0(15) . . ?
N5 O2 Cd1 94.1(14) . . ?
C7 N3 Cd1 119(2) . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
C10 C11 C12 112(3) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
N1 C1 H1A 108.3 . . ?
N1 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
C2 C1 N1 116(4) . . ?
C2 C1 H1A 108.3 . . ?
C2 C1 H1B 108.3 . . ?
O1 N5 O2 118.6(16) . . ?
O1 N5 O3 120.7(16) . . ?
O3 N5 O2 118.3(16) . . ?
N2 C4 H4A 110.6 . . ?
N2 C4 H4B 110.6 . . ?
H4A C4 H4B 108.8 . . ?
C5 C4 N2 106(5) . . ?
C5 C4 H4A 110.6 . . ?
C5 C4 H4B 110.6 . . ?
N3 C7 H7A 107.2 . . ?
N3 C7 H7B 107.2 . . ?
H7A C7 H7B 106.9 . . ?
C8 C7 N3 120(4) . . ?
C8 C7 H7A 107.2 . . ?
C8 C7 H7B 107.2 . . ?
C11 C12 H12A 102.4 . . ?
C11 C12 H12B 102.4 . . ?
C12 C12 C11 139(8) 2_666 . ?
C12 C12 H12A 102.4 2_666 . ?
C12 C12 H12B 102.4 2_666 . ?
H12A C12 H12B 104.9 . . ?
C1 C2 H2A 108.0 . . ?
C1 C2 H2B 108.0 . . ?
C1 C2 C3 117(4) . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 H2A 108.0 . . ?
C3 C2 H2B 108.0 . . ?
C4 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
C4 C5 C6 110(5) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
C7 C8 H8A 107.5 . . ?
C7 C8 H8B 107.5 . . ?
C7 C8 C9 119(5) . . ?
H8A C8 H8B 107.0 . . ?
C9 C8 H8A 107.5 . . ?
C9 C8 H8B 107.5 . . ?
C2 C3 C3 117(5) . 2_755 ?
C2 C3 H3A 108.0 . . ?
C2 C3 H3B 108.0 . . ?
C3 C3 H3A 108.0 2_755 . ?
C3 C3 H3B 108.0 2_755 . ?
H3A C3 H3B 107.3 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C6 C6 C5 113(5) 2_675 . ?
C6 C6 H6A 108.9 2_675 . ?
C6 C6 H6B 108.9 2_675 . ?
H6A C6 H6B 107.8 . . ?
C8 C9 H9A 107.7 . . ?
C8 C9 H9B 107.7 . . ?
C9 C9 C8 118(3) 2_876 . ?
C9 C9 H9A 107.7 2_876 . ?
C9 C9 H9B 107.7 2_876 . ?
H9A C9 H9B 107.1 . . ?
O5 N6 O4 119.6(15) . . ?
O5 N6 O6 119.3(14) . . ?
O6 N6 O4 120.8(15) . . ?
N6 O4 Cd1 100(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 177(5) . . . . ?
N4 C10 C11 C12 60(5) . . . . ?
Cd1 N2 C4 C5 -169(5) . . . . ?
Cd1 N4 C10 C11 -178(2) . . . . ?
Cd1 N1 C1 C2 170(5) . . . . ?
Cd1 O1 N5 O2 7(3) . . . . ?
Cd1 O1 N5 O3 -155(4) . . . . ?
Cd1 O2 N5 O1 -7(3) . . . . ?
Cd1 O2 N5 O3 155(4) . . . . ?
Cd1 N3 C7 C8 164(3) . . . . ?
C10 C11 C12 C12 48(9) . . . 2_666 ?
N1 C1 C2 C3 177(5) . . . . ?
N3 C7 C8 C9 -178(2) . . . . ?
C1 C2 C3 C3 64(8) . . . 2_755 ?
C4 C5 C6 C6 159(6) . . . 2_675 ?
C7 C8 C9 C9 -67(5) . . . 2_876 ?
O5 N6 O4 Cd1 28(3) . . . . ?
O6 N6 O4 Cd1 -146(3) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.900
_oxdiff_exptl_absorpt_empirical_full_min 0.594
####################################################################### 
# 
# 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_1_65_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262345'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT027_1_65_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_vrf_PLAT029_1_65_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.358 Why?
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_vrf_PLAT088_1_65_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.88 Note
RESPONSE: The data/parameter ratio is affected by the access limits 
of the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_1_65_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.07667 Ang.
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_vrf_PLAT911_1_65_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1958 Report
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N5 O3, N O3'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12 H32 N6 O6'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.340(3)
_cell_length_b                   9.701(4)
_cell_length_c                   11.109(4)
_cell_angle_alpha                111.06(4)
_cell_angle_beta                 105.20(3)
_cell_angle_gamma                95.86(3)
_cell_volume                     884.6(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2004
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5130
_cell_measurement_theta_min      2.3100
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.044
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 8 0 0.0485
-3 -11 13 0.0555
-5 3 -12 0.0737
-6 -11 8 0.0399
7 11 -6 0.0309
-7 -11 6 0.0309
2 10 -14 0.0820

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.9935 7.7437 0.3428 -0.0181 0.8138 -0.5809
-2.6321 -10.7087 13.4096 0.0208 -0.8368 -0.5471
-4.8247 2.5007 -12.0987 -0.0022 0.0091 1.0000
-6.2281 -11.2695 8.4730 0.0254 -0.9994 -0.0254
6.9074 10.7250 -5.5400 0.0012 0.9812 -0.1932
-6.9074 -10.7250 5.5400 -0.0012 -0.9812 0.1932
1.9681 10.0226 -14.1460 -0.0414 0.7692 0.6431

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1620
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.358
_diffrn_reflns_Laue_measured_fraction_max 0.200
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6284
_diffrn_reflns_point_group_measured_fraction_full 0.358
_diffrn_reflns_point_group_measured_fraction_max 0.200
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         28.248
_diffrn_reflns_theta_min         2.075
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.358
_diffrn_measured_fraction_theta_max 0.200
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.65(2) GPa
 (1650000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     20.00  47.00   0.75   11.50    --  -24.60-135.00  57.00   36
  2  ω    -30.00  45.00   0.75   11.50    --  -24.60 -26.00   8.00  100
  3  ω    -66.00   9.00   0.75   11.50    --  -24.60  81.00 151.00  100
  4  ω    -20.00   8.50   0.75   11.50    --  -24.60 -53.00  17.00   38
  5  ω   -108.00 -72.00   0.75   11.50    --  -24.60-178.00  90.00   48
  6  ω    -33.00  42.00   0.75   11.50    --  -24.60 -13.00   3.00  100
  7  ω     -2.00  25.00   0.75   11.50    --  -24.60 -97.00  35.00   36
  8  ω    -25.00  21.50   0.75   11.50    --  -24.60 -39.00-167.00   62
  9  ω   -108.00 -72.00   0.75   11.50    --  -24.60-178.00 120.00   48
 10  ω     16.75  82.00   0.75   11.50    --   25.46-114.00-135.00   87
 11  ω    -34.00  36.50   0.75   11.50    --   25.46   0.00-180.00   94
 12  ω     72.00 107.25   0.75   11.50    --   25.46 178.00  90.00   47
 13  ω     -8.00  19.00   0.75   11.50    --   25.46  53.00 -17.00   36
 14  ω    -35.00 -12.50   0.75   11.50    --  -24.60  77.00 120.00   30
 15  ω    -50.00  25.00   0.75   11.50    --  -24.60  19.00-180.00  100
 16  ω      7.00  35.50   0.75   11.50    --  -24.60-114.00-135.00   38
 17  ω    -59.00  13.00   0.75   11.50    --  -24.60  67.00 -23.00   96
 18  ω     -9.00  16.50   0.75   11.50    --  -24.60 -81.00-151.00   34
 19  ω     34.00  61.00   0.75   11.50    --   25.46 -99.00  30.00   36
 20  ω     12.00  34.50   0.75   11.50    --   25.46 -77.00  30.00   30
 21  ω    -21.00  24.00   0.75   11.50    --   25.46  39.00 -12.00   60
 22  ω    -25.00   2.00   0.75   11.50    --   25.46  97.00 -35.00   36
 23  ω     -2.00  47.50   0.75   11.50    --   25.46 -57.00-150.00   66
 24  ω    -25.00   2.00   0.75   11.50    --   25.46  97.00 143.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0474231000
_diffrn_orient_matrix_UB_12      0.0453553000
_diffrn_orient_matrix_UB_13      0.0284639000
_diffrn_orient_matrix_UB_21      0.0406217000
_diffrn_orient_matrix_UB_22      0.0633266000
_diffrn_orient_matrix_UB_23      -0.0038590000
_diffrn_orient_matrix_UB_31      -0.0510262000
_diffrn_orient_matrix_UB_32      -0.0194088000
_diffrn_orient_matrix_UB_33      -0.0663138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                699
_reflns_number_total             877
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         877
_refine_ls_number_restraints     300
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0866
_refine_ls_restrained_S_all      0.910
_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)+(0.1137P)²+18.9294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2348
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C2-C1
 1.45 with sigma of 0.02
 C5-C4
 1.45 with sigma of 0.02
 C3_$1-C3
 1.45 with sigma of 0.02
3. Rigid bond restraints
 O6, N6, O5, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, N3, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O6 \\sim N6 \\sim O4 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C12 \\sim C11 \\sim C10 \\sim N4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O6) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O6, N6, O5, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O1, O3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_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
N2 N 0.685(6) 0.747(6) 0.231(4) 0.047(8) Uani 1 1 d . U . . .
H2A H 0.594405 0.695288 0.219006 0.056 Uiso 1 1 calc R U . . .
H2B H 0.710655 0.831121 0.306141 0.056 Uiso 1 1 calc R U . . .
N4 N 0.759(5) 0.481(5) 0.352(4) 0.06(2) Uani 1 1 d . U . . .
H4A H 0.822909 0.427360 0.378446 0.071 Uiso 1 1 calc R U . . .
H4B H 0.755314 0.552913 0.427113 0.071 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8695(5) 0.5978(4) 0.2477(3) 0.049(6) Uani 1 1 d . . . . .
C10 C 0.609(7) 0.381(7) 0.285(5) 0.053(15) Uani 1 1 d . U . . .
H10A H 0.615056 0.289554 0.213276 0.064 Uiso 1 1 calc R U . . .
H10B H 0.540092 0.430200 0.241757 0.064 Uiso 1 1 calc R U . . .
N1 N 1.045(5) 0.446(5) 0.236(4) 0.06(3) Uani 1 1 d . U . . .
H1A H 1.112237 0.478370 0.202620 0.076 Uiso 1 1 calc R U . . .
H1B H 1.095049 0.456588 0.319745 0.076 Uiso 1 1 calc R U . . .
O1 O 0.662(5) 0.417(5) 0.022(3) 0.09(3) Uani 1 1 d . . . . .
O2 O 0.852(5) 0.535(5) -0.004(3) 0.10(4) Uani 1 1 d . U . . .
N3 N 1.059(5) 0.784(5) 0.271(3) 0.04(3) Uani 1 1 d . U . . .
H3A H 1.070677 0.758382 0.188952 0.048 Uiso 1 1 calc R U . . .
H3B H 1.021709 0.867261 0.286050 0.048 Uiso 1 1 calc R U . . .
C11 C 0.540(8) 0.333(7) 0.386(5) 0.053(11) Uani 1 1 d . U . . .
H11A H 0.434012 0.282086 0.335710 0.064 Uiso 1 1 calc R U . . .
H11B H 0.591831 0.258456 0.405850 0.064 Uiso 1 1 calc R U . . .
C1 C 0.979(6) 0.285(5) 0.151(4) 0.07(2) Uani 1 1 d D U . . .
H1C H 0.903145 0.248875 0.184687 0.086 Uiso 1 1 calc R U . . .
H1D H 0.929024 0.271131 0.058106 0.086 Uiso 1 1 calc R U . . .
N5 N 0.723(6) 0.454(6) -0.051(4) 0.07(3) Uani 1 1 d . . . . .
C4 C 0.682(5) 0.782(5) 0.111(3) 0.044(7) Uani 1 1 d D U . . .
H4C H 0.784020 0.823852 0.116647 0.053 Uiso 1 1 calc R U . . .
H4D H 0.637996 0.692638 0.026859 0.053 Uiso 1 1 calc R U . . .
C7 C 1.208(6) 0.830(6) 0.365(4) 0.05(2) Uani 1 1 d . U . . .
H7A H 1.240031 0.741414 0.374224 0.064 Uiso 1 1 calc R U . . .
H7B H 1.204886 0.896674 0.453264 0.064 Uiso 1 1 calc R U . . .
C12 C 0.543(7) 0.443(7) 0.511(5) 0.050(10) Uani 1 1 d . U . . .
H12A H 0.647903 0.493170 0.566013 0.060 Uiso 1 1 calc R U . . .
H12B H 0.499683 0.394827 0.559917 0.060 Uiso 1 1 calc R U . . .
C2 C 1.097(6) 0.198(5) 0.155(4) 0.07(2) Uani 1 1 d D U . . .
H2C H 1.149611 0.218854 0.249559 0.089 Uiso 1 1 calc R U . . .
H2D H 1.170650 0.235230 0.119926 0.089 Uiso 1 1 calc R U . . .
O3 O 0.652(5) 0.418(5) -0.173(3) 0.07(4) Uani 1 1 d . . . . .
C5 C 0.589(5) 0.893(5) 0.119(4) 0.050(8) Uani 1 1 d D U . . .
H5A H 0.629243 0.972481 0.210281 0.060 Uiso 1 1 calc R U . . .
H5B H 0.487850 0.844459 0.109282 0.060 Uiso 1 1 calc R U . . .
C8 C 1.334(7) 0.917(7) 0.325(5) 0.05(2) Uani 1 1 d . U . . .
H8A H 1.330749 0.854792 0.233217 0.060 Uiso 1 1 calc R U . . .
H8B H 1.308544 1.011276 0.325605 0.060 Uiso 1 1 calc R U . . .
C3 C 1.042(6) 0.020(5) 0.072(3) 0.06(3) Uani 1 1 d D U . . .
H3C H 1.129772 -0.025671 0.078880 0.075 Uiso 1 1 calc R U . . .
H3D H 0.977168 -0.019718 0.112930 0.075 Uiso 1 1 calc R U . . .
C6 C 0.570(6) 0.971(6) 0.016(4) 0.033(8) Uani 1 1 d . U . . .
H6A H 0.656618 1.055262 0.052029 0.039 Uiso 1 1 calc R U . . .
H6B H 0.576135 0.898994 -0.068484 0.039 Uiso 1 1 calc R U . . .
C9 C 1.494(6) 0.949(6) 0.421(4) 0.05(3) Uani 1 1 d . U . . .
H9A H 1.564064 1.002964 0.394060 0.060 Uiso 1 1 calc R U . . .
H9B H 1.522972 0.854478 0.415608 0.060 Uiso 1 1 calc R U . . .
N6 N 1.013(7) 0.808(6) 0.567(4) 0.052(7) Uani 1 1 d . U . . .
O5 O 0.867(7) 0.849(7) 0.533(5) 0.091(10) Uani 1 1 d . U . . .
O4 O 1.035(6) 0.683(6) 0.521(4) 0.065(8) Uani 1 1 d . U . . .
O6 O 1.110(6) 0.918(5) 0.661(4) 0.074(11) Uani 1 1 d . U . . .


_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 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 Cd1 2.37(7) . ?
N2 C4 1.49(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.24(3) . ?
N4 C10 1.46(4) . ?
Cd1 N1 2.31(7) . ?
Cd1 O1 2.589(19) . ?
Cd1 O2 2.60(4) . ?
Cd1 N3 2.292(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.61(7) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.47(5) . ?
O1 N5 1.24(5) . ?
O2 N5 1.24(4) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.41(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.40(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.46(2) . ?
N5 O3 1.24(3) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.45(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.62(6) . ?
C12 C12 1.48(16) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.59(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.56(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.52(6) . ?
C3 C3 1.48(2) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.49(14) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.63(13) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N6 O5 1.45(11) . ?
N6 O4 1.20(10) . ?
N6 O6 1.25(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
H2A N2 H2B 108.7 . . ?
Cd1 N2 H2A 110.5 . . ?
Cd1 N2 H2B 110.5 . . ?
C4 N2 H2A 110.5 . . ?
C4 N2 H2B 110.5 . . ?
C4 N2 Cd1 106(5) . . ?
H4A N4 H4B 106.6 . . ?
Cd1 N4 H4A 106.7 . . ?
Cd1 N4 H4B 106.7 . . ?
C10 N4 H4A 106.7 . . ?
C10 N4 H4B 106.7 . . ?
C10 N4 Cd1 122.4(18) . . ?
N2 Cd1 O1 78.7(17) . . ?
N2 Cd1 O2 90(2) . . ?
N4 Cd1 N2 93.6(19) . . ?
N4 Cd1 N1 91.2(19) . . ?
N4 Cd1 O1 87.1(9) . . ?
N4 Cd1 O2 134.3(10) . . ?
N4 Cd1 N3 146.9(9) . . ?
N1 Cd1 N2 172.8(12) . . ?
N1 Cd1 O1 96.3(17) . . ?
N1 Cd1 O2 82.6(18) . . ?
O1 Cd1 O2 49.1(11) . . ?
N3 Cd1 N2 92.5(15) . . ?
N3 Cd1 N1 86.2(16) . . ?
N3 Cd1 O1 125.9(9) . . ?
N3 Cd1 O2 78.1(9) . . ?
N4 C10 H10A 108.8 . . ?
N4 C10 H10B 108.8 . . ?
N4 C10 C11 114(3) . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
Cd1 N1 H1A 108.7 . . ?
Cd1 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
C1 N1 Cd1 114(3) . . ?
C1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
N5 O1 Cd1 94.6(15) . . ?
N5 O2 Cd1 94(3) . . ?
Cd1 N3 H3A 105.9 . . ?
Cd1 N3 H3B 105.9 . . ?
H3A N3 H3B 106.2 . . ?
C7 N3 Cd1 125.8(13) . . ?
C7 N3 H3A 105.9 . . ?
C7 N3 H3B 105.9 . . ?
C10 C11 H11A 107.2 . . ?
C10 C11 H11B 107.2 . . ?
H11A C11 H11B 106.9 . . ?
C12 C11 C10 120(3) . . ?
C12 C11 H11A 107.2 . . ?
C12 C11 H11B 107.2 . . ?
N1 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
H1C C1 H1D 108.2 . . ?
C2 C1 N1 110(4) . . ?
C2 C1 H1C 109.6 . . ?
C2 C1 H1D 109.6 . . ?
O1 N5 O3 121(3) . . ?
O2 N5 O1 121(3) . . ?
O2 N5 O3 118(4) . . ?
N2 C4 H4C 111.0 . . ?
N2 C4 H4D 111.0 . . ?
H4C C4 H4D 109.0 . . ?
C5 C4 N2 104(4) . . ?
C5 C4 H4C 111.0 . . ?
C5 C4 H4D 111.0 . . ?
N3 C7 H7A 108.6 . . ?
N3 C7 H7B 108.6 . . ?
N3 C7 C8 114.8(19) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C11 C12 C12 111(4) . 2_666 ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C12 C12 H12A 109.5 2_666 . ?
C12 C12 H12B 109.5 2_666 . ?
H12A C12 H12B 108.1 . . ?
C1 C2 H2C 108.3 . . ?
C1 C2 H2D 108.3 . . ?
C1 C2 C3 116(4) . . ?
H2C C2 H2D 107.4 . . ?
C3 C2 H2C 108.3 . . ?
C3 C2 H2D 108.3 . . ?
C4 C5 H5A 107.5 . . ?
C4 C5 H5B 107.5 . . ?
C4 C5 C6 119(4) . . ?
H5A C5 H5B 107.0 . . ?
C6 C5 H5A 107.5 . . ?
C6 C5 H5B 107.5 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 C7 113(2) . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C2 C3 H3C 109.3 . . ?
C2 C3 H3D 109.3 . . ?
C3 C3 C2 112(4) 2_755 . ?
C3 C3 H3C 109.3 2_755 . ?
C3 C3 H3D 109.3 2_755 . ?
H3C C3 H3D 107.9 . . ?
C5 C6 H6A 107.8 . . ?
C5 C6 H6B 107.8 . . ?
C6 C6 C5 118(6) 2_675 . ?
C6 C6 H6A 107.8 2_675 . ?
C6 C6 H6B 107.8 2_675 . ?
H6A C6 H6B 107.1 . . ?
C8 C9 C9 111(8) . 2_876 ?
C8 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C9 C9 H9A 109.3 2_876 . ?
C9 C9 H9B 109.3 2_876 . ?
H9A C9 H9B 108.0 . . ?
O4 N6 O5 125(3) . . ?
O4 N6 O6 124(6) . . ?
O6 N6 O5 111(7) . . ?

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 C4 C5 C6 174.4(19) . . . . ?
N4 C10 C11 C12 47(9) . . . . ?
Cd1 N2 C4 C5 -170.6(18) . . . . ?
Cd1 N4 C10 C11 -170(5) . . . . ?
Cd1 N1 C1 C2 -178(2) . . . . ?
Cd1 O1 N5 O2 9(8) . . . . ?
Cd1 O1 N5 O3 -167(6) . . . . ?
Cd1 O2 N5 O1 -9(7) . . . . ?
Cd1 O2 N5 O3 167(6) . . . . ?
Cd1 N3 C7 C8 159(5) . . . . ?
C10 C11 C12 C12 61(8) . . . 2_666 ?
N1 C1 C2 C3 178(3) . . . . ?
N3 C7 C8 C9 -174(6) . . . . ?
C1 C2 C3 C3 57(8) . . . 2_755 ?
C4 C5 C6 C6 154(5) . . . 2_675 ?
C7 C8 C9 C9 -58(7) . . . 2_876 ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.416
_oxdiff_exptl_absorpt_empirical_full_min 0.344
####################################################################### 
# 
# 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_1_4_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262343'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We made several attempts to obtain better quality data for this structure however, due to absorption of the sample, disorder, poor crystal quality etc. crystal diffracted weakly. Furthermore the data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.285 Report
RESPONSE: We made several attempts to obtain better quality data for this structure however, due to absorption of the sample, disorder, poor crystal quality etc. crystal diffracted weakly. Furthermore the data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT029_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.255 Why?
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT084_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.54 Report
RESPONSE: We made several attempts to obtain better quality data for this structure however, due to absorption of the sample, disorder, poor crystal quality etc. crystal diffracted weakly. Furthermore the data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT088_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.92 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT082_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: High R1 Value ..................................       0.20 Report
RESPONSE: We made several attempts to obtain better quality data for this structure however, due to absorption of the sample, disorder, poor crystal quality etc. crystal diffracted weakly. Furthermore the data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT342_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.07308 Ang.
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT911_1_4_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2294 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 26 September 2023 04:16 PM
# end Validation Reply Form

_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N4, 2(N O3)'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C10 N4 O4'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.3296(18)
_cell_length_b                   9.719(3)
_cell_length_c                   11.132(6)
_cell_angle_alpha                110.81(4)
_cell_angle_beta                 105.15(3)
_cell_angle_gamma                95.96(2)
_cell_volume                     888.7(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7700
_cell_measurement_theta_min      3.9970
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.742
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -9 2 0.0986
-11 9 -2 0.1448
-6 -10 11 0.0608
9 8 -11 0.0311
-1 -4 -11 0.0213
1 4 11 0.0148
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.4705 -9.1107 2.4021 -0.0012 0.0756 0.9971
-10.6580 8.8872 -2.1307 0.0031 -0.0995 -0.9950
-6.4749 -10.2810 11.4561 0.0768 -0.9758 0.2049
8.7643 8.3692 -10.9950 -0.0775 0.9970 0.0090
-0.9590 -4.4961 -10.7030 0.9970 0.0775 -0.0093
0.9590 4.4961 10.7030 -0.9970 -0.0775 0.0093

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2850
_diffrn_reflns_av_unetI/netI     0.1658
_diffrn_reflns_Laue_measured_fraction_full 0.255
_diffrn_reflns_Laue_measured_fraction_max 0.251
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5855
_diffrn_reflns_point_group_measured_fraction_full 0.255
_diffrn_reflns_point_group_measured_fraction_max 0.251
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.665
_diffrn_reflns_theta_min         3.449
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.255
_diffrn_measured_fraction_theta_max 0.251
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.40(2) GPa
 (1400000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  49.00   1.00   22.50    --   16.41 -81.00  29.00   54
  2  ω     -8.00  23.00   1.00   22.50    --   16.41  39.00 167.00   31
  3  ω    -10.00  42.00   1.00   22.50    --   16.41 -37.00-180.00   52
  4  ω     61.00  93.00   1.00   22.50    --   16.41-178.00 -90.00   32
  5  ω    -21.00  42.00   1.00   22.50    --   16.41 -39.00-167.00   63
  6  ω    -22.00  27.00   1.00   22.50    --  -17.19 -19.00-180.00   49
  7  ω    -79.00 -21.00   1.00   22.50    --  -17.19 134.00 123.00   58
  8  ω    -41.00  13.00   1.00   22.50    --  -17.19  67.00 157.00   54
  9  ω    -50.00   7.00   1.00   22.50    --  -17.19  81.00 -29.00   57
 10  ω     -7.00  15.00   1.00   22.50    --  -17.19 -81.00-151.00   22
 11  ω      9.00  33.00   1.00   22.50    --  -17.19-114.00  44.00   24
 12  ω    -16.00  27.00   1.00   22.50    --   16.41  26.00 172.00   43
 13  ω    -47.00 -21.00   1.00   22.50    --   16.41 134.00 123.00   26
 14  ω    -15.00  27.00   1.00   22.50    --   16.41  26.00  -7.00   42
 15  ω    -24.00  44.00   1.00   22.50    --   16.41 -26.00   7.00   68
 16  ω    -34.00  -9.00   1.00   22.50    --   16.41 114.00 -44.00   25
 17  ω    -79.00 -21.00   1.00   22.50    --  -17.19 134.00 -56.00   58
 18  ω    -41.00  23.00   1.00   22.50    --  -17.19  39.00 -12.00   64
 19  ω    -42.00  -7.00   1.00   22.50    --  -17.19  39.00 167.00   35
 20  ω    -26.00  15.00   1.00   22.50    --  -17.19 -26.00   7.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356148000
_diffrn_orient_matrix_UB_12      -0.0580844000
_diffrn_orient_matrix_UB_13      -0.0655555000
_diffrn_orient_matrix_UB_21      0.0452480000
_diffrn_orient_matrix_UB_22      0.0366661000
_diffrn_orient_matrix_UB_23      -0.0266958000
_diffrn_orient_matrix_UB_31      0.0565510000
_diffrn_orient_matrix_UB_32      -0.0410183000
_diffrn_orient_matrix_UB_33      0.0130356000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                406
_reflns_number_total             847
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.611
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         847
_refine_ls_number_restraints     417
_refine_ls_R_factor_all          0.2897
_refine_ls_R_factor_gt           0.1980
_refine_ls_restrained_S_all      1.518
_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          0.4378
_refine_ls_wR_factor_ref         0.5365
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C3-C3_$1
 1.45 with sigma of 0.02
 C9-C8
 1.45 with sigma of 0.02
 C9-C9_$3
 1.45 with sigma of 0.02
 C6_$4-C10
 3.55 with sigma of 0.02
 C12-C12_$2
 1.54 with sigma of 0.02
 C12-C11 = C11-C10 = C12-C12_$2
 1.5 with sigma of 0.02
 C11-C10 = C12-C11 = C12-C12_$2
 1.48 with sigma of 0.02
 C12-C12_$2 = C12-C11 = C11-C10
 1.46 with sigma of 0.02
 C11_$2-C12
 2.2 with sigma of 0.02
 H6B_$4-H10A
 2.1 with sigma of 0.02
 H11A-H12A_$2
 2.1 with sigma of 0.02
 O2-N5 \\sim O1-N5 \\sim O3-N5
 with sigma of 0.02
 O6-O4 \\sim O6-O5 \\sim O5-O4
 with sigma of 0.02
 C9-C8 \\sim C8-C7 \\sim C6-C5 \\sim C5-C4 \\sim C11-C10 \\sim C12-C11 \\sim
C2-C1 \\sim C3-C2
 with sigma of 0.02
 O5-O4 \\sim O6-O5 \\sim O6-O4
 with sigma of 0.02
 N3-C7 \\sim N1-C1 \\sim N4-C10 \\sim N2-C4
 with sigma of 0.02
 O2-O1 \\sim O3-O2 \\sim O3-O1
 with sigma of 0.02
 O4-N6 \\sim O6-N6 \\sim O5-N6
 with sigma of 0.02
3. Restrained planarity
 O1, O2, N5, O3
 with sigma of 0.1
 O5, N6, O4, O6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5 \\sim Cd1 \\sim N3 \\sim N4 \\sim N1 \\sim N2 \\sim O2 \\sim O1 \\sim C7
\\sim C10 \\sim C1 \\sim C4 \\sim N5 \\sim O3 \\sim C8 \\sim C11 \\sim C2 \\sim
C9 \\sim C12 \\sim C3 \\sim C6 \\sim O5 \\sim N6 \\sim O4 \\sim O6: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N4 \\sim N2 \\sim Cd1 \\sim N3 \\sim N1: within 2A with sigma of 0.05 and sigma
for terminal atoms of 0.1 within 2A
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.08
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) = Uanis(O1) = Uanis(O3)
Uanis(O5) = Uanis(O4) = Uanis(O6)
Uanis(C7) = Uanis(C8) = Uanis(C9)
Uanis(N3) = Uanis(N2) = Uanis(N4) = Uanis(N1)
5. Rigid body (RIGU) restrains
 O5, Cd1, N4, N1, N2, N3, O4, C10, C1, C4, C7, N6, C11, C2, C5, C8, O6, C12,
 C3, C6, C9, O3, O1, N5, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_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
Cd1 Cd 0.8712(7) 0.5992(10) 0.2498(11) 0.089(4) Uani 1 1 d . U . . .
N4 N 0.746(5) 0.471(7) 0.339(7) 0.051(5) Uani 1 1 d D U . . .
H4A H 0.808184 0.415699 0.363698 0.062 Uiso 1 1 calc R U . . .
H4B H 0.742134 0.540426 0.414879 0.062 Uiso 1 1 calc R U . . .
C10 C 0.596(5) 0.372(7) 0.274(7) 0.063(10) Uani 1 1 d D U . . .
H10A H 0.600287 0.276717 0.208173 0.075 Uiso 1 1 calc DR U . . .
H10B H 0.525888 0.417916 0.227524 0.075 Uiso 1 1 calc R U . . .
N1 N 1.033(5) 0.447(7) 0.233(8) 0.051(5) Uani 1 1 d D U . . .
H1A H 1.095352 0.479695 0.195394 0.062 Uiso 1 1 calc R U . . .
H1B H 1.089767 0.468647 0.318050 0.062 Uiso 1 1 calc R U . . .
O1 O 0.630(5) 0.367(9) -0.018(8) 0.098(12) Uani 1 1 d D U . . .
N2 N 0.684(6) 0.719(9) 0.210(9) 0.051(5) Uani 1 1 d D U . . .
H2A H 0.597176 0.652312 0.182498 0.062 Uiso 1 1 calc R U . . .
H2B H 0.690130 0.788986 0.289863 0.062 Uiso 1 1 calc R U . . .
O2 O 0.829(5) 0.510(7) -0.020(6) 0.098(12) Uani 1 1 d D U . . .
N3 N 1.043(5) 0.782(9) 0.262(8) 0.051(5) Uani 1 1 d D U . . .
H3A H 1.042309 0.762941 0.177815 0.062 Uiso 1 1 calc R U . . .
H3B H 1.008971 0.866250 0.289869 0.062 Uiso 1 1 calc R U . . .
C11 C 0.544(7) 0.348(3) 0.382(5) 0.086(13) Uani 1 1 d D U . . .
H11A H 0.435537 0.305903 0.340931 0.103 Uiso 1 1 calc DR U . . .
H11B H 0.589901 0.268108 0.397584 0.103 Uiso 1 1 calc R U . . .
C1 C 1.001(7) 0.284(7) 0.166(8) 0.064(11) Uani 1 1 d D U . . .
H1C H 0.929100 0.262154 0.077649 0.077 Uiso 1 1 calc R U . . .
H1D H 0.941265 0.250549 0.214476 0.077 Uiso 1 1 calc R U . . .
N5 N 0.696(4) 0.425(6) -0.081(6) 0.073(13) Uani 1 1 d D U . . .
C4 C 0.668(6) 0.793(9) 0.116(9) 0.047(9) Uani 1 1 d D U . . .
H4C H 0.635209 0.714132 0.025116 0.056 Uiso 1 1 calc R U . . .
H4D H 0.768461 0.847398 0.131155 0.056 Uiso 1 1 calc R U . . .
C7 C 1.201(4) 0.815(8) 0.346(9) 0.045(6) Uani 1 1 d D U . . .
H7A H 1.229509 0.719331 0.334416 0.054 Uiso 1 1 calc R U . . .
H7B H 1.204699 0.863228 0.439452 0.054 Uiso 1 1 calc R U . . .
C12 C 0.565(4) 0.464(5) 0.518(3) 0.087(16) Uani 1 1 d D U . . .
H12A H 0.662120 0.534764 0.555264 0.104 Uiso 1 1 calc R U . . .
H12B H 0.553954 0.419438 0.581608 0.104 Uiso 1 1 calc R U . . .
C2 C 1.097(6) 0.170(5) 0.138(7) 0.064(12) Uani 1 1 d D U . . .
H2C H 1.153288 0.194777 0.083484 0.077 Uiso 1 1 calc R U . . .
H2D H 1.170325 0.187309 0.223742 0.077 Uiso 1 1 calc R U . . .
O3 O 0.629(5) 0.398(7) -0.206(6) 0.098(12) Uani 1 1 d D U . . .
C5 C 0.564(8) 0.899(10) 0.117(10) 0.065(11) Uani 1 1 d D U . . .
H5A H 0.592100 0.977147 0.207368 0.078 Uiso 1 1 calc R U . . .
H5B H 0.460913 0.844950 0.093758 0.078 Uiso 1 1 calc R U . . .
C8 C 1.324(3) 0.911(6) 0.327(5) 0.045(6) Uani 1 1 d D U . . .
H8A H 1.333516 0.853573 0.239350 0.054 Uiso 1 1 calc R U . . .
H8B H 1.287000 0.998437 0.321217 0.054 Uiso 1 1 calc R U . . .
C3 C 1.030(5) 0.005(5) 0.069(2) 0.055(11) Uani 1 1 d D U . . .
H3C H 1.106114 -0.053789 0.078112 0.066 Uiso 1 1 calc R U . . .
H3D H 0.949631 -0.023868 0.101414 0.066 Uiso 1 1 calc R U . . .
C6 C 0.569(5) 0.971(7) 0.019(7) 0.072(13) Uani 1 1 d D U . . .
H6A H 0.657587 1.053776 0.059436 0.086 Uiso 1 1 calc R U . . .
H6B H 0.579915 0.897771 -0.062299 0.086 Uiso 1 1 calc R U . . .
C9 C 1.480(4) 0.967(4) 0.4261(12) 0.045(6) Uani 1 1 d D U . . .
H9A H 1.529762 0.882235 0.405213 0.054 Uiso 1 1 calc R U . . .
H9B H 1.531004 1.040903 0.402682 0.054 Uiso 1 1 calc R U . . .
O5 O 0.877(6) 0.830(7) 0.510(7) 0.094(14) Uani 1 1 d D U . . .
N6 N 0.998(5) 0.805(6) 0.558(6) 0.13(2) Uani 1 1 d D U . . .
O4 O 1.023(5) 0.680(6) 0.511(7) 0.094(14) Uani 1 1 d D U . . .
O6 O 1.092(6) 0.901(6) 0.659(6) 0.094(14) Uani 1 1 d D U . . .


_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
Cd1 N4 2.25(3) . ?
Cd1 N1 2.22(4) . ?
Cd1 N2 2.23(3) . ?
Cd1 N3 2.20(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C10 1.45(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.487(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.45(5) . ?
O1 N5 1.28(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C4 1.45(4) . ?
O2 N5 1.29(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.46(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.484(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.491(19) . ?
N5 O3 1.28(3) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.486(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.502(18) . ?
C12 C12 1.494(11) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.488(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.495(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.483(15) . ?
C3 C3 1.45(2) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.48(8) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.46(2) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O5 N6 1.21(3) . ?
N6 O4 1.22(3) . ?
N6 O6 1.21(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N4 91.2(14) . . ?
N1 Cd1 N2 165(3) . . ?
N2 Cd1 N4 92.6(12) . . ?
N3 Cd1 N4 154(3) . . ?
N3 Cd1 N1 90.5(17) . . ?
N3 Cd1 N2 92.2(15) . . ?
Cd1 N4 H4A 105.4 . . ?
Cd1 N4 H4B 105.4 . . ?
H4A N4 H4B 106.0 . . ?
C10 N4 Cd1 128(3) . . ?
C10 N4 H4A 105.4 . . ?
C10 N4 H4B 105.4 . . ?
N4 C10 H10A 110.1 . . ?
N4 C10 H10B 110.1 . . ?
N4 C10 C11 108(4) . . ?
H10A C10 H10B 108.4 . . ?
C11 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
Cd1 N1 H1A 105.2 . . ?
Cd1 N1 H1B 105.2 . . ?
H1A N1 H1B 105.9 . . ?
C1 N1 Cd1 129(3) . . ?
C1 N1 H1A 105.2 . . ?
C1 N1 H1B 105.2 . . ?
Cd1 N2 H2A 106.6 . . ?
Cd1 N2 H2B 106.6 . . ?
H2A N2 H2B 106.5 . . ?
C4 N2 Cd1 123(2) . . ?
C4 N2 H2A 106.6 . . ?
C4 N2 H2B 106.6 . . ?
Cd1 N3 H3A 106.8 . . ?
Cd1 N3 H3B 106.8 . . ?
H3A N3 H3B 106.7 . . ?
C7 N3 Cd1 122(2) . . ?
C7 N3 H3A 106.8 . . ?
C7 N3 H3B 106.8 . . ?
C10 C11 H11A 105.8 . . ?
C10 C11 H11B 105.8 . . ?
H11A C11 H11B 106.2 . . ?
C12 C11 C10 126(5) . . ?
C12 C11 H11A 105.8 . . ?
C12 C11 H11B 105.8 . . ?
N1 C1 H1C 103.7 . . ?
N1 C1 H1D 103.7 . . ?
N1 C1 C2 134(5) . . ?
H1C C1 H1D 105.3 . . ?
C2 C1 H1C 103.7 . . ?
C2 C1 H1D 103.7 . . ?
O1 N5 O2 120.0(15) . . ?
O1 N5 O3 120.1(15) . . ?
O3 N5 O2 119.8(15) . . ?
N2 C4 H4C 107.3 . . ?
N2 C4 H4D 107.3 . . ?
N2 C4 C5 120(4) . . ?
H4C C4 H4D 106.9 . . ?
C5 C4 H4C 107.3 . . ?
C5 C4 H4D 107.3 . . ?
N3 C7 H7A 106.9 . . ?
N3 C7 H7B 106.9 . . ?
N3 C7 C8 122(4) . . ?
H7A C7 H7B 106.7 . . ?
C8 C7 H7A 106.9 . . ?
C8 C7 H7B 106.9 . . ?
C11 C12 C12 99.1(12) . 2_666 ?
C11 C12 H12A 111.9 . . ?
C11 C12 H12B 111.9 . . ?
C12 C12 H12A 111.9 2_666 . ?
C12 C12 H12B 111.9 2_666 . ?
H12A C12 H12B 109.6 . . ?
C1 C2 H2C 106.8 . . ?
C1 C2 H2D 106.8 . . ?
H2C C2 H2D 106.7 . . ?
C3 C2 C1 122(5) . . ?
C3 C2 H2C 106.8 . . ?
C3 C2 H2D 106.8 . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
C4 C5 C6 113(3) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C7 C8 H8A 106.9 . . ?
C7 C8 H8B 106.9 . . ?
H8A C8 H8B 106.7 . . ?
C9 C8 C7 122(4) . . ?
C9 C8 H8A 106.9 . . ?
C9 C8 H8B 106.9 . . ?
C2 C3 H3C 112.0 . . ?
C2 C3 H3D 112.0 . . ?
C3 C3 C2 99(5) 2_755 . ?
C3 C3 H3C 112.0 2_755 . ?
C3 C3 H3D 112.0 2_755 . ?
H3C C3 H3D 109.7 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C6 C6 C5 112(4) 2_675 . ?
C6 C6 H6A 109.1 2_675 . ?
C6 C6 H6B 109.1 2_675 . ?
H6A C6 H6B 107.8 . . ?
C8 C9 H9A 105.8 . . ?
C8 C9 H9B 105.8 . . ?
C9 C9 C8 126(5) 2_876 . ?
C9 C9 H9A 105.8 2_876 . ?
C9 C9 H9B 105.8 2_876 . ?
H9A C9 H9B 106.2 . . ?
O5 N6 O4 120.1(16) . . ?
O5 N6 O6 120.5(16) . . ?
O6 N6 O4 119.1(16) . . ?

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
Cd1 N4 C10 C11 -165(4) . . . . ?
Cd1 N1 C1 C2 174(6) . . . . ?
Cd1 N2 C4 C5 -166(7) . . . . ?
Cd1 N3 C7 C8 164(6) . . . . ?
N4 C10 C11 C12 41(6) . . . . ?
C10 C11 C12 C12 81(7) . . . 2_666 ?
N1 C1 C2 C3 178(5) . . . . ?
N2 C4 C5 C6 177(8) . . . . ?
N3 C7 C8 C9 169(5) . . . . ?
C1 C2 C3 C3 77(6) . . . 2_755 ?
C4 C5 C6 C6 158(9) . . . 2_675 ?
C7 C8 C9 C9 -45(8) . . . 2_876 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1241
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 4.020
_oxdiff_exptl_absorpt_empirical_full_min 0.397
####################################################################### 
# 
# 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_1_25_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262342'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_25_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.405 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT088_1_25_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.02 Note
RESPONSE: The data/parameter ratio is affected by the access limits of
 the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_1_25_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0425 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_1_25_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2035 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2022-07-29
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N5 O3, N O3'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd N4 O4 H10 C10'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.369(2)
_cell_length_b                   9.730(2)
_cell_length_c                   11.176(3)
_cell_angle_alpha                111.06(2)
_cell_angle_beta                 105.360(20)
_cell_angle_gamma                95.987(19)
_cell_volume                     893.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9940
_cell_measurement_theta_min      2.3080
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.804
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 8 0 0.0485
-3 -11 14 0.0555
-5 2 -12 0.0737
-6 -11 9 0.0399
7 11 -6 0.0309
-7 -11 6 0.0309
2 10 -14 0.0820
-11 7 5 0.0325
11 -7 -5 0.0325

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.9987 7.7663 0.3015 -0.0181 0.8138 -0.5809
-2.6444 -10.7203 13.5088 0.0208 -0.8368 -0.5471
-4.8185 2.4907 -12.1491 -0.0022 0.0091 1.0000
-6.2390 -11.2897 8.5604 0.0254 -0.9994 -0.0254
6.9156 10.7482 -5.6142 0.0012 0.9811 -0.1932
-6.9156 -10.7482 5.6142 -0.0012 -0.9811 0.1932
1.9813 10.0310 -14.2448 -0.0414 0.7692 0.6431
-11.1455 7.3605 4.7985 0.9942 -0.0058 0.1076
11.1455 -7.3605 -4.7985 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.405
_diffrn_reflns_Laue_measured_fraction_max 0.255
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15465
_diffrn_reflns_point_group_measured_fraction_full 0.405
_diffrn_reflns_point_group_measured_fraction_max 0.255
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.387
_diffrn_reflns_theta_min         2.065
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.405
_diffrn_measured_fraction_theta_max 0.255
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.25(2) GPa
 (1250000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  14.00   0.75   18.00    --  -30.50  67.00 157.00  100
  2  ω    -61.00  14.00   0.75   18.00    --  -30.50  67.00 -23.00  100
  3  ω      7.00  29.50   0.75   18.00    --  -30.50-114.00-135.00   30
  4  ω    -25.00  15.50   0.75   18.00    --  -30.50 -39.00  12.00   54
  5  ω      7.00  29.50   0.75   18.00    --  -30.50-114.00  45.00   30
  6  ω    -25.00  47.00   0.75   18.00    --  -30.50 -19.00-180.00   96
  7  ω    -26.00   1.00   0.75   18.00    --  -30.50 -57.00-150.00   36
  8  ω    -95.00 -20.00   0.75   18.00    --  -30.50 135.00 123.00  100
  9  ω    -33.00  42.00   0.75   18.00    --  -30.50 -13.00   3.00  100
 10  ω     -2.00  19.00   0.75   18.00    --  -30.50 -97.00  35.00   28
 11  ω    -26.00   1.00   0.75   18.00    --  -30.50 -57.00  30.00   36
 12  ω    -25.00  15.50   0.75   18.00    --  -30.50 -39.00-167.00   54
 13  ω     16.75  82.00   0.75   18.00    --   33.86-114.00  45.00   87
 14  ω      0.00  19.50   0.75   18.00    --   33.86  53.00 162.00   26
 15  ω    -25.00  36.50   0.75   18.00    --   33.86   0.00   0.00   82
 16  ω     -6.50  61.00   0.75   18.00    --   33.86 -67.00-157.00   90
 17  ω      0.00  19.50   0.75   18.00    --   33.86  53.00 -17.00   26
 18  ω    -15.25  50.00   0.75   18.00    --   33.86 -19.00-180.00   87
 19  ω    -45.00  30.00   0.75   18.00    --  -30.50  26.00  -8.00  100
 20  ω    -14.00  16.00   0.75   18.00    --  -30.50 -38.00-180.00   40
 21  ω     -2.00  19.00   0.75   18.00    --  -30.50 -97.00-143.00   28
 22  ω    -12.00   9.00   0.75   18.00    --  -30.50 -77.00-150.00   28
 23  ω     -9.00  12.00   0.75   18.00    --  -30.50 -81.00-151.00   28
 24  ω     -9.00  12.00   0.75   18.00    --  -30.50 -81.00  29.00   28
 25  ω   -117.00 -72.00   0.75   18.00    --  -30.50 178.00 -90.00   60
 26  ω    -30.00  39.00   0.75   18.00    --  -30.50 -26.00   8.00   92
 27  ω    -20.00   2.50   0.75   18.00    --  -30.50 -53.00  17.00   30
 28  ω    -61.00  14.00   0.75   18.00    --  -30.50  38.00-180.00  100
 29  ω      1.50  66.00   0.75   18.00    --   33.86 -81.00  29.00   86
 30  ω    -12.00  24.00   0.75   18.00    --   33.86  39.00 167.00   48
 31  ω    -37.00  29.00   0.75   18.00    --   33.86  26.00  -8.00   88
 32  ω     -2.00  47.50   0.75   18.00    --   33.86 -57.00-150.00   66
 33  ω    -13.00  50.00   0.75   18.00    --   33.86 -39.00  12.00   84
 34  ω    -50.00  25.00   0.75   18.00    --  -30.50  19.00-180.00  100
 35  ω    -50.00  -5.00   0.75   18.00    --  -30.50  19.00-150.00   60
 36  ω    -66.00   9.00   0.75   18.00    --  -30.50  81.00 -29.00  100
 37  ω    -55.00  20.00   0.75   18.00    --  -30.50  53.00 162.00  100
 38  ω    -73.00   2.00   0.75   18.00    --  -30.50  97.00 143.00  100
 39  ω    -33.00  42.00   0.75   18.00    --  -30.50 -13.00   3.00  100
 40  ω    -42.00  33.00   0.75   18.00    --  -30.50  13.00  -3.00  100
 41  ω    -50.00  25.00   0.75   18.00    --  -30.50  39.00 -12.00  100
 42  ω    -55.00  20.00   0.75   18.00    --  -30.50  53.00 -17.00  100
 43  ω    -61.00  14.00   0.75   18.00    --  -30.50  67.00 -23.00  100
 44  ω    -32.25  33.00   0.75   18.00    --   33.86  13.00  -3.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0472172000
_diffrn_orient_matrix_UB_12      0.0452051000
_diffrn_orient_matrix_UB_13      0.0281719000
_diffrn_orient_matrix_UB_21      0.0405589000
_diffrn_orient_matrix_UB_22      0.0631602000
_diffrn_orient_matrix_UB_23      -0.0038836000
_diffrn_orient_matrix_UB_31      -0.0510717000
_diffrn_orient_matrix_UB_32      -0.0196331000
_diffrn_orient_matrix_UB_33      -0.0660766000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                860
_reflns_number_total             1139
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         1139
_refine_ls_number_restraints     403
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0806
_refine_ls_restrained_S_all      0.926
_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)+(0.0698P)²+17.1750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2064
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C12-C12_$1
 1.45 with sigma of 0.05
 C3-C3_$2
 1.45 with sigma of 0.05
 C9-C9_$3
 1.45 with sigma of 0.05
 C6-C6_$4
 1.45 with sigma of 0.05
 O4-N5 \\sim O6-N5 \\sim O5-N5 \\sim O1-N7 \\sim O2-N7 \\sim O3-N7
 with sigma of 0.05
 N4-C10 \\sim N1-C1 \\sim N3-C7 \\sim N2-C4
 with sigma of 0.05
 C8-C7 \\sim C9-C8 \\sim C5-C4 \\sim C6-C5 \\sim C11-C10 \\sim C12-C11 \\sim
C3-C2 \\sim C2-C1
 with sigma of 0.05
3. Rigid bond restraints
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, O6, O4, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, N7, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C5, C6, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N5 \\sim O6 \\sim O4 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N4 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O2 \\sim N7 \\sim O3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O3) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O6, O4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O2, N7, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_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
N2 N 0.696(4) 0.733(4) 0.222(2) 0.048(6) Uani 1 1 d D U . . .
H2A H 0.606088 0.678198 0.207160 0.058 Uiso 1 1 calc R U . . .
H2B H 0.717372 0.814000 0.299546 0.058 Uiso 1 1 calc R U . . .
N4 N 0.757(3) 0.479(4) 0.350(2) 0.070(14) Uani 1 1 d D U . . .
H4A H 0.815400 0.417861 0.368722 0.084 Uiso 1 1 calc R U . . .
H4B H 0.762634 0.549699 0.429560 0.084 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8703(3) 0.5978(3) 0.2473(2) 0.068(4) Uani 1 1 d . . . . .
C10 C 0.598(4) 0.389(5) 0.287(3) 0.066(10) Uani 1 1 d D U . . .
H10A H 0.588919 0.306268 0.202528 0.080 Uiso 1 1 calc R U . . .
H10B H 0.530529 0.452113 0.266095 0.080 Uiso 1 1 calc R U . . .
N1 N 1.047(4) 0.445(3) 0.239(2) 0.046(5) Uani 1 1 d D U . . .
H1A H 1.117129 0.476578 0.208393 0.055 Uiso 1 1 calc R U . . .
H1B H 1.094215 0.451918 0.322181 0.055 Uiso 1 1 calc R U . . .
O1 O 0.670(3) 0.413(3) 0.022(2) 0.066(6) Uani 1 1 d D U . . .
O2 O 0.852(3) 0.541(3) -0.001(2) 0.060(6) Uani 1 1 d D U . . .
N3 N 1.061(3) 0.783(3) 0.270(2) 0.045(6) Uani 1 1 d D U . . .
H3A H 1.068519 0.759306 0.187298 0.054 Uiso 1 1 calc R U . . .
H3B H 1.026140 0.867180 0.289302 0.054 Uiso 1 1 calc R U . . .
C11 C 0.549(4) 0.324(4) 0.381(3) 0.066(7) Uani 1 1 d D U . . .
H11A H 0.449645 0.257459 0.331520 0.079 Uiso 1 1 calc R U . . .
H11B H 0.619601 0.264300 0.403972 0.079 Uiso 1 1 calc R U . . .
C1 C 0.974(4) 0.287(3) 0.151(2) 0.048(5) Uani 1 1 d D U . . .
H1C H 0.924982 0.276586 0.058879 0.058 Uiso 1 1 calc R U . . .
H1D H 0.898373 0.250049 0.183031 0.058 Uiso 1 1 calc R U . . .
N7 N 0.723(4) 0.453(4) -0.054(2) 0.055(6) Uani 1 1 d D U . . .
C4 C 0.684(4) 0.784(4) 0.113(2) 0.047(6) Uani 1 1 d D U . . .
H4C H 0.641235 0.698184 0.026121 0.057 Uiso 1 1 calc R U . . .
H4D H 0.783950 0.830231 0.119262 0.057 Uiso 1 1 calc R U . . .
C7 C 1.220(4) 0.827(4) 0.364(3) 0.046(6) Uani 1 1 d D U . . .
H7A H 1.253478 0.735728 0.362926 0.055 Uiso 1 1 calc R U . . .
H7B H 1.220195 0.884810 0.454803 0.055 Uiso 1 1 calc R U . . .
C12 C 0.543(3) 0.443(3) 0.511(2) 0.058(6) Uani 1 1 d D U . . .
H12A H 0.497310 0.393741 0.557189 0.070 Uiso 1 1 calc R U . . .
H12B H 0.646160 0.495530 0.569750 0.070 Uiso 1 1 calc R U . . .
C2 C 1.101(4) 0.196(3) 0.154(2) 0.047(5) Uani 1 1 d D U . . .
H2C H 1.155249 0.217027 0.247357 0.056 Uiso 1 1 calc R U . . .
H2D H 1.171850 0.231298 0.116335 0.056 Uiso 1 1 calc R U . . .
O3 O 0.654(4) 0.414(3) -0.175(2) 0.059(7) Uani 1 1 d D U . . .
C5 C 0.585(4) 0.896(4) 0.120(3) 0.049(6) Uani 1 1 d D U . . .
H5A H 0.625802 0.977275 0.209861 0.058 Uiso 1 1 calc R U . . .
H5B H 0.485219 0.846792 0.111840 0.058 Uiso 1 1 calc R U . . .
C8 C 1.332(3) 0.919(4) 0.330(3) 0.048(6) Uani 1 1 d D U . . .
H8A H 1.331814 0.862619 0.238592 0.058 Uiso 1 1 calc R U . . .
H8B H 1.302331 1.012300 0.334437 0.058 Uiso 1 1 calc R U . . .
C3 C 1.043(4) 0.022(3) 0.074(2) 0.047(6) Uani 1 1 d D U . . .
H3C H 1.128480 -0.026216 0.081087 0.056 Uiso 1 1 calc R U . . .
H3D H 0.976455 -0.015819 0.114299 0.056 Uiso 1 1 calc R U . . .
C6 C 0.563(2) 0.968(3) 0.017(2) 0.042(7) Uani 1 1 d D U . . .
H6A H 0.653136 1.047377 0.047952 0.051 Uiso 1 1 calc R U . . .
H6B H 0.563757 0.891723 -0.067565 0.051 Uiso 1 1 calc R U . . .
C9 C 1.489(3) 0.953(3) 0.4268(17) 0.045(6) Uani 1 1 d D U . . .
H9A H 1.557680 1.006100 0.398128 0.054 Uiso 1 1 calc R U . . .
H9B H 1.517605 0.858710 0.419889 0.054 Uiso 1 1 calc R U . . .
N5 N 0.995(3) 1.186(3) 0.431(2) 0.058(9) Uani 1 1 d D U . . .
O6 O 1.125(4) 1.161(4) 0.476(3) 0.095(10) Uani 1 1 d D U . . .
O4 O 0.962(3) 1.316(3) 0.476(2) 0.074(9) Uani 1 1 d D U . . .
O5 O 0.896(4) 1.079(3) 0.336(2) 0.077(10) Uani 1 1 d D U . . .


_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 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 Cd1 2.23(4) . ?
N2 C4 1.46(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.262(19) . ?
N4 C10 1.49(3) . ?
Cd1 N1 2.34(4) . ?
Cd1 O1 2.575(15) . ?
Cd1 O2 2.58(3) . ?
Cd1 N3 2.297(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.54(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.46(3) . ?
O1 N7 1.24(3) . ?
O2 N7 1.25(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.48(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.52(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.55(4) . ?
N7 O3 1.23(2) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.50(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.52(3) . ?
C12 C12 1.48(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.56(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.53(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.49(3) . ?
C3 C3 1.51(3) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.42(5) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.50(4) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N5 O6 1.27(3) . ?
N5 O4 1.28(4) . ?
N5 O5 1.25(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
H2A N2 H2B 107.5 . . ?
Cd1 N2 H2A 108.5 . . ?
Cd1 N2 H2B 108.5 . . ?
C4 N2 H2A 108.5 . . ?
C4 N2 H2B 108.5 . . ?
C4 N2 Cd1 115(3) . . ?
H4A N4 H4B 106.6 . . ?
Cd1 N4 H4A 106.6 . . ?
Cd1 N4 H4B 106.6 . . ?
C10 N4 H4A 106.6 . . ?
C10 N4 H4B 106.6 . . ?
C10 N4 Cd1 122.9(12) . . ?
N2 Cd1 N4 94.7(13) . . ?
N2 Cd1 N1 171.4(9) . . ?
N2 Cd1 O1 78.6(11) . . ?
N2 Cd1 O2 86.9(13) . . ?
N2 Cd1 N3 92.8(11) . . ?
N4 Cd1 N1 90.7(13) . . ?
N4 Cd1 O1 87.0(6) . . ?
N4 Cd1 O2 134.6(7) . . ?
N4 Cd1 N3 147.5(7) . . ?
N1 Cd1 O1 95.0(11) . . ?
N1 Cd1 O2 84.5(11) . . ?
O1 Cd1 O2 48.8(7) . . ?
N3 Cd1 N1 86.2(11) . . ?
N3 Cd1 O1 125.4(6) . . ?
N3 Cd1 O2 77.3(7) . . ?
N4 C10 H10A 109.2 . . ?
N4 C10 H10B 109.2 . . ?
N4 C10 C11 111.9(18) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
Cd1 N1 H1A 109.4 . . ?
Cd1 N1 H1B 109.4 . . ?
H1A N1 H1B 108.0 . . ?
C1 N1 Cd1 111(2) . . ?
C1 N1 H1A 109.4 . . ?
C1 N1 H1B 109.4 . . ?
N7 O1 Cd1 96.8(11) . . ?
N7 O2 Cd1 96.1(18) . . ?
Cd1 N3 H3A 105.8 . . ?
Cd1 N3 H3B 105.8 . . ?
H3A N3 H3B 106.2 . . ?
C7 N3 Cd1 126.2(11) . . ?
C7 N3 H3A 105.8 . . ?
C7 N3 H3B 105.8 . . ?
C10 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 C10 114(3) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
N1 C1 H1C 110.3 . . ?
N1 C1 H1D 110.3 . . ?
N1 C1 C2 107(2) . . ?
H1C C1 H1D 108.6 . . ?
C2 C1 H1C 110.3 . . ?
C2 C1 H1D 110.3 . . ?
O1 N7 O2 117.3(17) . . ?
O3 N7 O1 123(2) . . ?
O3 N7 O2 120(2) . . ?
N2 C4 H4C 109.5 . . ?
N2 C4 H4D 109.5 . . ?
N2 C4 C5 111(3) . . ?
H4C C4 H4D 108.1 . . ?
C5 C4 H4C 109.5 . . ?
C5 C4 H4D 109.5 . . ?
N3 C7 H7A 108.6 . . ?
N3 C7 H7B 108.6 . . ?
N3 C7 C8 114.8(15) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
C12 C12 C11 114(3) 2_666 . ?
C12 C12 H12A 108.8 2_666 . ?
C12 C12 H12B 108.8 2_666 . ?
H12A C12 H12B 107.7 . . ?
C1 C2 H2C 108.6 . . ?
C1 C2 H2D 108.6 . . ?
C1 C2 C3 115(2) . . ?
H2C C2 H2D 107.6 . . ?
C3 C2 H2C 108.6 . . ?
C3 C2 H2D 108.6 . . ?
C4 C5 H5A 107.6 . . ?
C4 C5 H5B 107.6 . . ?
C4 C5 C6 119(3) . . ?
H5A C5 H5B 107.1 . . ?
C6 C5 H5A 107.6 . . ?
C6 C5 H5B 107.6 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 C7 111.1(15) . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C2 C3 H3C 109.2 . . ?
C2 C3 H3D 109.2 . . ?
C3 C3 C2 112(3) 2_755 . ?
C3 C3 H3C 109.2 2_755 . ?
C3 C3 H3D 109.2 2_755 . ?
H3C C3 H3D 107.9 . . ?
C5 C6 H6A 106.7 . . ?
C5 C6 H6B 106.7 . . ?
C6 C6 C5 123(3) 2_675 . ?
C6 C6 H6A 106.7 2_675 . ?
C6 C6 H6B 106.7 2_675 . ?
H6A C6 H6B 106.6 . . ?
C8 C9 C9 116(4) . 2_876 ?
C8 C9 H9A 108.2 . . ?
C8 C9 H9B 108.2 . . ?
C9 C9 H9A 108.2 2_876 . ?
C9 C9 H9B 108.2 2_876 . ?
H9A C9 H9B 107.4 . . ?
O6 N5 O4 124(2) . . ?
O5 N5 O6 117(3) . . ?
O5 N5 O4 119(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
N2 C4 C5 C6 177.5(15) . . . . ?
N4 C10 C11 C12 65(5) . . . . ?
Cd1 N2 C4 C5 -169.8(13) . . . . ?
Cd1 N4 C10 C11 -179(3) . . . . ?
Cd1 N1 C1 C2 -179.4(14) . . . . ?
Cd1 O1 N7 O2 10(4) . . . . ?
Cd1 O1 N7 O3 -168(4) . . . . ?
Cd1 O2 N7 O1 -10(4) . . . . ?
Cd1 O2 N7 O3 168(4) . . . . ?
Cd1 N3 C7 C8 163(3) . . . . ?
C10 C11 C12 C12 50(4) . . . 2_666 ?
N1 C1 C2 C3 175.4(18) . . . . ?
N3 C7 C8 C9 -178(4) . . . . ?
C1 C2 C3 C3 59(5) . . . 2_755 ?
C4 C5 C6 C6 158(3) . . . 2_675 ?
C7 C8 C9 C9 -62(4) . . . 2_876 ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.285
_oxdiff_exptl_absorpt_empirical_full_min 0.659
####################################################################### 
# 
# 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_1_5_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262344'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.347 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.94 Note
RESPONSE: The data/parameter ratio is affected by the access limits 
of the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_1_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.10333 Ang.
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_vrf_PLAT911_1_5_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1884 Report
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12 H32 N6 O6'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.3399(16)
_cell_length_b                   9.7227(16)
_cell_length_c                   11.104(3)
_cell_angle_alpha                110.89(2)
_cell_angle_beta                 105.022(19)
_cell_angle_gamma                96.004(14)
_cell_volume                     887.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9170
_cell_measurement_theta_min      2.3010
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.044
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 -2 8 0.0485
2 13 -4 0.0555
9 -10 -4 0.0737
9 9 -7 0.0399
-10 -7 8 0.0309
10 7 -8 0.0309
-1 -13 3 0.0820

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.5108 -1.9698 8.0175 -0.0181 0.8138 -0.5809
2.3223 12.8760 -3.7129 0.0208 -0.8368 -0.5471
9.1319 -9.5638 -3.8961 -0.0022 0.0091 1.0000
8.5648 9.4169 -6.8977 0.0254 -0.9994 -0.0254
-10.3276 -7.2660 7.9763 0.0012 0.9811 -0.1932
10.3276 7.2660 -7.9763 -0.0012 -0.9811 0.1932
-0.9209 -13.0895 2.5663 -0.0414 0.7692 0.6431

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1418
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.347
_diffrn_reflns_Laue_measured_fraction_max 0.202
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7141
_diffrn_reflns_point_group_measured_fraction_full 0.347
_diffrn_reflns_point_group_measured_fraction_max 0.202
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.287
_diffrn_reflns_theta_min         2.298
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.347
_diffrn_measured_fraction_theta_max 0.202
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.50(2) GPa
 (1500000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  32.50   0.75   10.00    --    0.00 -57.00-180.00   46
  2  ω     -9.00  42.00   0.75   10.00    --    0.00 -81.00-151.00   68
  3  ω      7.00  59.50   0.75   10.00    --    0.00-114.00-135.00   70
  4  ω    -25.00  15.50   0.75   12.50    --  -30.50 -39.00  12.00   54
  5  ω    -33.00  42.00   0.75   12.50    --  -30.50 -13.00   3.00  100
  6  ω    -37.00  36.50   0.75   12.50    --  -30.50   0.00-180.00   98
  7  ω    -55.00  20.00   0.75   12.50    --  -30.50  53.00 162.00  100
  8  ω    -25.00  15.50   0.75   12.50    --  -30.50 -39.00-167.00   54
  9  ω     -9.00  12.00   0.75   12.50    --  -30.50 -81.00-151.00   28
 10  ω   -109.00 -73.00   0.75   12.50    --  -30.50 178.00  90.00   48
 11  ω     -2.00  19.00   0.75   12.50    --  -30.50 -97.00  35.00   28
 12  ω    -14.00  16.00   0.75   12.50    --  -30.50 -38.00-180.00   40
 13  ω    -55.00  20.00   0.75   12.50    --  -30.50  53.00 -17.00  100
 14  ω    -30.00  39.00   0.75   12.50    --  -30.50 -26.00   8.00   92
 15  ω    -26.00   1.00   0.75   12.50    --  -30.50 -57.00  30.00   36
 16  ω    -82.00  -7.00   0.75   12.50    --  -30.50 114.00 -45.00  100
 17  ω     27.50  95.00   0.75   12.50    --   33.71-135.00  57.00   90
 18  ω     12.00  63.00   0.75   12.50    --   33.71 -77.00-150.00   68
 19  ω    -37.00   6.50   0.75   12.50    --   33.71   0.00-150.00   58
 20  ω    -12.00  24.00   0.75   12.50    --   33.71  39.00 -12.00   48
 21  ω      0.00  19.50   0.75   12.50    --   33.71  53.00 162.00   26
 22  ω    -51.00   1.50   0.75   10.00    --    0.00  97.00 -35.00   70
 23  ω    -35.00 -12.50   0.75   10.00    --    0.00  77.00 -30.00   30
 24  ω      7.00  29.50   0.75   12.50    --  -30.50-114.00-135.00   30
 25  ω      7.00  29.50   0.75   12.50    --  -30.50-114.00  45.00   30
 26  ω    -13.25  55.00   0.75   12.50    --   33.71 -53.00  17.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0426425000
_diffrn_orient_matrix_UB_12      0.0134125000
_diffrn_orient_matrix_UB_13      0.0675782000
_diffrn_orient_matrix_UB_21      -0.0560134000
_diffrn_orient_matrix_UB_22      -0.0546986000
_diffrn_orient_matrix_UB_23      0.0006552000
_diffrn_orient_matrix_UB_31      0.0391958000
_diffrn_orient_matrix_UB_32      -0.0568417000
_diffrn_orient_matrix_UB_33      -0.0252569000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                611
_reflns_number_total             891
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         891
_refine_ls_number_restraints     403
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0851
_refine_ls_restrained_S_all      0.894
_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)+(0.1181P)²+20.7060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2517
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 H7B_$1-H3B_$1
 2.1 with sigma of 0.02
 C4-N2
 1.35 with sigma of 0.02
 O1-N5 \\sim O3-N5 \\sim O2-N5 \\sim O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.02
3. Rigid bond restraints
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, O5, O4, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, N5, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O2 \\sim N5 \\sim O3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N6 \\sim O5 \\sim O4 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N4 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(Cd1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O1) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O6, N6, O5, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O2, N5, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C10, N4, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
N2 N 0.684(5) 0.738(3) 0.213(7) 0.041(6) Uani 1 1 d D U . . .
H2A H 0.593958 0.680118 0.193961 0.050 Uiso 1 1 calc R U . . .
H2B H 0.701059 0.815559 0.291152 0.050 Uiso 1 1 calc R U . . .
N4 N 0.752(5) 0.479(3) 0.352(7) 0.044(7) Uani 1 1 d . U . . .
H4A H 0.818900 0.430971 0.383317 0.053 Uiso 1 1 calc R U . . .
H4B H 0.748314 0.554023 0.425767 0.053 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8694(5) 0.5962(3) 0.2457(8) 0.045(4) Uani 1 1 d . U . . .
C10 C 0.617(7) 0.382(4) 0.306(10) 0.049(7) Uani 1 1 d . U . . .
H10A H 0.622408 0.295709 0.230788 0.058 Uiso 1 1 calc R U . . .
H10B H 0.543349 0.430323 0.266654 0.058 Uiso 1 1 calc R U . . .
N1 N 1.047(5) 0.447(2) 0.243(7) 0.031(6) Uani 1 1 d . U . . .
H1A H 1.123323 0.483991 0.221918 0.038 Uiso 1 1 calc R U . . .
H1B H 1.084723 0.446990 0.325856 0.038 Uiso 1 1 calc R U . . .
O1 O 0.668(4) 0.421(2) 0.031(5) 0.059(6) Uani 1 1 d D U . . .
O2 O 0.856(4) 0.537(2) 0.000(5) 0.056(7) Uani 1 1 d D U . . .
N3 N 1.052(4) 0.795(2) 0.275(6) 0.033(6) Uani 1 1 d . U . . .
H3A H 1.054260 0.782894 0.192077 0.040 Uiso 1 1 calc R U . . .
H3B H 1.016863 0.877937 0.305651 0.040 Uiso 1 1 calc R U . . .
C11 C 0.548(7) 0.322(3) 0.379(10) 0.044(7) Uani 1 1 d . U . . .
H11A H 0.599449 0.246093 0.396302 0.053 Uiso 1 1 calc R U . . .
H11B H 0.443147 0.272127 0.323715 0.053 Uiso 1 1 calc R U . . .
C1 C 0.972(6) 0.278(3) 0.136(9) 0.032(6) Uani 1 1 d . U . . .
H1C H 0.890999 0.234263 0.160454 0.038 Uiso 1 1 calc R U . . .
H1D H 0.928234 0.276094 0.045782 0.038 Uiso 1 1 calc R U . . .
N5 N 0.720(4) 0.452(4) -0.056(5) 0.052(7) Uani 1 1 d D U . . .
C4 C 0.674(5) 0.792(3) 0.115(7) 0.040(6) Uani 1 1 d D U . . .
H4C H 0.632459 0.708180 0.026783 0.047 Uiso 1 1 calc R U . . .
H4D H 0.774972 0.837779 0.123281 0.047 Uiso 1 1 calc R U . . .
C7 C 1.207(4) 0.830(3) 0.358(6) 0.032(6) Uani 1 1 d . U . . .
H7A H 1.239528 0.737127 0.352920 0.038 Uiso 1 1 calc R U . . .
H7B H 1.215588 0.888456 0.451900 0.038 Uiso 1 1 calc R U . . .
C12 C 0.550(6) 0.447(3) 0.521(9) 0.041(7) Uani 1 1 d . U . . .
H12A H 0.507659 0.401206 0.571841 0.049 Uiso 1 1 calc R U . . .
H12B H 0.652993 0.503325 0.575460 0.049 Uiso 1 1 calc R U . . .
C2 C 1.093(6) 0.188(3) 0.136(8) 0.033(6) Uani 1 1 d . U . . .
H2C H 1.159843 0.219647 0.092298 0.040 Uiso 1 1 calc R U . . .
H2D H 1.153141 0.214632 0.229802 0.040 Uiso 1 1 calc R U . . .
O3 O 0.640(4) 0.419(3) -0.182(6) 0.059(6) Uani 1 1 d D U . . .
C5 C 0.578(7) 0.904(3) 0.122(10) 0.042(6) Uani 1 1 d . U . . .
H5A H 0.619188 0.987486 0.210317 0.050 Uiso 1 1 calc R U . . .
H5B H 0.476558 0.857811 0.114138 0.050 Uiso 1 1 calc R U . . .
C8 C 1.309(7) 0.919(3) 0.312(10) 0.040(6) Uani 1 1 d . U . . .
H8A H 1.277135 1.012025 0.315110 0.048 Uiso 1 1 calc R U . . .
H8B H 1.305665 0.860193 0.219321 0.048 Uiso 1 1 calc R U . . .
C3 C 1.043(9) 0.021(4) 0.069(13) 0.033(7) Uani 1 1 d . U . . .
H3C H 1.131225 -0.024181 0.073922 0.040 Uiso 1 1 calc R U . . .
H3D H 0.982430 -0.014580 0.114906 0.040 Uiso 1 1 calc R U . . .
C6 C 0.566(6) 0.967(3) 0.007(9) 0.036(6) Uani 1 1 d . U . . .
H6A H 0.656814 1.041893 0.030733 0.043 Uiso 1 1 calc R U . . .
H6B H 0.555658 0.885280 -0.079057 0.043 Uiso 1 1 calc R U . . .
C9 C 1.483(6) 0.955(3) 0.421(9) 0.037(7) Uani 1 1 d . U . . .
H9A H 1.510603 0.858717 0.409127 0.044 Uiso 1 1 calc R U . . .
H9B H 1.551854 1.009476 0.393503 0.044 Uiso 1 1 calc R U . . .
N6 N 0.999(4) 0.812(2) 0.563(5) 0.043(6) Uani 1 1 d D U . . .
O5 O 0.866(5) 0.828(3) 0.504(6) 0.073(9) Uani 1 1 d D U . . .
O4 O 1.020(5) 0.676(2) 0.498(8) 0.036(6) Uani 1 1 d D U . . .
O6 O 1.104(5) 0.923(3) 0.662(7) 0.071(9) Uani 1 1 d D U . . .


_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 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 Cd1 2.36(4) . ?
N2 C4 1.35(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.30(4) . ?
N4 C10 1.35(5) . ?
Cd1 N1 2.32(3) . ?
Cd1 O1 2.50(5) . ?
Cd1 O2 2.54(5) . ?
Cd1 N3 2.310(19) . ?
Cd1 O4 2.57(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.39(7) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.60(6) . ?
O1 N5 1.30(3) . ?
O2 N5 1.30(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.43(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.61(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.50(5) . ?
N5 O3 1.30(3) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.48(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.52(4) . ?
C12 C12 1.57(12) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.48(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.59(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.68(12) . ?
C3 C3 1.4(3) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.45(9) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.57(17) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N6 O5 1.30(3) . ?
N6 O4 1.32(2) . ?
N6 O6 1.31(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H2A N2 H2B 107.1 . . ?
Cd1 N2 H2A 107.8 . . ?
Cd1 N2 H2B 107.8 . . ?
C4 N2 H2A 107.8 . . ?
C4 N2 H2B 107.8 . . ?
C4 N2 Cd1 118(2) . . ?
H4A N4 H4B 105.7 . . ?
Cd1 N4 H4A 104.6 . . ?
Cd1 N4 H4B 104.6 . . ?
C10 N4 H4A 104.6 . . ?
C10 N4 H4B 104.6 . . ?
C10 N4 Cd1 131(6) . . ?
N2 Cd1 O1 75.6(15) . . ?
N2 Cd1 O2 86.5(17) . . ?
N2 Cd1 O4 112.7(17) . . ?
N4 Cd1 N2 94.8(14) . . ?
N4 Cd1 N1 90.8(11) . . ?
N4 Cd1 O1 85.9(19) . . ?
N4 Cd1 O2 134.8(16) . . ?
N4 Cd1 N3 146(2) . . ?
N4 Cd1 O4 66.9(18) . . ?
N1 Cd1 N2 171(2) . . ?
N1 Cd1 O1 98.2(16) . . ?
N1 Cd1 O2 84.8(19) . . ?
N1 Cd1 O4 75.7(18) . . ?
O1 Cd1 O2 50.6(10) . . ?
O1 Cd1 O4 151.8(9) . . ?
O2 Cd1 O4 151.6(8) . . ?
N3 Cd1 N2 89.1(10) . . ?
N3 Cd1 N1 90.1(8) . . ?
N3 Cd1 O1 127.8(17) . . ?
N3 Cd1 O2 79.4(14) . . ?
N3 Cd1 O4 80.2(15) . . ?
N4 C10 H10A 105.3 . . ?
N4 C10 H10B 105.3 . . ?
N4 C10 C11 128(9) . . ?
H10A C10 H10B 106.0 . . ?
C11 C10 H10A 105.3 . . ?
C11 C10 H10B 105.3 . . ?
Cd1 N1 H1A 109.5 . . ?
Cd1 N1 H1B 109.5 . . ?
H1A N1 H1B 108.1 . . ?
C1 N1 Cd1 111(3) . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
N5 O1 Cd1 99(2) . . ?
N5 O2 Cd1 97(2) . . ?
Cd1 N3 H3A 106.2 . . ?
Cd1 N3 H3B 106.2 . . ?
H3A N3 H3B 106.4 . . ?
C7 N3 Cd1 124.4(18) . . ?
C7 N3 H3A 106.2 . . ?
C7 N3 H3B 106.2 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
C10 C11 C12 113(3) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
N1 C1 H1C 110.1 . . ?
N1 C1 H1D 110.1 . . ?
H1C C1 H1D 108.4 . . ?
C2 C1 N1 108(5) . . ?
C2 C1 H1C 110.1 . . ?
C2 C1 H1D 110.1 . . ?
O1 N5 O2 112(4) . . ?
O1 N5 O3 124(4) . . ?
O2 N5 O3 123(4) . . ?
N2 C4 H4C 108.9 . . ?
N2 C4 H4D 108.9 . . ?
N2 C4 C5 113(4) . . ?
H4C C4 H4D 107.7 . . ?
C5 C4 H4C 108.9 . . ?
C5 C4 H4D 108.9 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
N3 C7 C8 111(4) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C11 C12 H12A 110.8 . . ?
C11 C12 H12B 110.8 . . ?
C12 C12 C11 105(9) 2_666 . ?
C12 C12 H12A 110.8 2_666 . ?
C12 C12 H12B 110.8 2_666 . ?
H12A C12 H12B 108.9 . . ?
C1 C2 H2C 108.0 . . ?
C1 C2 H2D 108.0 . . ?
H2C C2 H2D 107.2 . . ?
C3 C2 C1 117(5) . . ?
C3 C2 H2C 108.0 . . ?
C3 C2 H2D 108.0 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113(4) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C7 C8 H8A 110.8 . . ?
C7 C8 H8B 110.8 . . ?
C7 C8 C9 105(6) . . ?
H8A C8 H8B 108.9 . . ?
C9 C8 H8A 110.8 . . ?
C9 C8 H8B 110.8 . . ?
C2 C3 H3C 109.8 . . ?
C2 C3 H3D 109.8 . . ?
C3 C3 C2 109(8) 2_755 . ?
C3 C3 H3C 109.8 2_755 . ?
C3 C3 H3D 109.8 2_755 . ?
H3C C3 H3D 108.3 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
C6 C6 C5 108(5) 2_675 . ?
C6 C6 H6A 110.0 2_675 . ?
C6 C6 H6B 110.0 2_675 . ?
H6A C6 H6B 108.4 . . ?
C8 C9 H9A 107.1 . . ?
C8 C9 H9B 107.1 . . ?
C9 C9 C8 121(3) 2_876 . ?
C9 C9 H9A 107.1 2_876 . ?
C9 C9 H9B 107.1 2_876 . ?
H9A C9 H9B 106.8 . . ?
O5 N6 O4 111(4) . . ?
O5 N6 O6 123(3) . . ?
O6 N6 O4 125(4) . . ?
N6 O4 Cd1 106(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 C4 C5 C6 -180(4) . . . . ?
N4 C10 C11 C12 47(7) . . . . ?
Cd1 N2 C4 C5 -168(4) . . . . ?
Cd1 N4 C10 C11 -176(2) . . . . ?
Cd1 N1 C1 C2 178(4) . . . . ?
Cd1 O1 N5 O2 9(3) . . . . ?
Cd1 O1 N5 O3 -162(4) . . . . ?
Cd1 O2 N5 O1 -9(3) . . . . ?
Cd1 O2 N5 O3 163(3) . . . . ?
Cd1 N3 C7 C8 156(2) . . . . ?
C10 C11 C12 C12 64(6) . . . 2_666 ?
N1 C1 C2 C3 166(7) . . . . ?
N3 C7 C8 C9 178(2) . . . . ?
C1 C2 C3 C3 58(7) . . . 2_755 ?
C4 C5 C6 C6 161(5) . . . 2_675 ?
C7 C8 C9 C9 -59(4) . . . 2_876 ?
O5 N6 O4 Cd1 32(3) . . . . ?
O6 N6 O4 Cd1 -140(3) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 11.253
_oxdiff_exptl_absorpt_empirical_full_min 0.413
####################################################################### 
# 
# 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_1_77_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262346'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT027_1_77_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT029_1_77_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.341 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_77_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.90 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC,
 particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_1_77_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.06833 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_1_77_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1878 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12H32 N6 O6 '
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'
Cd Cd -0.8075 1.2024 '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      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                   9.319(3)
_cell_length_b                   9.7075(18)
_cell_length_c                   11.051(5)
_cell_angle_alpha                110.92(3)
_cell_angle_beta                 104.97(3)
_cell_angle_gamma                96.149(18)
_cell_volume                     879.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1090
_cell_measurement_theta_min      2.2980
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.044
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.70304
_exptl_absorpt_correction_T_min  0.69528
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 8 0.0485
2 13 -4 0.0555
9 -10 -4 0.0737
9 9 -7 0.0399
-10 -7 8 0.0309
10 7 -8 0.0309
-1 -13 3 0.0820

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.4783 -1.9395 7.9896 -0.0181 0.8138 -0.5809
2.3198 12.8426 -3.6950 0.0208 -0.8368 -0.5471
9.1051 -9.5615 -3.8868 -0.0022 0.0091 1.0000
8.5449 9.3782 -6.8705 0.0254 -0.9994 -0.0254
-10.3018 -7.2291 7.9458 0.0012 0.9811 -0.1932
10.3018 7.2291 -7.9458 -0.0012 -0.9811 0.1932
-0.9226 -13.0580 2.5527 -0.0414 0.7692 0.6431

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.341
_diffrn_reflns_Laue_measured_fraction_max 0.203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6027
_diffrn_reflns_point_group_measured_fraction_full 0.341
_diffrn_reflns_point_group_measured_fraction_max 0.203
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         28.263
_diffrn_reflns_theta_min         2.303
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.341
_diffrn_measured_fraction_theta_max 0.203
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.77(2) GPa
 (1770000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     57.00  88.50   0.75   25.00    --    0.00-178.00 -90.00   42
  2  ω     -2.00  19.00   0.75   25.00    --  -30.50 -97.00  35.00   28
  3  ω      7.00  29.50   0.75   25.00    --  -30.50-114.00  45.00   30
  4  ω    -66.00   9.00   0.75   25.00    --  -30.50  81.00 151.00  100
  5  ω    -25.00  15.50   0.75   25.00    --  -30.50 -39.00-167.00   54
  6  ω   -109.00 -73.00   0.75   25.00    --  -30.50 178.00  90.00   48
  7  ω    -30.00  39.00   0.75   25.00    --  -30.50 -26.00-171.00   92
  8  ω    -37.00  36.50   0.75   25.00    --  -30.50   0.00-180.00   98
  9  ω    -20.00   2.50   0.75   25.00    --  -30.50 -53.00-162.00   30
 10  ω    -42.00  33.00   0.75   25.00    --  -30.50  13.00 176.00  100
 11  ω    -25.00  15.50   0.75   25.00    --  -30.50 -39.00  12.00   54
 12  ω    -55.00  20.00   0.75   25.00    --  -30.50  53.00 162.00  100
 13  ω    -61.00  14.00   0.75   25.00    --  -30.50  67.00 -23.00  100
 14  ω   -117.00 -72.00   0.75   25.00    --  -30.50 178.00 -90.00   60
 15  ω    -61.00  14.00   0.75   25.00    --  -30.50  38.00-180.00  100
 16  ω     -2.00  19.00   0.75   25.00    --  -30.50 -97.00-143.00   28
 17  ω    -20.00   2.50   0.75   25.00    --  -30.50 -53.00  17.00   30
 18  ω     26.75  95.00   0.75   25.00    --   33.71-135.00-123.00   91
 19  ω     27.50  93.50   0.75   25.00    --   33.71-135.00  57.00   88
 20  ω     -9.00  42.00   0.75   25.00    --   33.71 -53.00-162.00   68
 21  ω     34.75  61.00   0.75   25.00    --   33.71 -67.00  23.00   35
 22  ω    -20.00   6.25   0.75   25.00    --   33.71   0.00-150.00   35
 23  ω    -11.00  23.50   0.75   25.00    --   33.71  39.00 -12.00   46
 24  ω     39.00  64.50   0.75   25.00    --   33.71 -97.00-143.00   34
 25  ω      2.00  28.25   0.75   25.00    --   33.71 -97.00-143.00   35
 26  ω     74.00  99.50   0.75   25.00    --   33.71 178.00  90.00   34
 27  ω    -19.00   7.25   0.75   25.00    --   33.71 -19.00-180.00   35
 28  ω      0.00  19.50   0.75   25.00    --   33.71  53.00 162.00   26
 29  ω    -20.00   5.50   0.75   25.00    --    0.00 -53.00  17.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0428164000
_diffrn_orient_matrix_UB_12      0.0134118000
_diffrn_orient_matrix_UB_13      0.0678619000
_diffrn_orient_matrix_UB_21      -0.0562690000
_diffrn_orient_matrix_UB_22      -0.0548028000
_diffrn_orient_matrix_UB_23      0.0006680000
_diffrn_orient_matrix_UB_31      0.0390634000
_diffrn_orient_matrix_UB_32      -0.0570027000
_diffrn_orient_matrix_UB_33      -0.0255352000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                569
_reflns_number_total             885
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.017(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         885
_refine_ls_number_restraints     421
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0949
_refine_ls_restrained_S_all      0.902
_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)+(0.0484P)²+46.0754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2567
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C3_$1-C3
 1.45 with sigma of 0.05
 C6_$2-C6
 1.45 with sigma of 0.05
 C9-C9_$3
 1.45 with sigma of 0.05
 C9-C8 \\sim C8-C7 \\sim C6-C5 \\sim C5-C4 \\sim C11-C10 \\sim C12-C11 \\sim
C2-C1 \\sim C3-C2
 with sigma of 0.02
 O4-N6 \\sim O6-N6 \\sim O5-N6 \\sim O1-N5 \\sim O2-N5 \\sim O3-N5
 with sigma of 0.02
 N2-C4 \\sim N3-C7 \\sim N1-C1 \\sim N4-C10
 with sigma of 0.05
 O1-N5 \\sim O3-N5 \\sim O2-N5 \\sim O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.05
 C9-C8 \\sim C8-C7 \\sim C2-C1 \\sim C3-C2 \\sim C11-C10 \\sim C12-C11 \\sim
C5-C4 \\sim C6-C5
 with sigma of 0.05
3. Rigid bond restraints
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C12 \\sim N4 \\sim C10 \\sim C11: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, O5, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C9, N3, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O2, N5, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
N2 N 0.678(6) 0.730(4) 0.201(9) 0.047(7) Uani 1 1 d D U . . .
H2A H 0.588137 0.670439 0.181726 0.056 Uiso 1 1 calc R U . . .
H2B H 0.692280 0.808105 0.279647 0.056 Uiso 1 1 calc R U . . .
N4 N 0.758(5) 0.480(3) 0.358(8) 0.05(2) Uani 1 1 d D U . . .
H4A H 0.822375 0.428145 0.385915 0.054 Uiso 1 1 calc R U . . .
H4B H 0.755451 0.554265 0.433355 0.054 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8660(7) 0.5942(4) 0.2405(11) 0.045(5) Uani 1 1 d . U . . .
C10 C 0.610(6) 0.381(4) 0.298(8) 0.05(2) Uani 1 1 d D U . . .
H10A H 0.611635 0.296499 0.218418 0.063 Uiso 1 1 calc R U . . .
H10B H 0.537835 0.435248 0.265115 0.063 Uiso 1 1 calc R U . . .
N1 N 1.043(5) 0.444(2) 0.237(8) 0.033(7) Uani 1 1 d D U . . .
H1A H 1.112977 0.476353 0.206151 0.040 Uiso 1 1 calc R U . . .
H1B H 1.089701 0.456192 0.322684 0.040 Uiso 1 1 calc R U . . .
O1 O 0.677(4) 0.422(2) 0.044(5) 0.051(7) Uani 1 1 d D U . . .
O2 O 0.857(4) 0.534(3) -0.002(6) 0.054(7) Uani 1 1 d D U . . .
N3 N 1.054(5) 0.793(3) 0.276(7) 0.032(7) Uani 1 1 d D U . . .
H3A H 1.056756 0.782032 0.193246 0.038 Uiso 1 1 calc R U . . .
H3B H 1.018735 0.875707 0.307313 0.038 Uiso 1 1 calc R U . . .
C11 C 0.551(6) 0.320(4) 0.385(7) 0.05(2) Uani 1 1 d D U . . .
H11A H 0.613371 0.253468 0.408271 0.060 Uiso 1 1 calc R U . . .
H11B H 0.447797 0.260185 0.334360 0.060 Uiso 1 1 calc R U . . .
C1 C 0.983(5) 0.284(3) 0.155(8) 0.036(7) Uani 1 1 d D U . . .
H1C H 0.927416 0.269471 0.062749 0.044 Uiso 1 1 calc R U . . .
H1D H 0.910695 0.245928 0.191885 0.044 Uiso 1 1 calc R U . . .
N5 N 0.716(4) 0.435(3) -0.065(5) 0.045(8) Uani 1 1 d D U . . .
C4 C 0.665(6) 0.786(4) 0.100(9) 0.042(7) Uani 1 1 d D U . . .
H4C H 0.614369 0.704470 0.010873 0.050 Uiso 1 1 calc R U . . .
H4D H 0.765981 0.826016 0.101727 0.050 Uiso 1 1 calc R U . . .
C7 C 1.211(5) 0.831(3) 0.360(8) 0.036(9) Uani 1 1 d D U . . .
H7A H 1.242282 0.736768 0.352391 0.043 Uiso 1 1 calc R U . . .
H7B H 1.215037 0.883215 0.454125 0.043 Uiso 1 1 calc R U . . .
C12 C 0.550(6) 0.442(4) 0.513(8) 0.05(2) Uani 1 1 d D U . . .
H12A H 0.654255 0.497469 0.566320 0.059 Uiso 1 1 calc R U . . .
H12B H 0.511738 0.396655 0.567074 0.059 Uiso 1 1 calc R U . . .
C2 C 1.101(5) 0.192(2) 0.150(7) 0.033(7) Uani 1 1 d D U . . .
H2C H 1.157365 0.209665 0.243431 0.040 Uiso 1 1 calc R U . . .
H2D H 1.172615 0.231480 0.113722 0.040 Uiso 1 1 calc R U . . .
O3 O 0.629(5) 0.424(3) -0.192(6) 0.053(7) Uani 1 1 d D U . . .
C5 C 0.578(5) 0.908(4) 0.118(6) 0.049(8) Uani 1 1 d D U . . .
H5A H 0.628419 0.990212 0.206692 0.059 Uiso 1 1 calc R U . . .
H5B H 0.476589 0.868495 0.116255 0.059 Uiso 1 1 calc R U . . .
C8 C 1.326(4) 0.924(3) 0.333(6) 0.046(9) Uani 1 1 d D U . . .
H8A H 1.298072 1.020141 0.342527 0.056 Uiso 1 1 calc R U . . .
H8B H 1.324325 0.873123 0.239310 0.056 Uiso 1 1 calc R U . . .
C3 C 1.052(4) 0.025(3) 0.070(3) 0.028(7) Uani 1 1 d D U . . .
H3C H 1.141980 -0.015455 0.065176 0.033 Uiso 1 1 calc R U . . .
H3D H 1.002773 -0.018550 0.119144 0.033 Uiso 1 1 calc R U . . .
C6 C 0.565(4) 0.965(4) 0.008(6) 0.043(8) Uani 1 1 d D U . . .
H6A H 0.657495 1.039327 0.031743 0.051 Uiso 1 1 calc R U . . .
H6B H 0.554741 0.882486 -0.076991 0.051 Uiso 1 1 calc R U . . .
C9 C 1.485(4) 0.954(3) 0.427(3) 0.036(8) Uani 1 1 d D U . . .
H9A H 1.510047 0.857495 0.417329 0.043 Uiso 1 1 calc R U . . .
H9B H 1.553214 1.004379 0.394843 0.043 Uiso 1 1 calc R U . . .
N6 N 0.993(4) 0.802(3) 0.544(6) 0.051(8) Uani 1 1 d D U . . .
O5 O 0.850(5) 0.821(3) 0.486(7) 0.069(10) Uani 1 1 d D U . . .
O4 O 0.999(6) 0.657(2) 0.460(8) 0.026(7) Uani 1 1 d D U . . .
O6 O 1.098(5) 0.919(3) 0.657(7) 0.076(10) Uani 1 1 d D U . . .


_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 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 Cd1 2.35(5) . ?
N2 C4 1.40(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.33(4) . ?
N4 C10 1.43(5) . ?
Cd1 N1 2.32(3) . ?
Cd1 O1 2.33(5) . ?
Cd1 O2 2.51(6) . ?
Cd1 N3 2.31(2) . ?
Cd1 O4 2.24(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.49(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.45(4) . ?
O1 N5 1.39(3) . ?
O2 N5 1.38(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.44(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.49(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.49(3) . ?
N5 O3 1.39(3) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.49(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.49(3) . ?
C12 C12 1.60(10) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.49(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.49(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.50(3) . ?
C3 C3 1.46(6) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.45(5) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.48(5) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N6 O5 1.38(3) . ?
N6 O4 1.40(3) . ?
N6 O6 1.39(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H2A N2 H2B 106.9 . . ?
Cd1 N2 H2A 107.4 . . ?
Cd1 N2 H2B 107.4 . . ?
C4 N2 H2A 107.4 . . ?
C4 N2 H2B 107.4 . . ?
C4 N2 Cd1 120(2) . . ?
H4A N4 H4B 106.6 . . ?
Cd1 N4 H4A 106.7 . . ?
Cd1 N4 H4B 106.7 . . ?
C10 N4 H4A 106.7 . . ?
C10 N4 H4B 106.7 . . ?
C10 N4 Cd1 122(4) . . ?
N2 Cd1 O2 86(2) . . ?
N4 Cd1 N2 96.6(15) . . ?
N4 Cd1 O1 86.1(19) . . ?
N4 Cd1 O2 137.4(17) . . ?
N1 Cd1 N2 170(3) . . ?
N1 Cd1 N4 89.6(13) . . ?
N1 Cd1 O1 96.5(17) . . ?
N1 Cd1 O2 84(2) . . ?
O1 Cd1 N2 75.7(19) . . ?
O1 Cd1 O2 53.3(12) . . ?
N3 Cd1 N2 91.1(12) . . ?
N3 Cd1 N4 142(2) . . ?
N3 Cd1 N1 89.2(9) . . ?
N3 Cd1 O1 132(2) . . ?
N3 Cd1 O2 80.5(18) . . ?
O4 Cd1 N2 116(2) . . ?
O4 Cd1 N4 63.3(18) . . ?
O4 Cd1 N1 74.3(19) . . ?
O4 Cd1 O1 147.7(11) . . ?
O4 Cd1 O2 150.2(10) . . ?
O4 Cd1 N3 79.4(19) . . ?
N4 C10 H10A 108.0 . . ?
N4 C10 H10B 108.0 . . ?
N4 C10 C11 117(4) . . ?
H10A C10 H10B 107.2 . . ?
C11 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
Cd1 N1 H1A 108.4 . . ?
Cd1 N1 H1B 108.4 . . ?
H1A N1 H1B 107.4 . . ?
C1 N1 Cd1 116(3) . . ?
C1 N1 H1A 108.4 . . ?
C1 N1 H1B 108.4 . . ?
N5 O1 Cd1 105.8(19) . . ?
N5 O2 Cd1 97(2) . . ?
Cd1 N3 H3A 105.5 . . ?
Cd1 N3 H3B 105.5 . . ?
H3A N3 H3B 106.1 . . ?
C7 N3 Cd1 127(3) . . ?
C7 N3 H3A 105.5 . . ?
C7 N3 H3B 105.5 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C10 C11 C12 112(3) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
N1 C1 H1C 108.8 . . ?
N1 C1 H1D 108.8 . . ?
N1 C1 C2 114(4) . . ?
H1C C1 H1D 107.7 . . ?
C2 C1 H1C 108.8 . . ?
C2 C1 H1D 108.8 . . ?
O2 N5 O1 103(3) . . ?
O2 N5 O3 119(4) . . ?
O3 N5 O1 132(4) . . ?
N2 C4 H4C 109.2 . . ?
N2 C4 H4D 109.2 . . ?
N2 C4 C5 112(4) . . ?
H4C C4 H4D 107.9 . . ?
C5 C4 H4C 109.2 . . ?
C5 C4 H4D 109.2 . . ?
N3 C7 H7A 107.6 . . ?
N3 C7 H7B 107.6 . . ?
N3 C7 C8 119(5) . . ?
H7A C7 H7B 107.0 . . ?
C8 C7 H7A 107.6 . . ?
C8 C7 H7B 107.6 . . ?
C11 C12 C12 113(7) . 2_666 ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C12 C12 H12A 108.9 2_666 . ?
C12 C12 H12B 108.9 2_666 . ?
H12A C12 H12B 107.7 . . ?
C1 C2 H2C 107.7 . . ?
C1 C2 H2D 107.7 . . ?
C1 C2 C3 118(3) . . ?
H2C C2 H2D 107.1 . . ?
C3 C2 H2C 107.7 . . ?
C3 C2 H2D 107.7 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 C6 111(4) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C7 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
C7 C8 C9 113(4) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C2 C3 H3C 108.3 . . ?
C2 C3 H3D 108.3 . . ?
C3 C3 C2 116(5) 2_755 . ?
C3 C3 H3C 108.3 2_755 . ?
C3 C3 H3D 108.3 2_755 . ?
H3C C3 H3D 107.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C6 C6 C5 111(5) 2_675 . ?
C6 C6 H6A 109.5 2_675 . ?
C6 C6 H6B 109.5 2_675 . ?
H6A C6 H6B 108.1 . . ?
C8 C9 H9A 107.9 . . ?
C8 C9 H9B 107.9 . . ?
C9 C9 C8 118(4) 2_876 . ?
C9 C9 H9A 107.9 2_876 . ?
C9 C9 H9B 107.9 2_876 . ?
H9A C9 H9B 107.2 . . ?
O5 N6 O4 105(4) . . ?
O5 N6 O6 121(3) . . ?
O6 N6 O4 134(4) . . ?
N6 O4 Cd1 112(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 C4 C5 C6 -180(3) . . . . ?
N4 C10 C11 C12 55(4) . . . . ?
Cd1 N2 C4 C5 -162(4) . . . . ?
Cd1 N4 C10 C11 -178(2) . . . . ?
Cd1 N1 C1 C2 177(4) . . . . ?
Cd1 O1 N5 O2 6(3) . . . . ?
Cd1 O1 N5 O3 -145(3) . . . . ?
Cd1 O2 N5 O1 -5(3) . . . . ?
Cd1 O2 N5 O3 151(3) . . . . ?
Cd1 N3 C7 C8 158(3) . . . . ?
C10 C11 C12 C12 59(4) . . . 2_666 ?
N1 C1 C2 C3 179(5) . . . . ?
N3 C7 C8 C9 -180(3) . . . . ?
C1 C2 C3 C3 50(7) . . . 2_755 ?
C4 C5 C6 C6 157(5) . . . 2_675 ?
C7 C8 C9 C9 -65(5) . . . 2_876 ?
O5 N6 O4 Cd1 34(3) . . . . ?
O6 N6 O4 Cd1 -143(4) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.935
_oxdiff_exptl_absorpt_empirical_full_min 0.678
####################################################################### 
# 
# 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_1_96_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262347'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_96_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.346 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_96_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.80 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC, 
particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_1_96_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.06583 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_1_96_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1884 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12 H32 N6 O6'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.2950(18)
_cell_length_b                   9.6793(19)
_cell_length_c                   10.957(3)
_cell_angle_alpha                110.80(2)
_cell_angle_beta                 104.87(2)
_cell_angle_gamma                96.250(16)
_cell_volume                     868.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2350
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5810
_cell_measurement_theta_min      2.2890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 8 0.0485
2 13 -4 0.0555
9 -10 -4 0.0737
9 9 -7 0.0399
-10 -7 8 0.0309
10 7 -8 0.0309
-1 -13 3 0.0820
5 -4 13 0.0325
-5 4 -13 0.0325

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.4436 -1.8942 7.9175 -0.0181 0.8138 -0.5809
2.3073 12.8245 -3.7568 0.0208 -0.8368 -0.5471
9.0851 -9.5860 -3.7681 -0.0022 0.0091 1.0000
8.5173 9.3412 -6.8699 0.0254 -0.9994 -0.0254
-10.2704 -7.1842 7.9163 0.0012 0.9811 -0.1932
10.2704 7.1842 -7.9163 -0.0012 -0.9811 0.1932
-0.9138 -13.0475 2.6288 -0.0414 0.7692 0.6431
4.5548 -4.3113 12.5413 0.9942 -0.0058 0.1076
-4.5548 4.3113 -12.5413 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.346
_diffrn_reflns_Laue_measured_fraction_max 0.199
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5986
_diffrn_reflns_point_group_measured_fraction_full 0.346
_diffrn_reflns_point_group_measured_fraction_max 0.199
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.308
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.346
_diffrn_measured_fraction_theta_max 0.199
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.96(2) GPa
 (1960000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     57.00  88.50   0.75   13.50    --    0.00-178.00 -90.00   42
  2  ω    -61.00  14.00   0.75   13.50    --  -30.50  67.00 -23.00  100
  3  ω   -109.00 -73.00   0.75   13.50    --  -30.50 178.00  90.00   48
  4  ω    -95.00 -20.00   0.75   13.50    --  -30.50 135.00 123.00  100
  5  ω    -50.00  25.00   0.75   13.50    --  -30.50  19.00-180.00  100
  6  ω    -30.00  39.00   0.75   13.50    --  -30.50 -26.00   8.00   92
  7  ω     -2.00  19.00   0.75   13.50    --  -30.50 -97.00  35.00   28
  8  ω    -26.00   1.00   0.75   13.50    --  -30.50 -57.00  30.00   36
  9  ω    -50.00  25.00   0.75   13.50    --  -30.50  39.00 -12.00  100
 10  ω    -20.00   2.50   0.75   13.50    --  -30.50 -53.00-162.00   30
 11  ω    -20.00   2.50   0.75   13.50    --  -30.50 -53.00  17.00   30
 12  ω    -42.00  33.00   0.75   13.50    --  -30.50  13.00 176.00  100
 13  ω    -30.00  39.00   0.75   13.50    --  -30.50 -26.00-171.00   92
 14  ω   -117.00 -72.00   0.75   13.50    --  -30.50 178.00 -90.00   60
 15  ω    -61.00  14.00   0.75   13.50    --  -30.50  38.00-180.00  100
 16  ω    -37.00  36.50   0.75   13.50    --  -30.50   0.00-180.00   98
 17  ω     -8.00  61.00   0.75   13.50    --   33.71 -67.00-157.00   92
 18  ω     26.75  95.00   0.75   13.50    --   33.71-135.00-123.00   91
 19  ω     27.50  95.00   0.75   13.50    --   33.71-135.00  57.00   90
 20  ω    -36.00  33.00   0.75   13.50    --   33.71  13.00  -3.00   92
 21  ω      0.00  19.50   0.75   13.50    --   33.71  53.00 162.00   26
 22  ω    -35.00 -12.50   0.75   13.50    --    0.00  77.00 -30.00   30
 23  ω      7.00  29.50   0.75   13.50    --  -30.50-114.00  45.00   30
 24  ω      7.00  29.50   0.75   13.50    --  -30.50-114.00-135.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0429069000
_diffrn_orient_matrix_UB_12      0.0139675000
_diffrn_orient_matrix_UB_13      0.0684903000
_diffrn_orient_matrix_UB_21      -0.0563193000
_diffrn_orient_matrix_UB_22      -0.0547784000
_diffrn_orient_matrix_UB_23      0.0011609000
_diffrn_orient_matrix_UB_31      0.0392693000
_diffrn_orient_matrix_UB_32      -0.0571430000
_diffrn_orient_matrix_UB_33      -0.0253225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                558
_reflns_number_total             858
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         858
_refine_ls_number_restraints     386
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0888
_refine_ls_restrained_S_all      0.958
_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)+(0.1004P)²+31.4968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2706
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C12_$1-C12
 1.45 with sigma of 0.05
 C9_$2-C9
 1.45 with sigma of 0.05
 C6_$3-C6
 1.45 with sigma of 0.05
 C3-C3_$4
 1.45 with sigma of 0.05
 H6B_$5-H10A
 2.05 with sigma of 0.02
 C7-N3
 1.4 with sigma of 0.02
 O1-N5 \\sim O2-N5 \\sim O3-N5
 with sigma of 0.08
 C11-C10 \\sim C12-C11 \\sim C5-C4 \\sim C6-C5 \\sim C3-C2 \\sim C2-C1 \\sim
C9-C8 \\sim C8-C7
 with sigma of 0.08
 O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.08
 N4-C10 \\sim N2-C4 \\sim N1-C1 \\sim N3-C7
 with sigma of 0.08
3. Rigid bond restraints
 O1, O2, N5, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, O5, O4, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim N5 \\sim O3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N6 \\sim O5 \\sim O4 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(N6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O2, N5, O3, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, N6, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C11, C10, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N5, O2, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C10(H10A,H10B), N1(H1A,H1B), N3(H3A,H3B), C11(H11A,
 H11B), C1(H1C,H1D), C4(H4C,H4D), C7(H7A,H7B), C12(H12A,H12B), C2(H2C,H2D),
 C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B), C9(H9A,H9B)
;
_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
N2 N 0.694(6) 0.737(4) 0.230(9) 0.048(8) Uani 1 1 d D U . . .
H2A H 0.603610 0.682919 0.217036 0.058 Uiso 1 1 calc R U . . .
H2B H 0.719613 0.815697 0.310851 0.058 Uiso 1 1 calc R U . . .
N4 N 0.756(5) 0.476(3) 0.355(8) 0.05(2) Uani 1 1 d D U . . .
H4A H 0.821043 0.423949 0.382322 0.065 Uiso 1 1 calc R U . . .
H4B H 0.753049 0.549386 0.430406 0.065 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8666(7) 0.5933(4) 0.2415(11) 0.043(5) Uani 1 1 d . U . . .
C10 C 0.611(4) 0.378(4) 0.294(6) 0.049(15) Uani 1 1 d D U . . .
H10A H 0.613485 0.292193 0.214682 0.059 Uiso 1 1 calc DR U . . .
H10B H 0.538196 0.430804 0.259287 0.059 Uiso 1 1 calc R U . . .
N1 N 1.041(5) 0.445(2) 0.234(8) 0.031(7) Uani 1 1 d D U . . .
H1A H 1.110035 0.479268 0.202324 0.037 Uiso 1 1 calc R U . . .
H1B H 1.088858 0.457089 0.319767 0.037 Uiso 1 1 calc R U . . .
O1 O 0.666(5) 0.414(3) 0.023(8) 0.055(7) Uani 1 1 d D U . . .
O2 O 0.858(5) 0.531(3) -0.002(7) 0.053(7) Uani 1 1 d D U . . .
N3 N 1.050(5) 0.794(2) 0.271(7) 0.030(6) Uani 1 1 d D U . . .
H3A H 1.052595 0.782230 0.186889 0.036 Uiso 1 1 calc R U . . .
H3B H 1.015465 0.877270 0.302393 0.036 Uiso 1 1 calc R U . . .
C11 C 0.552(6) 0.318(3) 0.384(7) 0.039(9) Uani 1 1 d D U . . .
H11A H 0.617192 0.255230 0.410739 0.047 Uiso 1 1 calc R U . . .
H11B H 0.450142 0.255041 0.332371 0.047 Uiso 1 1 calc R U . . .
C1 C 0.981(6) 0.284(3) 0.150(9) 0.033(7) Uani 1 1 d D U . . .
H1C H 0.930236 0.269528 0.056085 0.039 Uiso 1 1 calc R U . . .
H1D H 0.905255 0.245602 0.184040 0.039 Uiso 1 1 calc R U . . .
N5 N 0.719(5) 0.441(4) -0.065(6) 0.046(7) Uani 1 1 d D U . . .
C4 C 0.680(6) 0.791(4) 0.127(9) 0.050(14) Uani 1 1 d D U . . .
H4C H 0.638668 0.705028 0.039435 0.060 Uiso 1 1 calc R U . . .
H4D H 0.781929 0.835721 0.133769 0.060 Uiso 1 1 calc R U . . .
C7 C 1.202(5) 0.826(3) 0.353(7) 0.039(7) Uani 1 1 d D U . . .
H7A H 1.231342 0.731310 0.344962 0.047 Uiso 1 1 calc R U . . .
H7B H 1.207514 0.880205 0.447945 0.047 Uiso 1 1 calc R U . . .
C12 C 0.547(4) 0.446(3) 0.512(6) 0.037(16) Uani 1 1 d D U . . .
H12A H 0.508175 0.401005 0.566813 0.044 Uiso 1 1 calc R U . . .
H12B H 0.650610 0.502241 0.565932 0.044 Uiso 1 1 calc R U . . .
C2 C 1.104(6) 0.195(3) 0.153(9) 0.031(7) Uani 1 1 d D U . . .
H2C H 1.158995 0.215385 0.247719 0.037 Uiso 1 1 calc R U . . .
H2D H 1.175722 0.229236 0.113567 0.037 Uiso 1 1 calc R U . . .
O3 O 0.631(6) 0.423(3) -0.188(8) 0.054(6) Uani 1 1 d D U . . .
C5 C 0.582(6) 0.908(4) 0.127(8) 0.048(8) Uani 1 1 d D U . . .
H5A H 0.622667 0.994027 0.215391 0.057 Uiso 1 1 calc R U . . .
H5B H 0.479493 0.863267 0.120172 0.057 Uiso 1 1 calc R U . . .
C8 C 1.321(5) 0.922(3) 0.320(8) 0.041(7) Uani 1 1 d D U . . .
H8A H 1.292245 1.016310 0.325254 0.050 Uiso 1 1 calc R U . . .
H8B H 1.322063 0.866576 0.227331 0.050 Uiso 1 1 calc R U . . .
C3 C 1.041(5) 0.021(4) 0.072(3) 0.032(7) Uani 1 1 d D U . . .
H3C H 1.125550 -0.029659 0.078856 0.038 Uiso 1 1 calc R U . . .
H3D H 0.973440 -0.014466 0.114218 0.038 Uiso 1 1 calc R U . . .
C6 C 0.568(3) 0.968(3) 0.009(6) 0.045(8) Uani 1 1 d D U . . .
H6A H 0.658445 1.046129 0.033599 0.053 Uiso 1 1 calc R U . . .
H6B H 0.561465 0.886208 -0.076212 0.053 Uiso 1 1 calc R U . . .
C9 C 1.487(4) 0.956(3) 0.426(3) 0.037(7) Uani 1 1 d D U . . .
H9A H 1.514908 0.859901 0.416088 0.044 Uiso 1 1 calc R U . . .
H9B H 1.557880 1.010212 0.397979 0.044 Uiso 1 1 calc R U . . .
N6 N 0.985(5) 0.801(3) 0.538(7) 0.047(7) Uani 1 1 d D U . . .
O5 O 0.858(7) 0.827(4) 0.500(10) 0.080(11) Uani 1 1 d D U . . .
O4 O 0.994(6) 0.656(3) 0.452(9) 0.029(7) Uani 1 1 d D U . . .
O6 O 1.091(6) 0.918(3) 0.644(9) 0.075(9) Uani 1 1 d D U . . .


_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 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 Cd1 2.24(4) . ?
N2 C4 1.38(7) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.30(4) . ?
N4 C10 1.41(5) . ?
Cd1 N1 2.27(3) . ?
Cd1 O1 2.51(7) . ?
Cd1 O2 2.49(7) . ?
Cd1 N3 2.31(2) . ?
Cd1 O4 2.13(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.49(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.46(5) . ?
O1 N5 1.28(6) . ?
O2 N5 1.33(6) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.39(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.52(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.51(5) . ?
N5 O3 1.32(7) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.53(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.55(4) . ?
C12 C12 1.49(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.56(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.58(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.59(6) . ?
C3 C3 1.45(6) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.47(5) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.48(5) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N6 O5 1.23(6) . ?
N6 O4 1.41(4) . ?
N6 O6 1.35(6) . ?

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
H2A N2 H2B 107.6 . . ?
Cd1 N2 H2A 108.6 . . ?
Cd1 N2 H2B 108.6 . . ?
C4 N2 H2A 108.6 . . ?
C4 N2 H2B 108.6 . . ?
C4 N2 Cd1 115(3) . . ?
H4A N4 H4B 106.5 . . ?
Cd1 N4 H4A 106.5 . . ?
Cd1 N4 H4B 106.5 . . ?
C10 N4 H4A 106.5 . . ?
C10 N4 H4B 106.5 . . ?
C10 N4 Cd1 123(5) . . ?
N2 Cd1 N4 93.5(16) . . ?
N2 Cd1 N1 175(3) . . ?
N2 Cd1 O1 81(2) . . ?
N2 Cd1 O2 93(2) . . ?
N2 Cd1 N3 88.7(11) . . ?
N4 Cd1 O1 87(2) . . ?
N4 Cd1 O2 135.7(17) . . ?
N4 Cd1 N3 144(2) . . ?
N1 Cd1 N4 90.4(13) . . ?
N1 Cd1 O1 96.4(18) . . ?
N1 Cd1 O2 82(2) . . ?
N1 Cd1 N3 89.9(9) . . ?
O2 Cd1 O1 50.7(13) . . ?
N3 Cd1 O1 128(2) . . ?
N3 Cd1 O2 79.6(17) . . ?
O4 Cd1 N2 109(2) . . ?
O4 Cd1 N4 65.1(19) . . ?
O4 Cd1 N1 76(2) . . ?
O4 Cd1 O1 150.9(13) . . ?
O4 Cd1 O2 150.0(11) . . ?
O4 Cd1 N3 80.6(17) . . ?
N4 C10 H10A 108.2 . . ?
N4 C10 H10B 108.2 . . ?
N4 C10 C11 116(5) . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
Cd1 N1 H1A 108.3 . . ?
Cd1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C1 N1 Cd1 116(3) . . ?
C1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
N5 O1 Cd1 100(3) . . ?
N5 O2 Cd1 99(3) . . ?
Cd1 N3 H3A 106.4 . . ?
Cd1 N3 H3B 106.4 . . ?
H3A N3 H3B 106.5 . . ?
C7 N3 Cd1 124(2) . . ?
C7 N3 H3A 106.4 . . ?
C7 N3 H3B 106.4 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C10 C11 C12 112(3) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
N1 C1 H1C 109.1 . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 C2 112(4) . . ?
H1C C1 H1D 107.9 . . ?
C2 C1 H1C 109.1 . . ?
C2 C1 H1D 109.1 . . ?
O1 N5 O2 110(6) . . ?
O1 N5 O3 123(5) . . ?
O3 N5 O2 124(5) . . ?
N2 C4 H4C 108.0 . . ?
N2 C4 H4D 108.0 . . ?
N2 C4 C5 117(4) . . ?
H4C C4 H4D 107.3 . . ?
C5 C4 H4C 108.0 . . ?
C5 C4 H4D 108.0 . . ?
N3 C7 H7A 108.2 . . ?
N3 C7 H7B 108.2 . . ?
N3 C7 C8 117(4) . . ?
H7A C7 H7B 107.3 . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
C11 C12 H12A 108.3 . . ?
C11 C12 H12B 108.3 . . ?
C12 C12 C11 116(6) 2_666 . ?
C12 C12 H12A 108.3 2_666 . ?
C12 C12 H12B 108.3 2_666 . ?
H12A C12 H12B 107.4 . . ?
C1 C2 H2C 108.9 . . ?
C1 C2 H2D 108.9 . . ?
C1 C2 C3 113(4) . . ?
H2C C2 H2D 107.8 . . ?
C3 C2 H2C 108.9 . . ?
C3 C2 H2D 108.9 . . ?
C4 C5 H5A 108.3 . . ?
C4 C5 H5B 108.3 . . ?
C4 C5 C6 116(4) . . ?
H5A C5 H5B 107.4 . . ?
C6 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C7 C8 C9 111(5) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C2 C3 H3C 109.0 . . ?
C2 C3 H3D 109.0 . . ?
C3 C3 C2 113(5) 2_755 . ?
C3 C3 H3C 109.0 2_755 . ?
C3 C3 H3D 109.0 2_755 . ?
H3C C3 H3D 107.8 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
C6 C6 C5 109(4) 2_675 . ?
C6 C6 H6A 109.9 2_675 . ?
C6 C6 H6B 109.9 2_675 . ?
H6A C6 H6B 108.3 . . ?
C8 C9 H9A 107.7 . . ?
C8 C9 H9B 107.7 . . ?
C9 C9 C8 118(3) 2_876 . ?
C9 C9 H9A 107.7 2_876 . ?
C9 C9 H9B 107.7 2_876 . ?
H9A C9 H9B 107.1 . . ?
O5 N6 O4 112(5) . . ?
O5 N6 O6 115(4) . . ?
O6 N6 O4 133(4) . . ?
N6 O4 Cd1 113(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 180(4) . . . . ?
N4 C10 C11 C12 57(5) . . . . ?
Cd1 N2 C4 C5 -172(4) . . . . ?
Cd1 N4 C10 C11 -177(2) . . . . ?
Cd1 N1 C1 C2 -179(4) . . . . ?
Cd1 O1 N5 O2 8(3) . . . . ?
Cd1 O1 N5 O3 -152(3) . . . . ?
Cd1 O2 N5 O1 -8(3) . . . . ?
Cd1 O2 N5 O3 152(3) . . . . ?
Cd1 N3 C7 C8 158(3) . . . . ?
C10 C11 C12 C12 58(5) . . . 2_666 ?
N1 C1 C2 C3 176(5) . . . . ?
N3 C7 C8 C9 177(2) . . . . ?
C1 C2 C3 C3 60(7) . . . 2_755 ?
C4 C5 C6 C6 159(5) . . . 2_675 ?
C7 C8 C9 C9 -61(5) . . . 2_876 ?
O5 N6 O4 Cd1 36(4) . . . . ?
O6 N6 O4 Cd1 -138(5) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999965 0.00000000 -0.00083793
omega rotation goniometer -1 . -0.71101000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.56449000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.124
_oxdiff_exptl_absorpt_empirical_full_min 0.750
####################################################################### 
# 
# 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_2_8_GPa_Cd_HDA_2_NO3_2

_database_code_depnum_ccdc_archive 'CCDC 2262351'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form
_audit_creation_date             2023-05-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N3 O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H32CdN6O6
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'
Cd Cd -0.8075 1.2024 '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      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                   9.188(2)
_cell_length_b                   9.5899(16)
_cell_length_c                   10.926(4)
_cell_angle_alpha                110.87(2)
_cell_angle_beta                 106.04(3)
_cell_angle_gamma                97.405(17)
_cell_volume                     836.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3100
_cell_measurement_theta_min      2.3370
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.793
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.94686
_exptl_absorpt_correction_T_min  0.94686
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 8 0.0485
2 13 -4 0.0555
9 -10 -4 0.0737
8 9 -7 0.0399
-10 -7 9 0.0309
10 7 -9 0.0309
-1 -13 3 0.0820
5 -4 12 0.0325
-5 4 -12 0.0325

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.2356 -1.7297 8.3948 -0.0181 0.8138 -0.5809
2.1251 12.7388 -4.3085 0.0208 -0.8368 -0.5471
9.0595 -9.6576 -3.7092 -0.0022 0.0091 1.0000
8.2824 9.1936 -7.4961 0.0254 -0.9994 -0.0254
-10.0313 -7.0155 8.5091 0.0012 0.9811 -0.1932
10.0313 7.0155 -8.5091 -0.0012 -0.9811 0.1932
-0.7522 -12.9857 3.1523 -0.0414 0.7692 0.6431
4.6429 -4.0134 12.1420 0.9942 -0.0058 0.1076
-4.6429 4.0134 -12.1420 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.342
_diffrn_reflns_Laue_measured_fraction_max 0.199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5631
_diffrn_reflns_point_group_measured_fraction_full 0.342
_diffrn_reflns_point_group_measured_fraction_max 0.199
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_min         2.349
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.342
_diffrn_measured_fraction_theta_max 0.199
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 2.80(2) GPa
 (2800000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  45.00   0.75   30.00    --  -24.60 -26.00   8.00  100
  2  ω   -109.00 -73.00   0.75   30.00    --  -24.60 178.00  90.00   48
  3  ω      7.00  35.50   0.75   30.00    --  -24.60-114.00  45.00   38
  4  ω   -115.00 -71.50   0.75   30.00    --  -24.60-178.00 -90.00   58
  5  ω    -57.00   1.50   0.75   30.00    --  -24.60  57.00-180.00   78
  6  ω    -20.00   8.50   0.75   30.00    --  -24.60 -53.00  17.00   38
  7  ω    -20.00   8.50   0.75   30.00    --  -24.60 -53.00-162.00   38
  8  ω    -57.00 -37.50   0.75   30.00    --  -24.60  57.00-150.00   26
  9  ω    -35.00 -12.50   0.75   30.00    --  -24.60  77.00 150.00   30
 10  ω    -25.00  21.50   0.75   30.00    --  -24.60 -39.00-167.00   62
 11  ω     71.00 107.00   0.75   30.00    --   25.46 178.00  90.00   48
 12  ω    -10.00  59.00   0.75   30.00    --   25.46 -67.00-157.00   92
 13  ω     32.00  95.00   0.75   30.00    --   25.46-135.00-123.00   84
 14  ω     61.00 108.25   0.75   30.00    --   25.46-178.00 -90.00   63
 15  ω    -17.50  50.00   0.75   30.00    --   25.46 -19.00-180.00   90
 16  ω    -27.00  45.00   0.75   30.00    --   25.46 -26.00-171.00   96
 17  ω     20.00  45.50   0.75   30.00    --  -24.60-135.00  57.00   34
 18  ω    -37.00  36.50   0.75   30.00    --  -24.60   0.00-180.00   98
 19  ω     20.00  47.00   0.75   30.00    --  -24.60-135.00-123.00   36
 20  ω    -35.00 -12.50   0.75   30.00    --  -24.60  77.00 120.00   30
 21  ω    -55.00  20.00   0.75   30.00    --  -24.60  53.00 -17.00  100
 22  ω     -2.00  25.00   0.75   30.00    --  -24.60 -97.00  35.00   36
 23  ω     -9.00  16.50   0.75   30.00    --  -24.60 -81.00-151.00   34
 24  ω    -22.50  45.00   0.75   30.00    --   25.46 -26.00   8.00   90
 25  ω    -25.00   2.00   0.75   30.00    --   25.46  97.00 -35.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0468509000
_diffrn_orient_matrix_UB_12      0.0173973000
_diffrn_orient_matrix_UB_13      0.0697140000
_diffrn_orient_matrix_UB_21      -0.0566837000
_diffrn_orient_matrix_UB_22      -0.0552404000
_diffrn_orient_matrix_UB_23      0.0029382000
_diffrn_orient_matrix_UB_31      0.0385160000
_diffrn_orient_matrix_UB_32      -0.0578184000
_diffrn_orient_matrix_UB_33      -0.0249734000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                584
_reflns_number_total             788
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.024(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         788
_refine_ls_number_restraints     363
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.1094
_refine_ls_restrained_S_all      0.872
_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)+(0.1520P)²+42.9730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2692
_refine_ls_wR_factor_ref         0.3037
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H5A(0.093) H5(0.093) H4A(0.061) H4B(0.061) H2A(0.038) H2B(0.038)
 H6A(0.127) H6B(0.127) H2C(0.047) H2D(0.047) H1A(0.044) H1B(0.044) H1C(0.027)
 H1D(0.027) H12A(0.054) H12B(0.054) H11A(0.059) H11B(0.059) H4C(0.062)
 H4(0.062) H7A(0.027) H7B(0.027) H3A(0.035) H3B(0.035) H9A(0.027) H9B(0.027)
 H3C(0.03) H3D(0.03) H10A(0.049) H10B(0.049) H8A(0.029) H8B(0.029)
 Fixed X: H5A(0.698439) H5(0.525109) H4A(0.605373) H4B(0.595256) H2A(1.147397)
 H2B(1.181685) H6A(0.644782) H6B(0.511524) H2C(0.586575) H2D(0.718158)
 H1A(1.0865) H1B(1.044017) H1C(0.914949) H1D(0.87891) H12A(0.384351)
 H12B(0.38846) H11A(0.461505) H11B(0.548084) H4C(0.576436) H4(0.754837)
 H7A(1.235468) H7B(1.204376) H3A(1.115012) H3B(0.950873) H9A(1.519523)
 H9B(1.558108) H3C(1.058054) H3D(1.013741) H10A(0.755186) H10B(0.739773)
 H8A(1.287685) H8B(1.314568)
 Fixed Y: H5A(1.008845) H5(0.917081) H4A(0.526853) H4B(0.391456) H2A(0.212804)
 H2B(0.245167) H6A(1.01741) H6B(0.860497) H2C(0.711413) H2D(0.843393)
 H1A(0.479122) H1B(0.447984) H1C(0.259069) H1D(0.224085) H12A(0.443165)
 H12B(0.383188) H11A(0.235963) H11B(0.240404) H4C(0.691184) H4(0.783727)
 H7A(0.730243) H7B(0.887207) H3A(-0.029916) H3B(-0.018414) H9A(0.860035)
 H9B(1.011154) H3C(0.745829) H3D(0.864881) H10A(0.447736) H10B(0.29711)
 H8A(1.002223) H8B(0.845085)
 Fixed Z: H5A(0.189297) H5(0.151031) H4A(0.318251) H4B(0.202547) H2A(0.271489)
 H2B(0.149141) H6A(-0.027899) H6B(-0.102767) H2C(0.197868) H2D(0.270396)
 H1A(0.228216) H1B(0.333692) H1C(0.060481) H1D(0.180345) H12A(0.372792)
 H12B(0.488434) H11A(0.287466) H11B(0.434965) H4C(-0.01013) H4(0.049063)
 H7A(0.370528) H7B(0.457056) H3A(0.092163) H3B(0.103201) H9A(0.421015)
 H9B(0.399304) H3C(0.173462) H3D(0.26796) H10A(0.472408) H10B(0.343925)
 H8A(0.317415) H8B(0.227282)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C5 C 0.611(9) 0.926(5) 0.117(13) 0.077(12) Uani 1 1 d D U . . .
H5A H 0.698439 1.008845 0.189297 0.093 Uiso 1 1 calc R U . A 1
H5 H 0.525109 0.917081 0.151031 0.093 Uiso 1 1 calc R U . A 1
N4 N 0.660(5) 0.461(4) 0.286(7) 0.051(7) Uani 1 1 d D U . . .
H4A H 0.605373 0.526853 0.318251 0.061 Uiso 1 1 calc R U . . .
H4B H 0.595256 0.391456 0.202547 0.061 Uiso 1 1 calc R U . . .
C2 C 1.102(6) 0.199(3) 0.175(9) 0.032(8) Uani 1 1 d D U . . .
H2A H 1.147397 0.212804 0.271489 0.038 Uiso 1 1 calc R U . . .
H2B H 1.181685 0.245167 0.149141 0.038 Uiso 1 1 calc R U . . .
C6 C 0.559(8) 0.955(7) -0.019(13) 0.106(16) Uani 1 1 d D U . . .
H6A H 0.644782 1.017410 -0.027899 0.127 Uiso 1 1 calc R U . . .
H6B H 0.511524 0.860497 -0.102767 0.127 Uiso 1 1 calc R U . . .
O6 O 1.080(5) 0.907(3) 0.641(6) 0.047(8) Uani 1 1 d D U . . .
N2 N 0.680(6) 0.751(4) 0.199(9) 0.039(10) Uani 1 1 d D . . . .
H2C H 0.586575 0.711413 0.197868 0.047 Uiso 1 1 calc R U . . .
H2D H 0.718158 0.843393 0.270396 0.047 Uiso 1 1 calc R U . . .
N1 N 1.006(6) 0.439(3) 0.246(9) 0.037(7) Uani 1 1 d D U . . .
H1A H 1.086500 0.479122 0.228216 0.044 Uiso 1 1 calc R U . . .
H1B H 1.044017 0.447984 0.333692 0.044 Uiso 1 1 calc R U . . .
C1 C 0.959(6) 0.275(3) 0.157(8) 0.022(7) Uani 1 1 d D U . . .
H1C H 0.914949 0.259069 0.060481 0.027 Uiso 1 1 calc R U . . .
H1D H 0.878910 0.224085 0.180345 0.027 Uiso 1 1 calc R U . . .
C12 C 0.454(4) 0.426(3) 0.448(5) 0.045(10) Uani 1 1 d D U . . .
H12A H 0.384351 0.443165 0.372792 0.054 Uiso 1 1 calc R U . . .
H12B H 0.388460 0.383188 0.488434 0.054 Uiso 1 1 calc R U . . .
O1 O 0.665(4) 0.416(3) -0.003(6) 0.046(4) Uani 1 1 d D U . . .
N6 N 0.963(5) 0.813(3) 0.539(7) 0.037(7) Uani 1 1 d D U . . .
N5 N 0.718(4) 0.446(4) -0.089(5) 0.046(4) Uani 1 1 d D U . . .
O4 O 0.972(5) 0.670(3) 0.469(8) 0.035(6) Uani 1 1 d D U . . .
C11 C 0.531(9) 0.303(5) 0.382(13) 0.049(9) Uani 1 1 d D U . . .
H11A H 0.461505 0.235963 0.287466 0.059 Uiso 1 1 calc R U . . .
H11B H 0.548084 0.240404 0.434965 0.059 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8439(8) 0.5939(4) 0.2448(11) 0.041(5) Uani 1 1 d . U . . .
C4 C 0.659(6) 0.773(4) 0.069(7) 0.052(15) Uani 1 1 d D . . . .
H4C H 0.576436 0.691184 -0.010130 0.062 Uiso 1 1 calc R U . . .
H4 H 0.754837 0.783727 0.049063 0.062 Uiso 1 1 calc R U . . .
C7 C 1.205(6) 0.822(4) 0.366(8) 0.022(6) Uani 1 1 d D U . . .
H7A H 1.235468 0.730243 0.370528 0.027 Uiso 1 1 calc R U . . .
H7B H 1.204376 0.887207 0.457056 0.027 Uiso 1 1 calc R U . . .
O3 O 0.631(4) 0.429(3) -0.205(5) 0.046(4) Uani 1 1 d D U . . .
C3 C 1.033(4) 0.022(4) 0.075(3) 0.029(8) Uani 1 1 d D U . . .
H3A H 1.115012 -0.029916 0.092163 0.035 Uiso 1 1 calc R U . . .
H3B H 0.950873 -0.018414 0.103201 0.035 Uiso 1 1 calc R U . . .
C9 C 1.488(3) 0.954(3) 0.4275(16) 0.023(7) Uani 1 1 d D U . . .
H9A H 1.519523 0.860035 0.421015 0.027 Uiso 1 1 calc R U . . .
H9B H 1.558108 1.011154 0.399304 0.027 Uiso 1 1 calc R U . . .
N3 N 1.046(6) 0.779(3) 0.256(7) 0.025(6) Uani 1 1 d D U . . .
H3C H 1.058054 0.745829 0.173462 0.030 Uiso 1 1 calc R U . . .
H3D H 1.013741 0.864881 0.267960 0.030 Uiso 1 1 calc R U . . .
C10 C 0.688(7) 0.377(4) 0.379(10) 0.041(7) Uani 1 1 d D U . . .
H10A H 0.755186 0.447736 0.472408 0.049 Uiso 1 1 calc R U . . .
H10B H 0.739773 0.297110 0.343925 0.049 Uiso 1 1 calc R U . . .
O2 O 0.859(4) 0.522(3) -0.037(6) 0.046(4) Uani 1 1 d D U . . .
O5 O 0.846(5) 0.854(3) 0.488(7) 0.066(10) Uani 1 1 d D U . . .
C8 C 1.318(4) 0.910(3) 0.320(6) 0.024(7) Uani 1 1 d D U . . .
H8A H 1.287685 1.002223 0.317415 0.029 Uiso 1 1 calc R U . . .
H8B H 1.314568 0.845085 0.227282 0.029 Uiso 1 1 calc R U . . .


_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
C5 H5A 0.9700 . ?
C5 H5 0.9700 . ?
C5 C6 1.56(5) . ?
C5 C4 1.54(4) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.23(3) . ?
N4 C10 1.50(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.57(4) . ?
C2 C3 1.58(4) . ?
C6 C6 1.53(5) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
O6 N6 1.26(4) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 Cd1 2.34(5) . ?
N2 C4 1.47(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.45(5) . ?
N1 Cd1 2.24(4) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C12 C12 1.42(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.52(3) . ?
O1 N5 1.26(3) . ?
O1 Cd1 2.55(5) . ?
N6 O4 1.34(3) . ?
N6 O5 1.25(4) . ?
N5 O3 1.24(4) . ?
N5 O2 1.27(3) . ?
O4 Cd1 2.20(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.54(4) . ?
Cd1 N3 2.34(2) . ?
C4 H4C 0.9700 . ?
C4 H4 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N3 1.50(6) . ?
C7 C8 1.56(3) . ?
C3 C3 1.46(6) 2_755 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C9 C9 1.45(2) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.57(5) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
H5A C5 H5 109.0 . . ?
C6 C5 H5A 111.0 . . ?
C6 C5 H5 111.0 . . ?
C4 C5 H5A 111.0 . . ?
C4 C5 H5 111.0 . . ?
C4 C5 C6 104(6) . . ?
H4A N4 H4B 106.2 . . ?
Cd1 N4 H4A 105.9 . . ?
Cd1 N4 H4B 105.9 . . ?
C10 N4 H4A 105.9 . . ?
C10 N4 H4B 105.9 . . ?
C10 N4 Cd1 126(3) . . ?
H2A C2 H2B 108.7 . . ?
C1 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
C1 C2 C3 106(4) . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C5 C6 H6A 112.5 . . ?
C5 C6 H6B 112.5 . . ?
C6 C6 C5 96(10) 2_675 . ?
C6 C6 H6A 112.5 2_675 . ?
C6 C6 H6B 112.5 2_675 . ?
H6A C6 H6B 110.1 . . ?
H2C N2 H2D 107.2 . . ?
Cd1 N2 H2C 107.9 . . ?
Cd1 N2 H2D 107.9 . . ?
C4 N2 H2C 107.9 . . ?
C4 N2 H2D 107.9 . . ?
C4 N2 Cd1 117(2) . . ?
H1A N1 H1B 106.5 . . ?
C1 N1 H1A 106.4 . . ?
C1 N1 H1B 106.4 . . ?
C1 N1 Cd1 124(4) . . ?
Cd1 N1 H1A 106.4 . . ?
Cd1 N1 H1B 106.4 . . ?
C2 C1 H1C 109.3 . . ?
C2 C1 H1D 109.3 . . ?
N1 C1 C2 112(4) . . ?
N1 C1 H1C 109.3 . . ?
N1 C1 H1D 109.3 . . ?
H1C C1 H1D 107.9 . . ?
C12 C12 H12A 107.1 2_666 . ?
C12 C12 H12B 107.1 2_666 . ?
C12 C12 C11 121(5) 2_666 . ?
H12A C12 H12B 106.8 . . ?
C11 C12 H12A 107.1 . . ?
C11 C12 H12B 107.1 . . ?
N5 O1 Cd1 109(2) . . ?
O6 N6 O4 119(3) . . ?
O5 N6 O6 122(3) . . ?
O5 N6 O4 118(3) . . ?
O1 N5 O2 115(3) . . ?
O3 N5 O1 122(3) . . ?
O3 N5 O2 122(3) . . ?
N6 O4 Cd1 110(3) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 C10 111(3) . . ?
H11A C11 H11B 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
N4 Cd1 N2 90.3(15) . . ?
N4 Cd1 N1 97.3(12) . . ?
N4 Cd1 O1 79.1(19) . . ?
N4 Cd1 N3 166(2) . . ?
N2 Cd1 O1 80(2) . . ?
N1 Cd1 N2 168(3) . . ?
N1 Cd1 O1 92(2) . . ?
N1 Cd1 N3 88.4(10) . . ?
O4 Cd1 N4 83.9(19) . . ?
O4 Cd1 N2 113(2) . . ?
O4 Cd1 N1 77(2) . . ?
O4 Cd1 O1 158.9(10) . . ?
O4 Cd1 N3 85(2) . . ?
N3 Cd1 N2 86.2(13) . . ?
N3 Cd1 O1 113.7(19) . . ?
C5 C4 H4C 112.4 . . ?
C5 C4 H4 112.4 . . ?
N2 C4 C5 97(5) . . ?
N2 C4 H4C 112.4 . . ?
N2 C4 H4 112.4 . . ?
H4C C4 H4 109.9 . . ?
H7A C7 H7B 108.8 . . ?
N3 C7 H7A 110.6 . . ?
N3 C7 H7B 110.7 . . ?
N3 C7 C8 105(4) . . ?
C8 C7 H7A 110.6 . . ?
C8 C7 H7B 110.6 . . ?
C2 C3 H3A 107.7 . . ?
C2 C3 H3B 107.7 . . ?
C3 C3 C2 118(5) 2_755 . ?
C3 C3 H3A 107.7 2_755 . ?
C3 C3 H3B 107.7 2_755 . ?
H3A C3 H3B 107.1 . . ?
C9 C9 H9A 108.1 2_876 . ?
C9 C9 H9B 108.1 2_876 . ?
C9 C9 C8 117(3) 2_876 . ?
H9A C9 H9B 107.3 . . ?
C8 C9 H9A 108.1 . . ?
C8 C9 H9B 108.1 . . ?
Cd1 N3 H3C 107.5 . . ?
Cd1 N3 H3D 107.5 . . ?
C7 N3 Cd1 119(3) . . ?
C7 N3 H3C 107.5 . . ?
C7 N3 H3D 107.5 . . ?
H3C N3 H3D 107.0 . . ?
N4 C10 C11 110(6) . . ?
N4 C10 H10A 109.7 . . ?
N4 C10 H10B 109.7 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C7 C8 C9 109(4) . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
C9 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 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
C6 C5 C4 N2 -172(4) . . . . ?
O6 N6 O4 Cd1 -142(3) . . . . ?
C1 C2 C3 C3 64(5) . . . 2_755 ?
C12 C12 C11 C10 -30(12) 2_666 . . . ?
C12 C11 C10 N4 -64(9) . . . . ?
Cd1 N4 C10 C11 179(4) . . . . ?
Cd1 N2 C4 C5 -157(4) . . . . ?
Cd1 N1 C1 C2 176(4) . . . . ?
Cd1 O1 N5 O3 -149(4) . . . . ?
Cd1 O1 N5 O2 17(4) . . . . ?
C4 C5 C6 C6 151(6) . . . 2_675 ?
C3 C2 C1 N1 179(5) . . . . ?
C9 C9 C8 C7 -57(4) 2_876 . . . ?
N3 C7 C8 C9 -178(2) . . . . ?
O5 N6 O4 Cd1 28(4) . . . . ?
C8 C7 N3 Cd1 165(2) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.109
_oxdiff_exptl_absorpt_empirical_full_min 0.507
# start Validation Reply Form
_vrf_PLAT029_2_8_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.342 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_2_8_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.77 Note
RESPONSE: The data/parameter ratio is affected by the access limits of 
the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_2_8_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0825 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_2_8_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1815 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
####################################################################### 
# 
# 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_2_3_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262349'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_2_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.228 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_2_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.20 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC,
 particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT084_2_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT342_2_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.08917 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_2_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.591       1970 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C12 N6 O6'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.234(2)
_cell_length_b                   9.5879(16)
_cell_length_c                   10.970(5)
_cell_angle_alpha                110.44(3)
_cell_angle_beta                 106.00(3)
_cell_angle_gamma                97.186(17)
_cell_volume                     848.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7420
_cell_measurement_theta_min      3.6480
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 -4 -8 0.1147
-9 9 5 0.0497
8 10 -8 0.1428
8 -10 -4 0.1012
-4 -12 6 0.0738
-4 4 -13 0.0197
4 -5 13 0.0270

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
11.8745 -3.6901 -8.0684 0.0254 0.9912 -0.1301
-9.2977 9.0985 4.6869 -0.0245 -0.9405 -0.3389
7.7805 9.6837 -8.4551 0.0071 0.3288 -0.9444
8.1596 -10.2996 -3.5065 0.0233 0.8867 0.4618
-4.4833 -11.9444 5.7664 0.0537 -0.0002 0.9986
-4.1715 3.9232 -12.5692 0.9954 -0.0255 -0.0924
3.9149 -4.5536 12.8357 -0.9890 0.0254 0.1459

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.228
_diffrn_reflns_Laue_measured_fraction_max 0.228
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5773
_diffrn_reflns_point_group_measured_fraction_full 0.228
_diffrn_reflns_point_group_measured_fraction_max 0.228
_diffrn_reflns_theta_full        24.824
_diffrn_reflns_theta_max         24.824
_diffrn_reflns_theta_min         3.654
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.228
_diffrn_measured_fraction_theta_max 0.228
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 2.30(2) GPa
 (2300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  18.20   0.85   15.00    --   16.41  39.00 167.00   32
  2  ω    -15.00  22.40   0.85   15.00    --   16.41  26.00  -7.00   44
  3  ω    -18.00  41.50   0.85   15.00    --   16.41 -39.00-167.00   70
  4  ω    -18.00  41.50   0.85   15.00    --   16.41 -39.00  12.00   70
  5  ω    -23.00  14.40   0.85   15.00    --  -17.19 -26.00-172.00   44
  6  ω    -80.00 -25.60   0.85   15.00    --  -17.19 134.00 -56.00   64
  7  ω    -23.00  14.40   0.85   15.00    --  -17.19 -26.00   7.00   44
  8  ω      4.00  23.55   0.85   15.00    --  -17.19 -97.00  35.00   23
  9  ω    -38.00  -4.00   0.85   15.00    --  -17.19  57.00 -30.00   40
 10  ω    -42.00  18.35   0.85   15.00    --  -17.19  39.00 167.00   71
 11  ω    -80.00 -25.60   0.85   15.00    --  -17.19 134.00 123.00   64
 12  ω     25.00  45.40   0.85   15.00    --  -17.19-134.00-123.00   24
 13  ω     25.00  45.40   0.85   15.00    --  -17.19-134.00  56.00   24
 14  ω    -14.00   5.55   0.85   15.00    --   16.41  77.00 150.00   23
 15  ω     20.00  45.50   0.85   15.00    --   16.41 -77.00  30.00   30
 16  ω     -5.00  19.65   0.85   15.00    --   16.41  57.00 -30.00   29
 17  ω     19.00  45.35   0.85   15.00    --   16.41 -77.00-150.00   31
 18  ω    -16.00  42.65   0.85   15.00    --   16.41 -19.00-180.00   69
 19  ω    -43.00   8.00   0.85   15.00    --  -17.19  37.00-180.00   60
 20  ω    -18.00  13.45   0.85   15.00    --  -17.19 -19.00  30.00   37
 21  ω    -19.00   7.35   0.85   15.00    --  -17.19 -39.00-167.00   31
 22  ω    -19.00   7.35   0.85   15.00    --  -17.19 -39.00  12.00   31
 23  ω    -20.00   3.80   0.85   15.00    --  -17.19 -57.00-150.00   28
 24  ω    -31.00   0.45   0.85   15.00    --   16.41   0.00   0.00   37
 25  ω    -42.00   9.00   0.85   15.00    --  -17.19  67.00 -23.00   60
 26  ω    -43.00 -11.55   0.85   15.00    --  -17.19  19.00   0.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0501388000
_diffrn_orient_matrix_UB_12      -0.0186961000
_diffrn_orient_matrix_UB_13      -0.0683893000
_diffrn_orient_matrix_UB_21      0.0549535000
_diffrn_orient_matrix_UB_22      -0.0334784000
_diffrn_orient_matrix_UB_23      -0.0266585000
_diffrn_orient_matrix_UB_31      -0.0355228000
_diffrn_orient_matrix_UB_32      -0.0718560000
_diffrn_orient_matrix_UB_33      -0.0032919000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                469
_reflns_number_total             665
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.589
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         665
_refine_ls_number_restraints     386
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.1111
_refine_ls_restrained_S_all      1.228
_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          0.3163
_refine_ls_wR_factor_ref         0.3571
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C6_$1-C6
 1.7 with sigma of 0.02
 C3_$2-C3
 1.7 with sigma of 0.02
 C12-C12_$3
 1.45 with sigma of 0.02
 H2B-H5A
 2.05 with sigma of 0.02
 C12_$3-C11_$3
 1.45 with sigma of 0.02
 H4A-H12A_$3
 2.05 with sigma of 0.02
 H4B-H4D_$4
 2.05 with sigma of 0.02
 O2-N5 \\sim O3-N5 \\sim O1-N5 \\sim O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.02
 N3-C7 \\sim N1-C1 \\sim N4-C10 \\sim N2-C4
 with sigma of 0.02
 C9-C8 \\sim C8-C7 \\sim C5-C4 \\sim C6-C5 \\sim C11-C10 \\sim C12-C11 \\sim
C3-C2 \\sim C2-C1
 with sigma of 0.02
 O2-O1 \\sim O3-O2 \\sim O3-O1 \\sim O5-O4 \\sim O6-O4 \\sim O6-O5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cd1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(N6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(N1)
4. Rigid body (RIGU) restrains
 N4, N3, Cd1, C7, N1, O1, N2, C8, C1, N5, C4, C10, C9, C2, O2, O3, C5, C11, C3,
  C6, C12, N6, O5, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B), C1(H1C,H1D), C4(H4,H4D),
 C7(H7A,H7B), C2(H2C,H2D), C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B),
 C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B), C12(H12A,H12B)
;
_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
N3 N 1.046(7) 0.782(4) 0.260(9) 0.041(8) Uani 1 1 d D U . . .
H3A H 1.058238 0.751400 0.177655 0.049 Uiso 1 1 calc R U . . .
H3B H 1.010333 0.866025 0.271101 0.049 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8502(8) 0.5939(4) 0.2452(11) 0.069(7) Uani 1 1 d . U . . .
N1 N 1.023(7) 0.442(3) 0.258(8) 0.053(6) Uani 1 1 d D U . . .
H1A H 1.109524 0.484779 0.250399 0.063 Uiso 1 1 calc R U . . .
H1B H 1.049193 0.438630 0.341695 0.063 Uiso 1 1 calc R U . . .
O1 O 0.670(6) 0.417(4) 0.022(6) 0.077(8) Uani 1 1 d D U . . .
N2 N 0.684(6) 0.751(4) 0.215(7) 0.049(8) Uani 1 1 d D U . . .
H2A H 0.591440 0.707774 0.212992 0.059 Uiso 1 1 calc R U . . .
H2B H 0.720452 0.840351 0.288321 0.059 Uiso 1 1 calc DR U . . .
O2 O 0.863(5) 0.540(4) -0.004(6) 0.079(14) Uani 1 1 d D U . . .
N4 N 0.652(5) 0.471(5) 0.257(5) 0.083(10) Uani 1 1 d D U . . .
H4A H 0.597514 0.538520 0.283256 0.100 Uiso 1 1 calc DR U . . .
H4B H 0.595687 0.406098 0.170218 0.100 Uiso 1 1 calc DR U . . .
C1 C 0.961(7) 0.276(4) 0.147(9) 0.053(6) Uani 1 1 d D U . . .
H1C H 0.875249 0.223644 0.162914 0.063 Uiso 1 1 calc R U . . .
H1D H 0.921169 0.278442 0.056468 0.063 Uiso 1 1 calc R U . . .
N5 N 0.729(5) 0.455(5) -0.055(6) 0.061(12) Uani 1 1 d D U . . .
C4 C 0.662(5) 0.781(4) 0.083(6) 0.056(11) Uani 1 1 d D U . . .
H4 H 0.759618 0.821986 0.076845 0.067 Uiso 1 1 calc R U . . .
H4D H 0.602587 0.690688 -0.000379 0.067 Uiso 1 1 calc R U . . .
C7 C 1.210(8) 0.832(5) 0.370(9) 0.052(11) Uani 1 1 d D U . . .
H7A H 1.208336 0.899559 0.459068 0.062 Uiso 1 1 calc R U . . .
H7B H 1.241891 0.742528 0.379323 0.062 Uiso 1 1 calc R U . . .
C2 C 1.085(7) 0.191(4) 0.151(10) 0.053(6) Uani 1 1 d D U . . .
H2C H 1.146527 0.221430 0.247773 0.063 Uiso 1 1 calc R U . . .
H2D H 1.153053 0.227656 0.109387 0.063 Uiso 1 1 calc R U . . .
O3 O 0.648(5) 0.423(5) -0.177(6) 0.075(10) Uani 1 1 d D U . . .
C5 C 0.571(7) 0.899(6) 0.116(8) 0.078(13) Uani 1 1 d D U . . .
H5A H 0.625715 0.983051 0.205923 0.093 Uiso 1 1 calc DR U . . .
H5B H 0.468490 0.855001 0.112174 0.093 Uiso 1 1 calc R U . . .
C8 C 1.320(8) 0.913(4) 0.326(10) 0.046(11) Uani 1 1 d D U . . .
H8A H 1.293601 1.008250 0.326382 0.055 Uiso 1 1 calc R U . . .
H8B H 1.310575 0.849785 0.231463 0.055 Uiso 1 1 calc R U . . .
C3 C 1.046(5) 0.018(4) 0.0846(16) 0.053(6) Uani 1 1 d D U . . .
H3C H 0.978457 -0.026913 0.121867 0.063 Uiso 1 1 calc R U . . .
H3D H 1.139210 -0.020451 0.096432 0.063 Uiso 1 1 calc R U . . .
C6 C 0.566(5) 0.945(5) -0.001(8) 0.079(14) Uani 1 1 d D U . . .
H6A H 0.532377 0.856076 -0.088545 0.095 Uiso 1 1 calc R U . . .
H6B H 0.667167 1.004234 0.012927 0.095 Uiso 1 1 calc R U . . .
C9 C 1.485(8) 0.949(4) 0.419(9) 0.048(11) Uani 1 1 d D U . . .
H9A H 1.552168 1.003136 0.387190 0.057 Uiso 1 1 calc R U . . .
H9B H 1.513719 0.852788 0.410693 0.057 Uiso 1 1 calc R U . . .
O5 O 0.860(6) 0.849(4) 0.509(7) 0.105(16) Uani 1 1 d D U . . .
O4 O 1.000(6) 0.683(3) 0.513(8) 0.057(8) Uani 1 1 d D U . . .
N6 N 0.983(6) 0.817(3) 0.562(7) 0.059(12) Uani 1 1 d D U . . .
O6 O 1.093(6) 0.920(4) 0.661(7) 0.081(14) Uani 1 1 d D U . . .
C11 C 0.548(10) 0.316(4) 0.404(9) 0.070(14) Uani 1 1 d D U . . .
H11A H 0.452090 0.256352 0.327999 0.083 Uiso 1 1 calc R U . . .
H11B H 0.591937 0.246326 0.441105 0.083 Uiso 1 1 calc R U . . .
C10 C 0.660(8) 0.378(6) 0.346(9) 0.065(12) Uani 1 1 d D U . . .
H10A H 0.690018 0.287715 0.295949 0.078 Uiso 1 1 calc R U . . .
H10B H 0.750739 0.438018 0.427730 0.078 Uiso 1 1 calc R U . . .
C12 C 0.512(6) 0.433(4) 0.513(5) 0.070(16) Uani 1 1 d D U . . .
H12A H 0.418776 0.386722 0.523265 0.084 Uiso 1 1 calc R U . . .
H12B H 0.596261 0.465368 0.600393 0.084 Uiso 1 1 calc R U . . .


_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
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 Cd1 2.32(3) . ?
N3 C7 1.54(5) . ?
Cd1 N1 2.30(5) . ?
Cd1 O1 2.40(6) . ?
Cd1 N2 2.32(4) . ?
Cd1 N4 2.11(4) . ?
Cd1 O4 2.65(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.54(5) . ?
O1 N5 1.25(2) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C4 1.54(4) . ?
O2 N5 1.25(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C10 1.54(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.50(3) . ?
N5 O3 1.25(2) . ?
C4 H4 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.49(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.49(2) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.51(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.50(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.50(3) . ?
C3 C3 1.70(2) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.71(2) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.63(15) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O5 N6 1.25(2) . ?
O4 N6 1.26(2) . ?
N6 O6 1.25(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.51(2) . ?
C11 C12 1.483(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C12 1.44(2) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?

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
H3A N3 H3B 106.7 . . ?
Cd1 N3 H3A 106.9 . . ?
Cd1 N3 H3B 106.9 . . ?
C7 N3 H3A 106.9 . . ?
C7 N3 H3B 106.9 . . ?
C7 N3 Cd1 122(3) . . ?
N3 Cd1 O1 120(2) . . ?
N3 Cd1 N2 87.4(15) . . ?
N3 Cd1 O4 85(2) . . ?
N1 Cd1 N3 88.9(14) . . ?
N1 Cd1 O1 95(2) . . ?
N1 Cd1 N2 174.4(18) . . ?
N1 Cd1 O4 75(2) . . ?
O1 Cd1 O4 154.0(11) . . ?
N2 Cd1 O1 82.7(18) . . ?
N2 Cd1 O4 108.8(17) . . ?
N4 Cd1 N3 165.5(12) . . ?
N4 Cd1 N1 103.6(14) . . ?
N4 Cd1 O1 66.7(15) . . ?
N4 Cd1 N2 80.6(14) . . ?
N4 Cd1 O4 91.6(14) . . ?
Cd1 N1 H1A 108.8 . . ?
Cd1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.7 . . ?
C1 N1 Cd1 114(4) . . ?
C1 N1 H1A 108.8 . . ?
C1 N1 H1B 108.8 . . ?
N5 O1 Cd1 99.8(18) . . ?
Cd1 N2 H2A 108.6 . . ?
Cd1 N2 H2B 108.6 . . ?
H2A N2 H2B 107.6 . . ?
C4 N2 Cd1 115(2) . . ?
C4 N2 H2A 108.6 . . ?
C4 N2 H2B 108.6 . . ?
Cd1 N4 H4A 106.4 . . ?
Cd1 N4 H4B 106.4 . . ?
H4A N4 H4B 106.5 . . ?
C10 N4 Cd1 124(3) . . ?
C10 N4 H4A 106.4 . . ?
C10 N4 H4B 106.4 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
H1C C1 H1D 108.1 . . ?
C2 C1 N1 111(4) . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
O1 N5 O2 119.3(17) . . ?
O3 N5 O1 120.2(17) . . ?
O3 N5 O2 120.0(17) . . ?
N2 C4 H4 112.5 . . ?
N2 C4 H4D 112.5 . . ?
H4 C4 H4D 110.0 . . ?
C5 C4 N2 96(2) . . ?
C5 C4 H4 112.5 . . ?
C5 C4 H4D 112.5 . . ?
N3 C7 H7A 110.0 . . ?
N3 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 N3 109(5) . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
C1 C2 H2C 107.0 . . ?
C1 C2 H2D 107.0 . . ?
C1 C2 C3 121(4) . . ?
H2C C2 H2D 106.8 . . ?
C3 C2 H2C 107.0 . . ?
C3 C2 H2D 107.0 . . ?
C4 C5 H5A 112.3 . . ?
C4 C5 H5B 112.3 . . ?
C4 C5 C6 97(3) . . ?
H5A C5 H5B 109.9 . . ?
C6 C5 H5A 112.3 . . ?
C6 C5 H5B 112.3 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C7 C8 C9 112(5) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C2 C3 C3 102(5) . 2_755 ?
C2 C3 H3C 111.4 . . ?
C2 C3 H3D 111.4 . . ?
C3 C3 H3C 111.4 2_755 . ?
C3 C3 H3D 111.4 2_755 . ?
H3C C3 H3D 109.3 . . ?
C5 C6 C6 103(5) . 2_675 ?
C5 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
C6 C6 H6A 111.1 2_675 . ?
C6 C6 H6B 111.1 2_675 . ?
H6A C6 H6B 109.0 . . ?
C8 C9 C9 114(5) . 2_876 ?
C8 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C9 C9 H9A 108.8 2_876 . ?
C9 C9 H9B 108.8 2_876 . ?
H9A C9 H9B 107.7 . . ?
N6 O4 Cd1 102(3) . . ?
O5 N6 O4 120.0(17) . . ?
O5 N6 O6 120.6(15) . . ?
O6 N6 O4 119.4(16) . . ?
H11A C11 H11B 107.5 . . ?
C10 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
C12 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C12 C11 C10 115(4) . . ?
N4 C10 H10A 103.5 . . ?
N4 C10 H10B 103.5 . . ?
C11 C10 N4 135(6) . . ?
C11 C10 H10A 103.5 . . ?
C11 C10 H10B 103.5 . . ?
H10A C10 H10B 105.3 . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C12 C12 C11 114(4) 2_666 . ?
C12 C12 H12A 108.7 2_666 . ?
C12 C12 H12B 108.7 2_666 . ?
H12A C12 H12B 107.6 . . ?

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
N3 C7 C8 C9 -173(3) . . . . ?
Cd1 N3 C7 C8 162(2) . . . . ?
Cd1 N1 C1 C2 173(3) . . . . ?
Cd1 O1 N5 O2 13(5) . . . . ?
Cd1 O1 N5 O3 -159(5) . . . . ?
Cd1 N2 C4 C5 -172(3) . . . . ?
Cd1 N4 C10 C11 161(7) . . . . ?
Cd1 O4 N6 O5 35(5) . . . . ?
Cd1 O4 N6 O6 -143(4) . . . . ?
N1 C1 C2 C3 162(6) . . . . ?
N2 C4 C5 C6 173(4) . . . . ?
C1 C2 C3 C3 62(7) . . . 2_755 ?
C4 C5 C6 C6 169(6) . . . 2_675 ?
C7 C8 C9 C9 -57(6) . . . 2_876 ?
C10 C11 C12 C12 42(9) . . . 2_666 ?
C12 C11 C10 N4 -69(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   862
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.900
_oxdiff_exptl_absorpt_empirical_full_min 0.677
####################################################################### 
# 
# 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_3_3_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262352'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_3_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.353 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_3_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.97 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC,
 particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_3_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0625 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT410_3_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Short Intra H...H Contact  H5       ..H6       .       1.82 Ang.
RESPONSE: Due to the high-pressure some atoms may have an ill-defined 
connectivity or are subjected to a unresolved spatial disorder. These factors
 contribute for inaccurate automatic placement of the hydrogen atoms.
;
_vrf_PLAT911_3_3_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1970 Report
RESPONSE: The data come from high-pressure studies and are limited by the
 DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H15 Cd0.5 N3 O3'
_chemical_formula_sum            'C6 H15 Cd0.50 N3 O3'
_chemical_formula_weight         233.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 H16 Cd0.5 N3 O3'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.147(2)
_cell_length_b                   9.5510(17)
_cell_length_c                   10.842(5)
_cell_angle_alpha                110.73(3)
_cell_angle_beta                 106.08(3)
_cell_angle_gamma                97.435(17)
_cell_volume                     823.5(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2657
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5010
_cell_measurement_theta_min      2.3260
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.790
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             480
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 9 0.0485
2 13 -5 0.0555
9 -10 -4 0.0737
8 9 -8 0.0399
-10 -7 9 0.0309
10 7 -9 0.0309
-1 -13 4 0.0820
5 -4 12 0.0325
-5 4 -12 0.0325

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.1201 -1.7690 8.5586 -0.0181 0.8138 -0.5809
1.9996 12.7884 -4.6640 0.0208 -0.8368 -0.5471
9.0668 -9.6660 -3.5429 -0.0022 0.0091 1.0000
8.1364 9.2485 -7.8185 0.0254 -0.9994 -0.0254
-9.8863 -7.0569 8.7823 0.0012 0.9811 -0.1932
9.8863 7.0569 -8.7823 -0.0012 -0.9811 0.1932
-0.6387 -13.0416 3.5085 -0.0414 0.7692 0.6431
4.7595 -3.5989 11.8638 0.9942 -0.0058 0.1076
-4.7595 3.5989 -11.8638 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.353
_diffrn_reflns_Laue_measured_fraction_max 0.201
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6161
_diffrn_reflns_point_group_measured_fraction_full 0.353
_diffrn_reflns_point_group_measured_fraction_max 0.201
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.292
_diffrn_reflns_theta_min         2.357
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.353
_diffrn_measured_fraction_theta_max 0.201
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 3.30(2) GPa
 (3300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  -5.00   0.75   15.00    --    0.00  19.00-150.00   60
  2  ω    -33.00  42.00   0.75   15.00    --    0.00 -13.00   3.00  100
  3  ω    -26.00   1.00   0.75   15.00    --  -30.50 -57.00-150.00   36
  4  ω    -95.00 -20.00   0.75   15.00    --  -30.50 135.00 -57.00  100
  5  ω      7.00  29.50   0.75   15.00    --  -30.50-114.00  45.00   30
  6  ω    -30.00  39.00   0.75   15.00    --  -30.50 -26.00-171.00   92
  7  ω    -30.00  39.00   0.75   15.00    --  -30.50 -26.00   8.00   92
  8  ω   -109.00 -73.00   0.75   15.00    --  -30.50 178.00  90.00   48
  9  ω    -25.00  15.50   0.75   15.00    --  -30.50 -39.00  12.00   54
 10  ω    -25.00  15.50   0.75   15.00    --  -30.50 -39.00-167.00   54
 11  ω    -20.00   2.50   0.75   15.00    --  -30.50 -53.00  17.00   30
 12  ω    -66.00   9.00   0.75   15.00    --  -30.50  81.00 -29.00  100
 13  ω    -66.00   9.00   0.75   15.00    --  -30.50  81.00 151.00  100
 14  ω     -2.00  19.00   0.75   15.00    --  -30.50 -97.00  35.00   28
 15  ω    -36.00  29.25   0.75   15.00    --   33.71  26.00  -8.00   87
 16  ω     10.00  73.00   0.75   15.00    --   33.71 -97.00-143.00   84
 17  ω     17.50  82.00   0.75   15.00    --   33.71-114.00  45.00   86
 18  ω    -14.00  13.00   0.75   15.00    --   33.71  38.00-180.00   36
 19  ω    -35.00 -12.50   0.75   15.00    --    0.00  77.00 -30.00   30
 20  ω    -12.00   9.00   0.75   15.00    --  -30.50 -77.00  30.00   28
 21  ω    -35.00 -12.50   0.75   15.00    --  -30.50  77.00 120.00   30
 22  ω    -50.00  25.00   0.75   15.00    --  -30.50  39.00 167.00  100
 23  ω      7.00  29.50   0.75   15.00    --  -30.50-114.00-135.00   30
 24  ω     -2.00  19.00   0.75   15.00    --  -30.50 -97.00-143.00   28
 25  ω    -14.00  34.00   0.75   15.00    --   33.71 -38.00-150.00   64
 26  ω    -24.00  30.00   0.75   15.00    --   33.71 -13.00   3.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0483255000
_diffrn_orient_matrix_UB_12      0.0197479000
_diffrn_orient_matrix_UB_13      0.0704020000
_diffrn_orient_matrix_UB_21      -0.0555082000
_diffrn_orient_matrix_UB_22      -0.0548850000
_diffrn_orient_matrix_UB_23      0.0051308000
_diffrn_orient_matrix_UB_31      0.0392702000
_diffrn_orient_matrix_UB_32      -0.0577458000
_diffrn_orient_matrix_UB_33      -0.0241979000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                647
_reflns_number_total             825
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         825
_refine_ls_number_restraints     409
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0879
_refine_ls_restrained_S_all      0.878
_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)+(0.0517P)²+46.7593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2253
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C12_$3-C12
 1.45 with sigma of 0.05
 C9-C9_$1
 1.45 with sigma of 0.05
 C3-C3_$2
 1.45 with sigma of 0.05
 C4-C5
 1.45 with sigma of 0.05
 C6_$4-C6
 1.45 with sigma of 0.05
 C4-C6
 2.1 with sigma of 0.1
 C6_$4-C5
 2.1 with sigma of 0.1
 C5-C6
 1.45 with sigma of 0.02
 C5-C4
 1.55 with sigma of 0.02
 H4C_$5-H4B_$3
 2.05 with sigma of 0.02
 H4A-H12B_$3
 2.05 with sigma of 0.02
 C6-C5
 1.55 with sigma of 0.02
 H4B-H6B_$6
 2.05 with sigma of 0.02
 O3-N5 \\sim O2-N5 \\sim O1-N5 \\sim O6-N6 \\sim O4-N6 \\sim O5-N6
 with sigma of 0.05
 N2-C4 \\sim N3-C7 \\sim N4-C10
 with sigma of 0.05
 C11-C10 \\sim C12-C11 \\sim C8-C7 \\sim C9-C8 \\sim C2-C1 \\sim C3-C2
 with sigma of 0.05
3. Restrained planarity
 O1, N5, O3, O2
 with sigma of 0.1
4. Rigid bond restraints
 O1, N5, O3, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, N6, O4, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C12, C11, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C9, N3, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, N1, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N2, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O1 \\sim N5 \\sim O3 \\sim O2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O6 \\sim N6 \\sim O4 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N4 \\sim C12 \\sim C11 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C7 \\sim C9 \\sim N3 \\sim C8: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C2 \\sim N1 \\sim C1 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C4 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C4 \\sim N2 \\sim C6 \\sim C5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N4) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) = Uanis(N6) = Uanis(O5) = Uanis(O6)
6. Rigid body (RIGU) restrains
 O1, N5, O3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, N6, O4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C12, C11, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C9, N3, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, N1, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C4, N2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B), C12(H12A,H12B), C11(H11A,H11B), C7(H7A,
 H7B), C3(H3A,H3B), C9(H9A,H9B), N3(H3C,H3D), C10(H10A,H10B), C8(H8A,H8B),
 C4(H4C,H4), N2(H2C,H2D), C6(H6,H6B), C5(H5A,H5)
;
_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
N4 N 0.659(3) 0.458(3) 0.286(4) 0.036(7) Uani 1 1 d D U . . .
H4A H 0.605559 0.523796 0.321292 0.043 Uiso 1 1 calc DR U . . .
H4B H 0.592674 0.390703 0.201234 0.043 Uiso 1 1 calc DR U . . .
C2 C 1.101(5) 0.199(3) 0.170(7) 0.021(6) Uani 1 1 d D U . . .
H2A H 1.180536 0.243468 0.142054 0.025 Uiso 1 1 calc R U . . .
H2B H 1.147314 0.216284 0.267937 0.025 Uiso 1 1 calc R U . . .
O6 O 1.080(5) 0.915(3) 0.647(7) 0.110(11) Uani 1 1 d D U . . .
N1 N 1.014(6) 0.437(3) 0.255(8) 0.027(6) Uani 1 1 d . U . . .
C1 C 0.958(5) 0.275(3) 0.150(8) 0.021(6) Uani 1 1 d D U . . .
H1A H 0.921014 0.271173 0.055610 0.025 Uiso 1 1 calc R U . . .
H1B H 0.871637 0.220440 0.164628 0.025 Uiso 1 1 calc R U . . .
C12 C 0.450(3) 0.424(2) 0.443(3) 0.025(7) Uani 1 1 d D U . . .
H12A H 0.397679 0.439201 0.359194 0.030 Uiso 1 1 calc R U . . .
H12B H 0.370521 0.381640 0.471947 0.030 Uiso 1 1 calc R U . . .
O1 O 0.659(5) 0.413(3) -0.013(6) 0.038(6) Uani 1 1 d D U . . .
N6 N 0.971(5) 0.815(3) 0.546(6) 0.110(11) Uani 1 1 d D U . . .
N5 N 0.715(4) 0.450(3) -0.090(5) 0.027(7) Uani 1 1 d D U . . .
O4 O 0.982(7) 0.677(4) 0.504(11) 0.110(11) Uani 1 1 d D U . . .
C11 C 0.550(7) 0.312(4) 0.409(10) 0.037(7) Uani 1 1 d D U . . .
H11A H 0.484291 0.216891 0.330530 0.045 Uiso 1 1 calc R U . . .
H11B H 0.591245 0.287637 0.489355 0.045 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8437(6) 0.5942(3) 0.2468(9) 0.031(4) Uani 1 1 d . U . . .
C7 C 1.192(6) 0.817(3) 0.350(7) 0.022(6) Uani 1 1 d D U . . .
H7A H 1.220959 0.722770 0.349569 0.027 Uiso 1 1 calc R U . . .
H7B H 1.189941 0.875355 0.443483 0.027 Uiso 1 1 calc R U . . .
O3 O 0.629(5) 0.425(3) -0.208(6) 0.038(6) Uani 1 1 d D U . . .
C3 C 1.034(4) 0.023(3) 0.076(3) 0.020(7) Uani 1 1 d D U . . .
H3A H 1.117742 -0.027507 0.093091 0.024 Uiso 1 1 calc R U . . .
H3B H 0.953295 -0.016482 0.105842 0.024 Uiso 1 1 calc R U . . .
C9 C 1.487(4) 0.950(2) 0.427(3) 0.023(6) Uani 1 1 d D U . . .
H9A H 1.510989 0.852722 0.424192 0.028 Uiso 1 1 calc R U . . .
H9B H 1.560490 0.997943 0.395370 0.028 Uiso 1 1 calc R U . . .
N3 N 1.036(5) 0.777(3) 0.249(6) 0.020(6) Uani 1 1 d D U . . .
H3C H 1.043773 0.743806 0.163434 0.025 Uiso 1 1 calc R U . . .
H3D H 1.003356 0.863430 0.262247 0.025 Uiso 1 1 calc R U . . .
C10 C 0.687(6) 0.371(4) 0.372(8) 0.036(6) Uani 1 1 d D U . . .
H10A H 0.773114 0.436083 0.459140 0.043 Uiso 1 1 calc R U . . .
H10B H 0.722691 0.282779 0.323700 0.043 Uiso 1 1 calc R U . . .
O2 O 0.853(5) 0.522(3) -0.046(7) 0.054(8) Uani 1 1 d D U . . .
O5 O 0.855(5) 0.858(3) 0.501(7) 0.110(11) Uani 1 1 d D U . . .
C8 C 1.316(4) 0.913(3) 0.321(6) 0.025(6) Uani 1 1 d D U . . .
H8A H 1.289485 1.009903 0.327274 0.030 Uiso 1 1 calc R U . . .
H8B H 1.313468 0.857258 0.226430 0.030 Uiso 1 1 calc R U . . .
C4 C 0.667(4) 0.780(3) 0.069(4) 0.059(8) Uani 1 1 d D U . . .
H4C H 0.583251 0.698434 -0.009924 0.071 Uiso 1 1 calc R U . . .
H4 H 0.764387 0.768947 0.052986 0.071 Uiso 1 1 calc R U . . .
N2 N 0.673(6) 0.751(3) 0.188(8) 0.041(7) Uani 1 1 d D U . . .
H2C H 0.576167 0.705035 0.176522 0.049 Uiso 1 1 calc R U . . .
H2D H 0.702449 0.841318 0.262150 0.049 Uiso 1 1 calc R U . . .
C6 C 0.470(5) 0.920(3) 0.006(6) 0.098(12) Uani 1 1 d D U . . .
H6 H 0.415590 0.928498 0.072536 0.117 Uiso 1 1 calc R U . . .
H6B H 0.413782 0.832133 -0.083330 0.117 Uiso 1 1 calc R U . . .
C5 C 0.641(6) 0.934(5) 0.064(8) 0.080(10) Uani 1 1 d D U . . .
H5A H 0.686796 1.016025 0.157673 0.096 Uiso 1 1 calc R U . . .
H5 H 0.693270 0.958747 0.004785 0.096 Uiso 1 1 calc R U . . .


_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
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.224(19) . ?
N4 C10 1.45(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.58(4) . ?
C2 C3 1.55(4) . ?
O6 N6 1.23(4) . ?
N1 C1 1.48(6) . ?
N1 Cd1 2.30(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C12 C12 1.49(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.51(3) . ?
O1 N5 1.22(4) . ?
O1 Cd1 2.63(6) . ?
N6 O4 1.26(3) . ?
N6 O5 1.22(4) . ?
N5 O3 1.22(4) . ?
N5 O2 1.23(4) . ?
O4 Cd1 2.49(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.52(3) . ?
Cd1 N3 2.305(18) . ?
Cd1 N2 2.41(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N3 1.44(6) . ?
C7 C8 1.54(3) . ?
C3 C3 1.46(6) 2_755 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C9 C9 1.46(5) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.57(4) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4 0.9700 . ?
C4 N2 1.40(6) . ?
C4 C5 1.53(2) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
C6 C6 1.62(5) 2_675 ?
C6 H6 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.488(16) . ?
C5 H5A 0.9700 . ?
C5 H5 0.9700 . ?

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
H4A N4 H4B 106.3 . . ?
Cd1 N4 H4A 106.0 . . ?
Cd1 N4 H4B 106.0 . . ?
C10 N4 H4A 106.0 . . ?
C10 N4 H4B 106.0 . . ?
C10 N4 Cd1 125(2) . . ?
H2A C2 H2B 108.6 . . ?
C1 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C3 C2 H2B 110.4 . . ?
C3 C2 C1 107(3) . . ?
C1 N1 Cd1 118(4) . . ?
C2 C1 H1A 110.3 . . ?
C2 C1 H1B 110.3 . . ?
N1 C1 C2 107(4) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
C12 C12 H12A 109.6 2_666 . ?
C12 C12 H12B 109.6 2_666 . ?
C12 C12 C11 110(4) 2_666 . ?
H12A C12 H12B 108.1 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
N5 O1 Cd1 107(3) . . ?
O6 N6 O4 118(5) . . ?
O5 N6 O6 116(3) . . ?
O5 N6 O4 126(5) . . ?
O1 N5 O2 120(5) . . ?
O3 N5 O1 119(4) . . ?
O3 N5 O2 121(4) . . ?
N6 O4 Cd1 99(6) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C12 C11 C10 114(2) . . ?
H11A C11 H11B 107.6 . . ?
C10 C11 H11A 108.6 . . ?
C10 C11 H11B 108.6 . . ?
N4 Cd1 N1 96.7(9) . . ?
N4 Cd1 O1 79.2(10) . . ?
N4 Cd1 O4 82.7(11) . . ?
N4 Cd1 N3 167.9(12) . . ?
N4 Cd1 N2 91.5(10) . . ?
N1 Cd1 O1 94.2(19) . . ?
N1 Cd1 O4 76.6(19) . . ?
N1 Cd1 N2 167(2) . . ?
O4 Cd1 O1 158.6(8) . . ?
N3 Cd1 N1 89.8(9) . . ?
N3 Cd1 O1 110.7(16) . . ?
N3 Cd1 O4 88.9(17) . . ?
N3 Cd1 N2 84.1(11) . . ?
N2 Cd1 O1 77.3(17) . . ?
N2 Cd1 O4 114.7(17) . . ?
H7A C7 H7B 107.8 . . ?
N3 C7 H7A 109.1 . . ?
N3 C7 H7B 109.1 . . ?
N3 C7 C8 113(4) . . ?
C8 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C2 C3 H3A 107.9 . . ?
C2 C3 H3B 107.9 . . ?
C3 C3 C2 117(4) 2_755 . ?
C3 C3 H3A 107.9 2_755 . ?
C3 C3 H3B 107.9 2_755 . ?
H3A C3 H3B 107.2 . . ?
C9 C9 H9A 108.6 2_876 . ?
C9 C9 H9B 108.6 2_876 . ?
C9 C9 C8 115(3) 2_876 . ?
H9A C9 H9B 107.5 . . ?
C8 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
Cd1 N3 H3C 107.9 . . ?
Cd1 N3 H3D 107.9 . . ?
C7 N3 Cd1 118(2) . . ?
C7 N3 H3C 107.9 . . ?
C7 N3 H3D 107.9 . . ?
H3C N3 H3D 107.2 . . ?
N4 C10 C11 117(4) . . ?
N4 C10 H10A 108.1 . . ?
N4 C10 H10B 108.1 . . ?
C11 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C7 C8 C9 113(4) . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
H4C C4 H4 106.7 . . ?
N2 C4 H4C 107.0 . . ?
N2 C4 H4 107.0 . . ?
N2 C4 C5 121(4) . . ?
C5 C4 H4C 107.0 . . ?
C5 C4 H4 107.0 . . ?
Cd1 N2 H2C 107.8 . . ?
Cd1 N2 H2D 107.8 . . ?
C4 N2 Cd1 117.9(18) . . ?
C4 N2 H2C 107.8 . . ?
C4 N2 H2D 107.8 . . ?
H2C N2 H2D 107.2 . . ?
C6 C6 H6 114.8 2_675 . ?
C6 C6 H6B 114.8 2_675 . ?
H6 C6 H6B 111.9 . . ?
C5 C6 C6 83(3) . 2_675 ?
C5 C6 H6 114.8 . . ?
C5 C6 H6B 114.8 . . ?
C4 C5 H5A 109.8 . . ?
C4 C5 H5 109.8 . . ?
C6 C5 C4 109(3) . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5 109.8 . . ?
H5A C5 H5 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 N6 O4 Cd1 -145(4) . . . . ?
C1 C2 C3 C3 63(4) . . . 2_755 ?
C12 C12 C11 C10 -55(7) 2_666 . . . ?
C12 C11 C10 N4 -40(8) . . . . ?
Cd1 N4 C10 C11 168(4) . . . . ?
Cd1 N1 C1 C2 175(3) . . . . ?
Cd1 O1 N5 O3 -155(2) . . . . ?
Cd1 O1 N5 O2 20(2) . . . . ?
C3 C2 C1 N1 172(4) . . . . ?
C9 C9 C8 C7 -66(4) 2_876 . . . ?
N3 C7 C8 C9 -177(2) . . . . ?
O5 N6 O4 Cd1 40(5) . . . . ?
C8 C7 N3 Cd1 168(2) . . . . ?
N2 C4 C5 C6 -90(5) . . . . ?
C6 C6 C5 C4 -167(5) 2_675 . . . ?
C5 C4 N2 Cd1 -147(3) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.016
_oxdiff_exptl_absorpt_empirical_full_min 0.707
####################################################################### 
# 
# 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_2_55_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262350'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_2_55_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.347 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_2_55_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.19 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC,
 particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_2_55_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.08 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_2_55_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2008 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12CdN6O6
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'
Cd Cd -0.8075 1.2024 '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      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                   9.202(3)
_cell_length_b                   9.608(2)
_cell_length_c                   10.973(6)
_cell_angle_alpha                110.88(4)
_cell_angle_beta                 106.16(4)
_cell_angle_gamma                97.29(2)
_cell_volume                     842.5(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1731
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7150
_cell_measurement_theta_min      2.3390
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.794
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 8 0.0485
2 13 -4 0.0555
9 -10 -4 0.0737
8 9 -7 0.0399
-10 -7 8 0.0309
10 7 -8 0.0309
-1 -13 3 0.0820
5 -4 12 0.0325
-5 4 -12 0.0325

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.2781 -1.7600 8.3528 -0.0181 0.8138 -0.5809
2.1345 12.7451 -4.1830 0.0208 -0.8368 -0.5471
9.0892 -9.6361 -3.7821 -0.0022 0.0091 1.0000
8.3123 9.2145 -7.3911 0.0254 -0.9994 -0.0254
-10.0694 -7.0437 8.4249 0.0012 0.9811 -0.1932
10.0694 7.0437 -8.4249 -0.0012 -0.9811 0.1932
-0.7550 -12.9860 3.0241 -0.0414 0.7692 0.6431
4.5642 -4.1215 12.2575 0.9942 -0.0058 0.1076
-4.5642 4.1215 -12.2575 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.347
_diffrn_reflns_Laue_measured_fraction_max 0.196
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5255
_diffrn_reflns_point_group_measured_fraction_full 0.347
_diffrn_reflns_point_group_measured_fraction_max 0.196
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.345
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.347
_diffrn_measured_fraction_theta_max 0.196
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 2.55(20) GPa
 (2550000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     63.00  90.00   0.75   13.50    --    0.00 178.00 -90.00   36
  2  ω    -14.00  34.00   0.75   13.50    --    0.00 -67.00  23.00   64
  3  ω    -30.00  39.00   0.75   13.50    --  -30.50 -26.00   8.00   92
  4  ω     -2.00  19.00   0.75   13.50    --  -30.50 -97.00  35.00   28
  5  ω    -25.00  15.50   0.75   13.50    --  -30.50 -39.00  12.00   54
  6  ω   -109.00 -73.00   0.75   13.50    --  -30.50 178.00  90.00   48
  7  ω    -61.00  14.00   0.75   13.50    --  -30.50  67.00 -23.00  100
  8  ω    -95.00 -20.00   0.75   13.50    --  -30.50 135.00 -57.00  100
  9  ω    -14.00  16.00   0.75   13.50    --  -30.50 -38.00-180.00   40
 10  ω    -26.00   1.00   0.75   13.50    --  -30.50 -57.00  30.00   36
 11  ω      7.00  29.50   0.75   13.50    --  -30.50-114.00  45.00   30
 12  ω    -61.00  14.00   0.75   13.50    --  -30.50  67.00 157.00  100
 13  ω    -12.00   9.00   0.75   13.50    --  -30.50 -77.00-150.00   28
 14  ω    -20.00   2.50   0.75   13.50    --  -30.50 -53.00  17.00   30
 15  ω    -37.00  29.00   0.75   13.50    --   33.71  26.00  -8.00   88
 16  ω      0.00  19.50   0.75   13.50    --   33.71  53.00 162.00   26
 17  ω    -36.00   6.00   0.75   13.50    --   33.71   0.00-150.00   56
 18  ω     71.00 107.00   0.75   13.50    --   33.71 178.00  90.00   48
 19  ω      3.00  66.00   0.75   13.50    --   33.71 -81.00-151.00   84
 20  ω      0.00  19.50   0.75   13.50    --   33.71  53.00 -17.00   26
 21  ω      5.50  73.00   0.75   13.50    --   33.71 -97.00  35.00   90
 22  ω    -14.00  47.50   0.75   13.50    --    0.00 -38.00-180.00   82
 23  ω    -50.00  -5.00   0.75   13.50    --    0.00  19.00-150.00   60
 24  ω      7.00  29.50   0.75   13.50    --  -30.50-114.00-135.00   30
 25  ω    -25.00  15.50   0.75   13.50    --  -30.50 -39.00-167.00   54
 26  ω    -50.00  25.00   0.75   13.50    --  -30.50  19.00-180.00  100
 27  ω    -14.00  19.00   0.75   13.50    --   33.71 -38.00-150.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0463373000
_diffrn_orient_matrix_UB_12      0.0166694000
_diffrn_orient_matrix_UB_13      0.0694579000
_diffrn_orient_matrix_UB_21      -0.0569171000
_diffrn_orient_matrix_UB_22      -0.0554429000
_diffrn_orient_matrix_UB_23      0.0020784000
_diffrn_orient_matrix_UB_31      0.0385935000
_diffrn_orient_matrix_UB_32      -0.0575773000
_diffrn_orient_matrix_UB_33      -0.0249481000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                506
_reflns_number_total             826
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         826
_refine_ls_number_restraints     464
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.0957
_refine_ls_restrained_S_all      0.840
_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)+(0.0639P)²+46.4077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2626
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C6_$2-C6_$3
 1.45 with sigma of 0.02
 C8-C7 \\sim C9-C8 \\sim C6-C5 \\sim C5-C4 \\sim C2-C1 \\sim C3-C2 \\sim
C11-C10 \\sim C12-C11
 with sigma of 0.02
 N4-C10 \\sim N1-C1 \\sim N3-C7 \\sim N2-C4
 with sigma of 0.02
 O2-N5 \\sim O1-N5 \\sim O3-N5 \\sim O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.02
 C6-C6_$1 \\sim C6-C5 \\sim C5-C4 \\sim C6-C5 \\sim C5-C4
 with sigma of 0.02
 C12-C12_$4 \\sim C12_$4-C11_$4 \\sim C11_$4-C10_$4 \\sim C12-C11 \\sim C11-C10
\\sim C2-C1 \\sim C3-
 C2 \\sim C3-C3_$5 \\sim C3_$5-C2_$5 \\sim C2_$5-C1_$5 \\sim C5-C4 \\sim C6-C5
\\sim C6-C6_$1 \\sim C6_$1-
 C5_$1 \\sim C5_$1-C4_$1
 with sigma of 0.02
3. Rigid bond restraints
 N3, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, N6, O5, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, N5, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C4, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N2 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N4 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O2 \\sim N5 \\sim O3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O4 \\sim N6 \\sim O5 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(Cd1) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(N6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cd1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) = Uanis(O5) = Uanis(O6)
Uanis(N5) = Uanis(O2) = Uanis(O3) = Uanis(O1)
5. Rigid body (RIGU) restrains
 N2, C4, C5, C6, C6, C5, C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(H5A)+Sof(H5B)]=1 with esd of 0.01
 Sof(H5A)=Sof(H5B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), N2(H2C,H2D), N4(H4A,H4B),
 N3(H3C,H3D), C4(H4C,H4D), C10(H10A,H10B), C7(H7A,H7B), C5(H5A,H5B), C11(H11A,
 H11B), C8(H8A,H8B), C6(H6A,H6B), C12(H12A,H12B), C9(H9A,H9B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
N1 N 1.012(6) 0.439(3) 0.249(9) 0.038(15) Uani 1 1 d D U . . .
H1A H 1.094507 0.480291 0.233577 0.046 Uiso 1 1 calc R U . . .
H1B H 1.047215 0.443765 0.334448 0.046 Uiso 1 1 calc R U . . .
C1 C 0.958(5) 0.273(3) 0.151(8) 0.031(8) Uani 1 1 d D U . . .
H1C H 0.909262 0.263862 0.056809 0.037 Uiso 1 1 calc R U . . .
H1D H 0.879976 0.221233 0.174681 0.037 Uiso 1 1 calc R U . . .
C2 C 1.088(5) 0.193(3) 0.154(8) 0.025(7) Uani 1 1 d D U . . .
H2A H 1.147492 0.218018 0.250278 0.031 Uiso 1 1 calc R U . . .
H2B H 1.157510 0.235606 0.116378 0.031 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8463(7) 0.5940(4) 0.2457(11) 0.047(4) Uani 1 1 d . U . . .
C3 C 1.040(5) 0.022(3) 0.0758(13) 0.029(7) Uani 1 1 d D U . . .
H3A H 1.132021 -0.018380 0.089263 0.034 Uiso 1 1 calc R U . . .
H3B H 0.970638 -0.022235 0.111857 0.034 Uiso 1 1 calc R U . . .
O4 O 0.985(8) 0.670(4) 0.483(11) 0.053(6) Uani 1 1 d D U . . .
N2 N 0.691(6) 0.754(4) 0.218(9) 0.053(9) Uani 1 1 d D U . . .
H2C H 0.598167 0.716051 0.219106 0.064 Uiso 1 1 calc R U . . .
H2D H 0.732743 0.844929 0.290609 0.064 Uiso 1 1 calc R U . . .
N4 N 0.653(6) 0.456(4) 0.278(8) 0.053(17) Uani 1 1 d D U . . .
H4A H 0.597808 0.521003 0.308969 0.063 Uiso 1 1 calc R U . . .
H4B H 0.591168 0.387718 0.193398 0.063 Uiso 1 1 calc R U . . .
N3 N 1.043(5) 0.781(3) 0.254(7) 0.018(5) Uani 1 1 d D U . . .
H3C H 1.052663 0.748870 0.171019 0.021 Uiso 1 1 calc R U . . .
H3D H 1.009616 0.866216 0.267626 0.021 Uiso 1 1 calc R U . . .
O1 O 0.671(5) 0.420(3) 0.000(7) 0.053(5) Uani 1 1 d D U . . .
O2 O 0.867(5) 0.532(3) -0.019(6) 0.053(5) Uani 1 1 d D U . . .
N6 N 0.972(5) 0.808(3) 0.540(6) 0.051(11) Uani 1 1 d D U . . .
C4 C 0.666(7) 0.780(5) 0.088(10) 0.065(10) Uani 1 1 d D U . . .
H4C H 0.594274 0.690278 0.007713 0.078 Uiso 1 1 calc R U . . .
H4D H 0.763967 0.800303 0.073033 0.078 Uiso 1 1 calc R U . . .
C10 C 0.680(6) 0.370(4) 0.369(9) 0.046(14) Uani 1 1 d D U . . .
H10A H 0.724970 0.286389 0.328932 0.055 Uiso 1 1 calc R U . . .
H10B H 0.754628 0.438433 0.459704 0.055 Uiso 1 1 calc R U . . .
C7 C 1.204(5) 0.825(4) 0.361(7) 0.029(7) Uani 1 1 d D U . . .
H7A H 1.235195 0.733103 0.364012 0.034 Uiso 1 1 calc R U . . .
H7B H 1.204150 0.888300 0.452307 0.034 Uiso 1 1 calc R U . . .
N5 N 0.725(5) 0.452(4) -0.084(5) 0.053(5) Uani 1 1 d D U . . .
O5 O 0.851(6) 0.853(3) 0.494(8) 0.053(6) Uani 1 1 d D U . . .
O6 O 1.079(6) 0.913(3) 0.649(8) 0.053(6) Uani 1 1 d D U . . .
C5 C 0.598(8) 0.916(5) 0.110(10) 0.098(13) Uani 1 1 d D U . . .
H5A H 0.671860 1.004007 0.189944 0.117 Uiso 1.000(11) 1 calc R U P . .
H5B H 0.503652 0.895181 0.130487 0.117 Uiso 1.000(11) 1 calc R U P . .
C11 C 0.534(8) 0.304(4) 0.386(11) 0.051(9) Uani 1 1 d D U . . .
H11A H 0.463595 0.226519 0.296378 0.061 Uiso 1 1 calc R U . . .
H11B H 0.560438 0.255278 0.449327 0.061 Uiso 1 1 calc R U . . .
C8 C 1.315(6) 0.912(4) 0.320(8) 0.029(7) Uani 1 1 d D U . . .
H8A H 1.307224 0.850796 0.225770 0.034 Uiso 1 1 calc R U . . .
H8B H 1.286197 1.006498 0.322937 0.034 Uiso 1 1 calc R U . . .
O3 O 0.631(4) 0.429(4) -0.203(6) 0.053(5) Uani 1 1 d D U . . .
C6 C 0.559(6) 0.956(6) -0.013(10) 0.104(15) Uani 1 1 d D U . . .
H6A H 0.649660 1.019272 -0.013692 0.125 Uiso 1 1 calc R U . . .
H6B H 0.515180 0.864904 -0.099981 0.125 Uiso 1 1 calc R U . . .
C12 C 0.454(3) 0.426(2) 0.440(3) 0.049(10) Uani 1 1 d D U . . .
H12A H 0.401182 0.450056 0.363203 0.058 Uiso 1 1 calc R U . . .
H12B H 0.373506 0.380287 0.465578 0.058 Uiso 1 1 calc R U . . .
C9 C 1.480(6) 0.950(3) 0.416(8) 0.026(8) Uani 1 1 d D U . . .
H9A H 1.546247 1.006509 0.385499 0.031 Uiso 1 1 calc R U . . .
H9B H 1.509363 0.853897 0.404322 0.031 Uiso 1 1 calc R U . . .


_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 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.49(5) . ?
N1 Cd1 2.27(4) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.495(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.496(19) . ?
Cd1 O4 2.34(11) . ?
Cd1 N2 2.27(5) . ?
Cd1 N4 2.26(2) . ?
Cd1 N3 2.339(19) . ?
Cd1 O1 2.52(6) . ?
C3 C3 1.49(2) 2_755 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O4 N6 1.29(3) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 C4 1.50(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C10 1.50(5) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 C7 1.50(5) . ?
O1 N5 1.27(3) . ?
O2 N5 1.28(3) . ?
N6 O5 1.28(3) . ?
N6 O6 1.28(3) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.493(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.493(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.50(2) . ?
N5 O3 1.27(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.49(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.492(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.50(2) . ?
C6 C6 1.485(17) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C12 C12 1.49(2) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C9 C9 1.65(14) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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
H1A N1 H1B 106.9 . . ?
C1 N1 H1A 107.3 . . ?
C1 N1 H1B 107.3 . . ?
C1 N1 Cd1 120(4) . . ?
Cd1 N1 H1A 107.3 . . ?
Cd1 N1 H1B 107.3 . . ?
N1 C1 H1C 109.0 . . ?
N1 C1 H1D 109.0 . . ?
N1 C1 C2 113(3) . . ?
H1C C1 H1D 107.8 . . ?
C2 C1 H1C 109.0 . . ?
C2 C1 H1D 109.0 . . ?
C1 C2 H2A 108.3 . . ?
C1 C2 H2B 108.3 . . ?
C1 C2 C3 116(3) . . ?
H2A C2 H2B 107.4 . . ?
C3 C2 H2A 108.3 . . ?
C3 C2 H2B 108.3 . . ?
N1 Cd1 O4 76(2) . . ?
N1 Cd1 N2 172(2) . . ?
N1 Cd1 N3 89.3(10) . . ?
N1 Cd1 O1 93(2) . . ?
O4 Cd1 O1 158.7(11) . . ?
N2 Cd1 O4 110(2) . . ?
N2 Cd1 N3 85.1(12) . . ?
N2 Cd1 O1 83(2) . . ?
N4 Cd1 N1 98.4(12) . . ?
N4 Cd1 O4 86(2) . . ?
N4 Cd1 N2 88.3(14) . . ?
N4 Cd1 N3 167.4(18) . . ?
N4 Cd1 O1 77(2) . . ?
N3 Cd1 O4 85.9(18) . . ?
N3 Cd1 O1 112.5(18) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C3 C3 C2 111(5) 2_755 . ?
C3 C3 H3A 109.5 2_755 . ?
C3 C3 H3B 109.5 2_755 . ?
H3A C3 H3B 108.1 . . ?
N6 O4 Cd1 104(6) . . ?
Cd1 N2 H2C 108.4 . . ?
Cd1 N2 H2D 108.4 . . ?
H2C N2 H2D 107.5 . . ?
C4 N2 Cd1 115(2) . . ?
C4 N2 H2C 108.4 . . ?
C4 N2 H2D 108.4 . . ?
Cd1 N4 H4A 106.2 . . ?
Cd1 N4 H4B 106.2 . . ?
H4A N4 H4B 106.4 . . ?
C10 N4 Cd1 124(3) . . ?
C10 N4 H4A 106.2 . . ?
C10 N4 H4B 106.2 . . ?
Cd1 N3 H3C 107.5 . . ?
Cd1 N3 H3D 107.5 . . ?
H3C N3 H3D 107.0 . . ?
C7 N3 Cd1 119(3) . . ?
C7 N3 H3C 107.5 . . ?
C7 N3 H3D 107.5 . . ?
N5 O1 Cd1 109(3) . . ?
O5 N6 O4 123(6) . . ?
O5 N6 O6 114(4) . . ?
O6 N6 O4 123(5) . . ?
N2 C4 H4C 110.7 . . ?
N2 C4 H4D 110.7 . . ?
N2 C4 C5 105(5) . . ?
H4C C4 H4D 108.8 . . ?
C5 C4 H4C 110.7 . . ?
C5 C4 H4D 110.7 . . ?
N4 C10 H10A 108.8 . . ?
N4 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 N4 114(5) . . ?
C11 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
N3 C7 H7A 110.1 . . ?
N3 C7 H7B 110.1 . . ?
N3 C7 C8 108(4) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.1 . . ?
C8 C7 H7B 110.1 . . ?
O1 N5 O2 109(4) . . ?
O1 N5 O3 119(5) . . ?
O3 N5 O2 130(4) . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113(5) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 C10 112(2) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 C7 111(4) . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C5 C6 H6A 111.7 . . ?
C5 C6 H6B 111.7 . . ?
C6 C6 C5 100(7) 2_675 . ?
C6 C6 H6A 111.7 2_675 . ?
C6 C6 H6B 111.7 2_675 . ?
H6A C6 H6B 109.5 . . ?
C11 C12 H12A 107.3 . . ?
C11 C12 H12B 107.3 . . ?
C12 C12 C11 120(5) 2_666 . ?
C12 C12 H12A 107.3 2_666 . ?
C12 C12 H12B 107.3 2_666 . ?
H12A C12 H12B 106.9 . . ?
C8 C9 C9 118(4) . 2_876 ?
C8 C9 H9A 107.8 . . ?
C8 C9 H9B 107.8 . . ?
C9 C9 H9A 107.8 2_876 . ?
C9 C9 H9B 107.8 2_876 . ?
H9A C9 H9B 107.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 171(5) . . . . ?
C1 C2 C3 C3 63(6) . . . 2_755 ?
Cd1 N1 C1 C2 172(4) . . . . ?
Cd1 O4 N6 O5 32(4) . . . . ?
Cd1 O4 N6 O6 -148(3) . . . . ?
Cd1 N2 C4 C5 -166(4) . . . . ?
Cd1 N4 C10 C11 173(4) . . . . ?
Cd1 N3 C7 C8 165(2) . . . . ?
Cd1 O1 N5 O2 16(4) . . . . ?
Cd1 O1 N5 O3 -152(4) . . . . ?
N2 C4 C5 C6 -178(5) . . . . ?
N4 C10 C11 C12 -56(9) . . . . ?
N3 C7 C8 C9 -176(2) . . . . ?
C4 C5 C6 C6 158(6) . . . 2_675 ?
C10 C11 C12 C12 -46(10) . . . 2_666 ?
C7 C8 C9 C9 -57(5) . . . 2_876 ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.852
_oxdiff_exptl_absorpt_empirical_full_min 0.564
####################################################################### 
# 
# 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_2_1_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262348'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_2_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.257 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_2_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.74 Note
RESPONSE: The data/parameter ratio is affected by the access limits of 
the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT342_2_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.05583 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_2_1_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       2076 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N6 O6'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd N4 O6 C6 H12'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.264(3)
_cell_length_b                   9.585(3)
_cell_length_c                   11.069(4)
_cell_angle_alpha                110.41(3)
_cell_angle_beta                 105.98(3)
_cell_angle_gamma                97.17(3)
_cell_volume                     858.6(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7410
_cell_measurement_theta_min      2.8620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 0.257
_diffrn_reflns_Laue_measured_fraction_max 0.199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5871
_diffrn_reflns_point_group_measured_fraction_full 0.257
_diffrn_reflns_point_group_measured_fraction_max 0.199
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.899
_diffrn_reflns_theta_min         2.886
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.257
_diffrn_measured_fraction_theta_max 0.199
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 2.10(2) GPa
 (2100000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -16.00  32.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -16.00  32.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -12.00  15.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -12.00  15.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0338036000
_diffrn_orient_matrix_UB_12      0.0438271000
_diffrn_orient_matrix_UB_13      -0.0297199000
_diffrn_orient_matrix_UB_21      0.0709034000
_diffrn_orient_matrix_UB_22      -0.0200504000
_diffrn_orient_matrix_UB_23      0.0217882000
_diffrn_orient_matrix_UB_31      -0.0240650000
_diffrn_orient_matrix_UB_32      -0.0656474000
_diffrn_orient_matrix_UB_33      -0.0627533000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                517
_reflns_number_total             985
_reflns_odcompleteness_completeness 20.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.83
_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       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         985
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0732
_refine_ls_restrained_S_all      0.953
_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)+(0.1421P)²+0.4947P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2402
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 H4B-H6A_$1
 2 with sigma of 0.02
 C4-N2
 1.4 with sigma of 0.02
 C10-N4
 1.4 with sigma of 0.02
 H4A-H12A
 2 with sigma of 0.02
 O3-N5 \\sim O1-N5 \\sim O2-N5
 with sigma of 0.02
 O4-N6 \\sim O5-N6 \\sim O6-N6
 with sigma of 0.02
 C5-C4 \\sim C6-C5
 with sigma of 0.02
 C9-C8 \\sim C8-C7
 with sigma of 0.02
 C10-C11 \\sim C11-C12
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim N6 \\sim O6: within 2A with sigma of 0.05 and sigma for
terminal atoms of 0.1 within 2A
Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N4) = Uanis(C10) = Uanis(C11) = Uanis(C12)
4. Rigid body (RIGU) restrains
 C10, N3, Cd1, C7, N4, N1, N2, O4, O1, C8, C1, C4, N6, N5, C9, C11, C2, C5, O5,
  O6, O2, O3, C12, C3, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B), C1(H1C,H1D), C4(H4C,H4D),
 C7(H7A,H7B), C2(H2C,H2D), C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C6(H6A,H6B),
 C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B), C12(H12A,H12B)
;
_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
N3 N 1.040(3) 0.783(3) 0.268(3) 0.110(16) Uani 1 1 d . . . . .
H3A H 1.043908 0.762296 0.184229 0.132 Uiso 1 1 calc R U . . .
H3B H 1.008941 0.868984 0.293027 0.132 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8525(3) 0.5943(4) 0.2485(3) 0.090(6) Uani 1 1 d . . . . .
N1 N 1.017(3) 0.430(3) 0.252(3) 0.12(2) Uani 1 1 d . . . . .
H1A H 1.101065 0.470591 0.240419 0.149 Uiso 1 1 calc R U . . .
H1B H 1.046550 0.430542 0.335927 0.149 Uiso 1 1 calc R U . . .
O1 O 0.674(3) 0.432(4) 0.001(3) 0.115(18) Uani 1 1 d D . . . .
N2 N 0.690(3) 0.757(3) 0.216(3) 0.118(17) Uani 1 1 d D . . . .
H2A H 0.598357 0.716903 0.216040 0.142 Uiso 1 1 calc R U . . .
H2B H 0.729396 0.846729 0.287700 0.142 Uiso 1 1 calc R U . . .
O2 O 0.863(3) 0.544(4) -0.019(3) 0.13(2) Uani 1 1 d D . . . .
N4 N 0.643(3) 0.455(3) 0.265(4) 0.147(14) Uani 1 1 d D . . . .
H4A H 0.584924 0.517112 0.295143 0.176 Uiso 1 1 calc DR U . . .
H4B H 0.584881 0.383989 0.182453 0.176 Uiso 1 1 calc DR U . . .
C1 C 0.961(5) 0.274(5) 0.156(4) 0.09(4) Uani 1 1 d . . . . .
H1C H 0.913600 0.270168 0.064611 0.112 Uiso 1 1 calc R U . . .
H1D H 0.883113 0.221210 0.178637 0.112 Uiso 1 1 calc R U . . .
N5 N 0.734(3) 0.464(3) -0.072(3) 0.099(19) Uani 1 1 d D . . . .
C4 C 0.668(3) 0.784(4) 0.097(3) 0.10(2) Uani 1 1 d D . . . .
H4C H 0.608177 0.691125 0.016245 0.124 Uiso 1 1 calc R U . . .
H4D H 0.766005 0.817869 0.088416 0.124 Uiso 1 1 calc R U . . .
C7 C 1.205(4) 0.817(5) 0.363(3) 0.09(2) Uani 1 1 d D . . . .
H7A H 1.236138 0.721482 0.349762 0.109 Uiso 1 1 calc R U . . .
H7B H 1.209040 0.864223 0.456945 0.109 Uiso 1 1 calc R U . . .
C2 C 1.099(4) 0.194(4) 0.159(3) 0.10(4) Uani 1 1 d . . . . .
H2C H 1.166836 0.235443 0.120863 0.114 Uiso 1 1 calc R U . . .
H2D H 1.157968 0.215588 0.253704 0.114 Uiso 1 1 calc R U . . .
O3 O 0.644(3) 0.423(3) -0.186(3) 0.14(2) Uani 1 1 d D . . . .
C5 C 0.585(4) 0.899(4) 0.111(4) 0.14(3) Uani 1 1 d D . . . .
H5A H 0.489686 0.864084 0.123596 0.171 Uiso 1 1 calc R U . . .
H5B H 0.646599 0.990056 0.192792 0.171 Uiso 1 1 calc R U . . .
C8 C 1.318(4) 0.925(4) 0.336(3) 0.10(2) Uani 1 1 d D . . . .
H8A H 1.289318 1.021635 0.351783 0.120 Uiso 1 1 calc R U . . .
H8B H 1.311904 0.879040 0.240722 0.120 Uiso 1 1 calc R U . . .
C3 C 1.042(4) 0.024(5) 0.080(4) 0.12(5) Uani 1 1 d . . . . .
H3C H 0.969267 -0.015423 0.115814 0.149 Uiso 1 1 calc R U . . .
H3D H 1.128397 -0.022335 0.093336 0.149 Uiso 1 1 calc R U . . .
C6 C 0.551(4) 0.937(3) -0.003(5) 0.17(3) Uani 1 1 d D U . . .
H6A H 0.496149 0.843783 -0.084333 0.208 Uiso 1 1 calc R U . . .
H6B H 0.648037 0.975746 -0.011753 0.208 Uiso 1 1 calc R U . . .
C9 C 1.487(3) 0.954(4) 0.431(3) 0.09(3) Uani 1 1 d D . . . .
H9A H 1.509495 0.855900 0.424245 0.108 Uiso 1 1 calc R U . . .
H9B H 1.557099 1.003121 0.398780 0.108 Uiso 1 1 calc R U . . .
O5 O 0.869(3) 0.854(4) 0.510(3) 0.15(4) Uani 1 1 d D U . . .
O4 O 1.003(3) 0.689(4) 0.509(3) 0.129(19) Uani 1 1 d D U . . .
N6 N 0.988(3) 0.819(3) 0.557(3) 0.09(2) Uani 1 1 d D U . . .
O6 O 1.091(3) 0.909(4) 0.658(3) 0.13(4) Uani 1 1 d D U . . .
C11 C 0.537(4) 0.314(6) 0.373(4) 0.147(14) Uani 1 1 d D . . . .
H11A H 0.468033 0.236654 0.284962 0.176 Uiso 1 1 calc R U . . .
H11B H 0.563772 0.262871 0.435127 0.176 Uiso 1 1 calc R U . . .
C10 C 0.690(5) 0.384(5) 0.355(4) 0.147(14) Uani 1 1 d D U . . .
H10A H 0.763327 0.457405 0.442240 0.176 Uiso 1 1 calc R U . . .
H10B H 0.738492 0.303034 0.316247 0.176 Uiso 1 1 calc R U . . .
C12 C 0.448(3) 0.438(5) 0.431(3) 0.147(14) Uani 1 1 d D . . . .
H12A H 0.413955 0.484497 0.366320 0.176 Uiso 1 1 calc DR U . . .
H12B H 0.356617 0.388493 0.441119 0.176 Uiso 1 1 calc R U . . .


_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
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 Cd1 2.25(5) . ?
N3 C7 1.51(3) . ?
Cd1 N1 2.323(17) . ?
Cd1 O1 2.56(2) . ?
Cd1 N2 2.34(2) . ?
Cd1 N4 2.31(4) . ?
Cd1 O4 2.59(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.42(3) . ?
O1 N5 1.20(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C4 1.40(2) . ?
O2 N5 1.20(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C10 1.40(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.57(3) . ?
N5 O3 1.20(2) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.41(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.54(4) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.49(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.40(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.55(3) . ?
C3 C3 1.59(7) 2_755 ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C6 C6 1.63(5) 2_675 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 C9 1.41(5) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O5 N6 1.216(14) . ?
O4 N6 1.215(16) . ?
N6 O6 1.199(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.59(4) . ?
C11 C12 1.59(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C12 1.52(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?

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
H3A N3 H3B 106.7 . . ?
Cd1 N3 H3A 106.9 . . ?
Cd1 N3 H3B 106.9 . . ?
C7 N3 H3A 106.9 . . ?
C7 N3 H3B 106.9 . . ?
C7 N3 Cd1 122(3) . . ?
N3 Cd1 N1 92.2(13) . . ?
N3 Cd1 O1 113.7(13) . . ?
N3 Cd1 N2 84.7(11) . . ?
N3 Cd1 N4 165.0(8) . . ?
N3 Cd1 O4 81.8(14) . . ?
N1 Cd1 O1 95.2(6) . . ?
N1 Cd1 N2 172.1(15) . . ?
N1 Cd1 O4 78.0(7) . . ?
O1 Cd1 O4 163.5(15) . . ?
N2 Cd1 O1 79.6(7) . . ?
N2 Cd1 O4 108.6(7) . . ?
N4 Cd1 N1 99.8(15) . . ?
N4 Cd1 O1 74.5(14) . . ?
N4 Cd1 N2 84.5(13) . . ?
N4 Cd1 O4 91.8(14) . . ?
Cd1 N1 H1A 107.6 . . ?
Cd1 N1 H1B 107.6 . . ?
H1A N1 H1B 107.1 . . ?
C1 N1 Cd1 118.8(12) . . ?
C1 N1 H1A 107.6 . . ?
C1 N1 H1B 107.6 . . ?
N5 O1 Cd1 107(2) . . ?
Cd1 N2 H2A 108.1 . . ?
Cd1 N2 H2B 108.1 . . ?
H2A N2 H2B 107.3 . . ?
C4 N2 Cd1 116.6(17) . . ?
C4 N2 H2A 108.1 . . ?
C4 N2 H2B 108.1 . . ?
Cd1 N4 H4A 109.4 . . ?
Cd1 N4 H4B 109.4 . . ?
H4A N4 H4B 108.0 . . ?
C10 N4 Cd1 111(2) . . ?
C10 N4 H4A 109.4 . . ?
C10 N4 H4B 109.4 . . ?
N1 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
N1 C1 C2 110(2) . . ?
H1C C1 H1D 108.2 . . ?
C2 C1 H1C 109.7 . . ?
C2 C1 H1D 109.7 . . ?
O1 N5 O2 117(4) . . ?
O3 N5 O1 112(4) . . ?
O3 N5 O2 130(4) . . ?
N2 C4 H4C 110.7 . . ?
N2 C4 H4D 110.7 . . ?
N2 C4 C5 105(3) . . ?
H4C C4 H4D 108.8 . . ?
C5 C4 H4C 110.7 . . ?
C5 C4 H4D 110.7 . . ?
N3 C7 H7A 109.2 . . ?
N3 C7 H7B 109.2 . . ?
N3 C7 C8 112(4) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C1 C2 H2C 109.4 . . ?
C1 C2 H2D 109.4 . . ?
H2C C2 H2D 108.0 . . ?
C3 C2 C1 111(3) . . ?
C3 C2 H2C 109.4 . . ?
C3 C2 H2D 109.4 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 C4 112(3) . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C7 C8 C9 111(4) . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C2 C3 C3 114(6) . 2_755 ?
C2 C3 H3C 108.9 . . ?
C2 C3 H3D 108.9 . . ?
C3 C3 H3C 108.9 2_755 . ?
C3 C3 H3D 108.9 2_755 . ?
H3C C3 H3D 107.7 . . ?
C5 C6 C6 115(6) . 2_675 ?
C5 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
C6 C6 H6A 108.6 2_675 . ?
C6 C6 H6B 108.6 2_675 . ?
H6A C6 H6B 107.6 . . ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C9 C9 C8 113(3) 2_876 . ?
C9 C9 H9A 109.0 2_876 . ?
C9 C9 H9B 109.0 2_876 . ?
H9A C9 H9B 107.8 . . ?
N6 O4 Cd1 103.9(18) . . ?
O4 N6 O5 121.5(18) . . ?
O6 N6 O5 121.6(18) . . ?
O6 N6 O4 116.7(18) . . ?
H11A C11 H11B 107.7 . . ?
C10 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
C12 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
C12 C11 C10 114(4) . . ?
N4 C10 C11 106(3) . . ?
N4 C10 H10A 110.6 . . ?
N4 C10 H10B 110.6 . . ?
C11 C10 H10A 110.6 . . ?
C11 C10 H10B 110.6 . . ?
H10A C10 H10B 108.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C12 C12 C11 111(3) 2_666 . ?
C12 C12 H12A 109.5 2_666 . ?
C12 C12 H12B 109.5 2_666 . ?
H12A C12 H12B 108.1 . . ?

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
N3 C7 C8 C9 -178.1(15) . . . . ?
Cd1 N3 C7 C8 168(2) . . . . ?
Cd1 N1 C1 C2 170(4) . . . . ?
Cd1 O1 N5 O2 8(4) . . . . ?
Cd1 O1 N5 O3 -163.1(15) . . . . ?
Cd1 N2 C4 C5 -172(2) . . . . ?
Cd1 N4 C10 C11 172(2) . . . . ?
Cd1 O4 N6 O5 35(5) . . . . ?
Cd1 O4 N6 O6 -150(4) . . . . ?
N1 C1 C2 C3 169(5) . . . . ?
N2 C4 C5 C6 -179(3) . . . . ?
C1 C2 C3 C3 65(7) . . . 2_755 ?
C4 C5 C6 C6 177(4) . . . 2_675 ?
C7 C8 C9 C9 -71(6) . . . 2_876 ?
C10 C11 C12 C12 -58(6) . . . 2_666 ?
C12 C11 C10 N4 -58(4) . . . . ?

_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 3.652
_oxdiff_exptl_absorpt_empirical_full_min 0.594
####################################################################### 
# 
# 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_0_4_GPa_Cd2_HDA_3_NO3_4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262360'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_0_4_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.353 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_0_4_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.77 Note
RESPONSE: The data/parameter ratio is affected by the access limits 
of the DAC.
;
_vrf_PLAT342_0_4_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.055 Ang.
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_vrf_PLAT911_0_4_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        913 Report
RESPONSE: The data come from high-pressure studies and are limited 
by the DAC opening angle.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C8 N4 O4'
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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.316(10)
_cell_length_b                   6.8838(4)
_cell_length_c                   15.7250(18)
_cell_angle_alpha                90
_cell_angle_beta                 97.17(3)
_cell_angle_gamma                90
_cell_volume                     1537.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2675
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2400
_cell_measurement_theta_min      1.8280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.08
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.353
_diffrn_reflns_Laue_measured_fraction_max 0.333
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12275
_diffrn_reflns_point_group_measured_fraction_full 0.353
_diffrn_reflns_point_group_measured_fraction_max 0.333
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.611
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.353
_diffrn_measured_fraction_theta_max 0.333
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.40(2) GPa
 (400000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
 17  ω    -23.00   9.00   1.00   25.00    --    0.12 -13.00   3.00   32
 18  ω    -22.00  11.00   1.00   25.00    --   30.76  53.00 -17.00   33
 19  ω     89.00 114.00   1.00   25.00    --   30.76 134.00 -57.00   25
 20  ω     -9.00  19.00   1.00   25.00    --  -30.53 -81.00-151.00   28
 21  ω      7.00  33.00   1.00   25.00    --  -30.53-114.00-135.00   26
 22  ω     58.00  90.00   1.00   25.00    --    0.12-178.00-120.00   32
 23  ω    -21.00   5.00   1.00   25.00    --    0.12  82.00 153.00   26
 24  ω    -25.00   0.00   1.00   25.00    --   30.76  53.00 162.00   25
 25  ω    -68.00 -15.00   1.00   25.00    --  -30.53  82.00 153.00   53
 26  ω    -24.00  18.00   1.00   25.00    --   30.76   0.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489362000
_diffrn_orient_matrix_UB_12      -0.0038180000
_diffrn_orient_matrix_UB_13      -0.0140709000
_diffrn_orient_matrix_UB_21      0.0030291000
_diffrn_orient_matrix_UB_22      0.0897910000
_diffrn_orient_matrix_UB_23      -0.0216788000
_diffrn_orient_matrix_UB_31      0.0091288000
_diffrn_orient_matrix_UB_32      -0.0506459000
_diffrn_orient_matrix_UB_33      -0.0374047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                727
_reflns_number_total             1061
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0479
_refine_ls_restrained_S_all      0.994
_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)+(0.0565P)²+5.0724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1301
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.06
Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of
0.06
Uanis(N5) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) = Uanis(O6)
3. Rigid body (RIGU) restrains
 C3, Cd1, O1, N1, N3, O4, N4, C1, C7, N5, O2, O3, C2, C8, O6, O5, C9, C4, C5,
 C6, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N5, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), N3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C8(H8A,H8B),
 C7(H7A,H7B), C6(H6A,H6B), C1(H1C,H1D), C2(H2C,H2D), C4(H4A,H4B), C3(H3C,H3D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 0.57831(16) 0.31792(10) 0.34886(7) 0.0490(18) Uani 1 1 d . . . . .
O2 O 0.7117(14) -0.2102(9) 0.2926(6) 0.059(9) Uani 1 1 d . . . . .
O6 O 0.4308(15) 0.7701(12) 0.4742(7) 0.079(4) Uani 1 1 d . . . . .
N4 N 0.663(2) -0.0618(12) 0.3027(9) 0.041(8) Uani 1 1 d . . . . .
O1 O 0.6801(16) 0.0342(11) 0.3692(7) 0.077(7) Uani 1 1 d . . . . .
N2 N -0.0907(19) -0.0478(13) 0.2817(8) 0.050(6) Uani 1 1 d . U . . .
H2A H -0.100875 0.078849 0.273782 0.060 Uiso 1 1 calc R U . . .
H2B H -0.141950 -0.097096 0.300278 0.060 Uiso 1 1 calc R U . . .
N1 N 0.454(2) 0.1337(15) 0.3620(8) 0.061(7) Uani 1 1 d . . . . .
H1A H 0.475761 0.015265 0.376416 0.073 Uiso 1 1 calc R U . . .
H1B H 0.428049 0.179199 0.406362 0.073 Uiso 1 1 calc R U . . .
N5 N 0.4455(17) 0.6543(13) 0.4202(6) 0.042(6) Uani 1 1 d . U . . .
N3 N 0.692(2) 0.4801(15) 0.4253(10) 0.062(5) Uani 1 1 d . . . . .
H3A H 0.691300 0.600991 0.405203 0.074 Uiso 1 1 calc R U . . .
H3B H 0.678017 0.486622 0.478926 0.074 Uiso 1 1 calc R U . . .
O3 O 0.601(2) -0.0034(16) 0.2490(8) 0.077(8) Uani 1 1 d . . . . .
O4 O 0.5074(16) 0.6643(12) 0.3768(7) 0.079(4) Uani 1 1 d . U . . .
C5 C 0.069(3) 0.0460(15) 0.3336(10) 0.044(6) Uani 1 1 d . U . . .
H5A H 0.054344 0.182954 0.337445 0.053 Uiso 1 1 calc R U . . .
H5B H 0.083026 0.020643 0.275805 0.053 Uiso 1 1 calc R U . . .
C9 C 0.962(5) 0.4456(16) 0.4733(13) 0.055(5) Uani 1 1 d . U . . .
H9A H 0.964215 0.310398 0.490752 0.067 Uiso 1 1 calc R U . . .
H9B H 0.973273 0.450811 0.413811 0.067 Uiso 1 1 calc R U . . .
C8 C 0.865(4) 0.5235(18) 0.4799(14) 0.062(5) Uani 1 1 d . . . . .
H8A H 0.861598 0.657029 0.460075 0.075 Uiso 1 1 calc R U . . .
H8B H 0.854438 0.523724 0.539723 0.075 Uiso 1 1 calc R U . . .
C7 C 0.784(4) 0.4051(19) 0.4274(13) 0.060(5) Uani 1 1 d . . . . .
H7A H 0.798748 0.394964 0.368839 0.072 Uiso 1 1 calc R U . . .
H7B H 0.785221 0.274526 0.450649 0.072 Uiso 1 1 calc R U . . .
C6 C -0.014(3) -0.0694(16) 0.3494(11) 0.046(6) Uani 1 1 d . U . . .
H6A H 0.003321 -0.205389 0.354762 0.055 Uiso 1 1 calc R U . . .
H6B H -0.034672 -0.028466 0.403093 0.055 Uiso 1 1 calc R U . . .
O5 O 0.3935(16) 0.5175(12) 0.4076(7) 0.089(7) Uani 1 1 d . . . . .
C1 C 0.380(2) 0.1112(15) 0.2917(10) 0.049(7) Uani 1 1 d . . . . .
H1C H 0.405550 0.043321 0.245701 0.059 Uiso 1 1 calc R U . . .
H1D H 0.361128 0.239485 0.270553 0.059 Uiso 1 1 calc R U . . .
C2 C 0.295(2) 0.0066(13) 0.3106(9) 0.052(7) Uani 1 1 d . . . . .
H2C H 0.311904 -0.127023 0.324840 0.062 Uiso 1 1 calc R U . . .
H2D H 0.249637 0.005067 0.259348 0.062 Uiso 1 1 calc R U . . .
C4 C 0.161(3) -0.0015(16) 0.3997(9) 0.048(6) Uani 1 1 d . U . . .
H4A H 0.147292 0.033302 0.456745 0.058 Uiso 1 1 calc R U . . .
H4B H 0.170998 -0.140680 0.399301 0.058 Uiso 1 1 calc R U . . .
C3 C 0.248(2) 0.0953(15) 0.3843(9) 0.048(6) Uani 1 1 d . U . . .
H3C H 0.292523 0.089340 0.436315 0.058 Uiso 1 1 calc R U . . .
H3D H 0.235200 0.231210 0.371660 0.058 Uiso 1 1 calc R U . . .


_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
Cd1 O1 2.434(15) . ?
Cd1 N2 2.278(10) 2 ?
Cd1 N1 2.21(2) . ?
Cd1 N3 2.20(3) . ?
Cd1 O4 2.649(11) . ?
O2 N4 1.257(19) . ?
O6 N5 1.202(11) . ?
N4 O1 1.235(17) . ?
N4 O3 1.22(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C6 1.44(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.44(4) . ?
N5 O4 1.19(2) . ?
N5 O5 1.20(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.42(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.48(4) . ?
C5 C4 1.60(5) . ?
C9 C9 1.50(11) 3_766 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.50(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.56(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.48(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.534(17) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.47(4) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?

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 Cd1 O4 159.3(6) . . ?
N2 Cd1 O1 109.4(5) 2 . ?
N2 Cd1 O4 81.9(4) 2 . ?
N1 Cd1 O1 90.1(7) . . ?
N1 Cd1 N2 118.1(8) . 2 ?
N1 Cd1 O4 99.9(6) . . ?
N3 Cd1 O1 87.0(6) . . ?
N3 Cd1 N2 98.7(6) . 2 ?
N3 Cd1 N1 141.8(5) . . ?
N3 Cd1 O4 74.0(7) . . ?
O1 N4 O2 119(2) . . ?
O3 N4 O2 123.3(14) . . ?
O3 N4 O1 117.4(16) . . ?
N4 O1 Cd1 105.5(15) . . ?
Cd1 N2 H2A 107.5 2_545 . ?
Cd1 N2 H2B 107.5 2_545 . ?
H2A N2 H2B 107.0 . . ?
C6 N2 Cd1 119.2(14) . 2_545 ?
C6 N2 H2A 107.5 . . ?
C6 N2 H2B 107.5 . . ?
Cd1 N1 H1A 107.1 . . ?
Cd1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C1 N1 Cd1 120.9(9) . . ?
C1 N1 H1A 107.1 . . ?
C1 N1 H1B 107.1 . . ?
O6 N5 O5 118.5(17) . . ?
O4 N5 O6 125.2(17) . . ?
O4 N5 O5 116.3(11) . . ?
Cd1 N3 H3A 108.1 . . ?
Cd1 N3 H3B 108.1 . . ?
H3A N3 H3B 107.3 . . ?
C7 N3 Cd1 116.8(14) . . ?
C7 N3 H3A 108.1 . . ?
C7 N3 H3B 108.1 . . ?
N5 O4 Cd1 111.9(7) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C6 C5 C4 113.1(13) . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
C9 C9 H9A 108.9 3_766 . ?
C9 C9 H9B 108.9 3_766 . ?
C9 C9 C8 113.5(16) 3_766 . ?
H9A C9 H9B 107.7 . . ?
C8 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C9 C8 C7 113.8(14) . . ?
H8A C8 H8B 107.7 . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
N3 C7 C8 116.6(15) . . ?
N3 C7 H7A 108.1 . . ?
N3 C7 H7B 108.1 . . ?
C8 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
N2 C6 C5 112.1(14) . . ?
N2 C6 H6A 109.2 . . ?
N2 C6 H6B 109.2 . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N1 C1 H1C 108.2 . . ?
N1 C1 H1D 108.2 . . ?
N1 C1 C2 116.4(13) . . ?
H1C C1 H1D 107.3 . . ?
C2 C1 H1C 108.2 . . ?
C2 C1 H1D 108.2 . . ?
C1 C2 H2C 108.8 . . ?
C1 C2 H2D 108.8 . . ?
C1 C2 C3 113.9(13) . . ?
H2C C2 H2D 107.7 . . ?
C3 C2 H2C 108.8 . . ?
C3 C2 H2D 108.8 . . ?
C5 C4 H4A 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C3 C4 C5 116.6(12) . . ?
C3 C4 H4A 108.1 . . ?
C3 C4 H4B 108.1 . . ?
C2 C3 H3C 108.8 . . ?
C2 C3 H3D 108.8 . . ?
C4 C3 C2 114.0(14) . . ?
C4 C3 H3C 108.8 . . ?
C4 C3 H3D 108.8 . . ?
H3C C3 H3D 107.7 . . ?

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
Cd1 N2 C6 C5 70.4(11) 2_545 . . . ?
Cd1 N1 C1 C2 -172.2(9) . . . . ?
Cd1 N3 C7 C8 178.6(7) . . . . ?
O2 N4 O1 Cd1 174.3(12) . . . . ?
O6 N5 O4 Cd1 142.8(15) . . . . ?
N1 C1 C2 C3 56(2) . . . . ?
O3 N4 O1 Cd1 -4(2) . . . . ?
C5 C4 C3 C2 -76(2) . . . . ?
C9 C9 C8 C7 -177.5(11) 3_766 . . . ?
C9 C8 C7 N3 -175.1(11) . . . . ?
C6 C5 C4 C3 175.2(9) . . . . ?
O5 N5 O4 Cd1 -38(2) . . . . ?
C1 C2 C3 C4 176(2) . . . . ?
C4 C5 C6 N2 -170.7(11) . . . . ?

_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 383.074
_oxdiff_exptl_absorpt_empirical_full_min 0.780
####################################################################### 
# 
# 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_3_7_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262353'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_3_7_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.358 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_3_7_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.88 Note
RESPONSE: The data/parameter ratio is affected by the access limits of t
he DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT084_3_7_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.41 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT342_3_7_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.08417 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_3_7_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1955 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-08
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H31 Cd N6 O6'
_chemical_formula_sum            'C12 H31 Cd N6 O6'
_chemical_formula_weight         467.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
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'
Cd Cd -0.8075 1.2024 '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      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                   9.127(2)
_cell_length_b                   9.5346(18)
_cell_length_c                   10.805(5)
_cell_angle_alpha                110.62(3)
_cell_angle_beta                 106.02(3)
_cell_angle_gamma                97.498(18)
_cell_volume                     818.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2552
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1220
_cell_measurement_theta_min      2.3370
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.789
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             482
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 9 0.0485
2 13 -5 0.0555
9 -10 -4 0.0737
8 9 -8 0.0399
-10 -7 9 0.0309
10 7 -9 0.0309
-1 -13 4 0.0820
5 -3 12 0.0325
-5 3 -12 0.0325

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.0482 -1.7646 8.6797 -0.0181 0.8138 -0.5809
1.9624 12.7993 -4.8269 0.0208 -0.8368 -0.5471
9.0353 -9.6796 -3.5079 -0.0022 0.0091 1.0000
8.0721 9.2533 -7.9922 0.0254 -0.9994 -0.0254
-9.8129 -7.0543 8.9413 0.0012 0.9811 -0.1932
9.8129 7.0543 -8.9413 -0.0012 -0.9811 0.1932
-0.6117 -13.0573 3.6666 -0.0414 0.7692 0.6431
4.8817 -3.4286 11.6990 0.9942 -0.0058 0.1076
-4.8817 3.4286 -11.6990 -0.9942 0.0058 -0.1076

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1696
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.358
_diffrn_reflns_Laue_measured_fraction_max 0.200
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7462
_diffrn_reflns_point_group_measured_fraction_full 0.358
_diffrn_reflns_point_group_measured_fraction_max 0.200
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.172
_diffrn_reflns_theta_min         2.359
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.358
_diffrn_measured_fraction_theta_max 0.200
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 3.70(2) GPa
 (3700000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  13.00   0.75   13.50    --  -24.60  67.00 -23.00   96
  2  ω   -108.00 -72.75   0.75   13.50    --  -24.60 178.00  90.00   47
  3  ω     -8.00  16.00   0.75   13.50    --  -24.60 -81.00  29.00   32
  4  ω    -30.00  45.00   0.75   13.50    --  -24.60 -26.00   8.00  100
  5  ω    -37.00   6.50   0.75   13.50    --  -24.60   0.00-150.00   58
  6  ω    -13.00  22.25   0.75   13.50    --  -24.60 -38.00-180.00   47
  7  ω   -114.00 -72.00   0.75   13.50    --  -24.60-178.00 -90.00   56
  8  ω    -17.50  50.00   0.75   13.50    --   25.46 -39.00  12.00   90
  9  ω     67.50 108.00   0.75   13.50    --   25.46 178.00 -90.00   54
 10  ω    -37.00   6.50   0.75   13.50    --   25.46   0.00-150.00   58
 11  ω     74.00 107.00   0.75   13.50    --   25.46 178.00 120.00   44
 12  ω    -12.50  55.00   0.75   13.50    --   25.46 -53.00-162.00   90
 13  ω     72.00 107.25   0.75   13.50    --   25.46 178.00  90.00   47
 14  ω    -24.25   2.00   0.75   13.50    --   25.46  97.00 -35.00   35
 15  ω    -24.00  21.00   0.75   13.50    --  -24.60 -39.00-167.00   60
 16  ω    -24.00  21.00   0.75   13.50    --  -24.60 -39.00  12.00   60
 17  ω      7.00  35.50   0.75   13.50    --  -24.60-114.00-135.00   38
 18  ω    -50.00  25.00   0.75   13.50    --  -24.60  39.00 167.00  100
 19  ω    -20.00   8.50   0.75   13.50    --  -24.60 -53.00  17.00   38
 20  ω     -2.00  25.00   0.75   13.50    --  -24.60 -97.00  35.00   36
 21  ω     -9.00  16.50   0.75   13.50    --  -24.60 -81.00-151.00   34
 22  ω     34.75  67.00   0.75   13.50    --   25.46 -99.00-150.00   43
 23  ω    -20.00  24.25   0.75   13.50    --   25.46  39.00 167.00   59
 24  ω    -20.00  24.25   0.75   13.50    --   25.46  39.00 -12.00   59
 25  ω     34.75  61.00   0.75   13.50    --   25.46 -99.00  60.00   35
 26  ω    -37.00  36.50   0.75   13.50    --  -24.60   0.00   0.00   98
 27  ω    -35.25  33.00   0.75   13.50    --   25.46  13.00  -3.00   91
 28  ω     29.75  95.00   0.75   13.50    --   25.46-135.00-123.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0492524000
_diffrn_orient_matrix_UB_12      0.0206548000
_diffrn_orient_matrix_UB_13      0.0704804000
_diffrn_orient_matrix_UB_21      -0.0549174000
_diffrn_orient_matrix_UB_22      -0.0545316000
_diffrn_orient_matrix_UB_23      0.0064387000
_diffrn_orient_matrix_UB_31      0.0392899000
_diffrn_orient_matrix_UB_32      -0.0578771000
_diffrn_orient_matrix_UB_33      -0.0241550000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                539
_reflns_number_total             806
_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       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         806
_refine_ls_number_restraints     443
_refine_ls_R_factor_all          0.1802
_refine_ls_R_factor_gt           0.1337
_refine_ls_restrained_S_all      1.364
_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          0.3530
_refine_ls_wR_factor_ref         0.4103
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C6-C6_$1
 1.45 with sigma of 0.05
 C12-C12_$2
 1.45 with sigma of 0.05
 C3-C3_$3
 1.45 with sigma of 0.05
 C9-C9_$4
 1.45 with sigma of 0.05
 C5-C4
 1.45 with sigma of 0.02
 C5-C6
 1.45 with sigma of 0.02
 H12B_$2-H4A
 2.05 with sigma of 0.02
 H6B_$5-H10B
 2.05 with sigma of 0.02
 O5-N6 \\sim O4-N6 \\sim O6-N6 \\sim O1-N5 \\sim O2-N5 \\sim O3-N5
 with sigma of 0.05
 C9-C8 \\sim C8-C7 \\sim C2-C1 \\sim C3-C2 \\sim C11-C10 \\sim C12-C11 \\sim
C4-C5 \\sim C5-C6
 with sigma of 0.05
 N2-C4 \\sim N3-C7 \\sim N1-C1 \\sim N4-C10
 with sigma of 0.05
3. Rigid bond restraints
 C7, N3, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, N6, O5, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C11, C12, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O3, N5, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C4, C5, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim N3 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O4 \\sim N6 \\sim O5 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N4 \\sim C11 \\sim C12 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O3 \\sim N5 \\sim O2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C6 \\sim C4 \\sim C5 \\sim N2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(Cd1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C7) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) = Uanis(N6) = Uanis(O5) = Uanis(O6)
5. Rigid body (RIGU) restrains
 O4, N6, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, N3, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C11, C12, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O3, N5, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C4, C5, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H4C(0.5) H4D(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6,H6B), N4(H4A,H4B), C7(H7A,H7B), C3(H3A,H3B), C4(H4C,H4D), C11(H11A,
 H11B), C2(H2A,H2B), N3(H3C,H), C5(H5A,H5), N2(H2C,H2D), C8(H8A,H8B), C1(H1A,
 H1B), C9(H9A,H9B), C12(H12A,H12B), C10(H10A,H10B), N1(H1C,H1D)
;
_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
O4 O 0.982(9) 0.670(5) 0.480(13) 0.054(6) Uani 1 1 d D U . . .
C6 C 0.483(8) 0.926(5) 0.009(9) 0.109(15) Uani 1 1 d D U . . .
H6 H 0.429513 0.933605 0.076391 0.130 Uiso 1 1 calc R U . . .
H6B H 0.423761 0.838581 -0.079727 0.130 Uiso 1 1 calc R U . . .
N4 N 0.648(5) 0.451(4) 0.271(5) 0.062(9) Uani 1 1 d D U . . .
H4A H 0.595291 0.516323 0.309336 0.074 Uiso 1 1 calc DR U . . .
H4B H 0.582680 0.389277 0.184265 0.074 Uiso 1 1 calc R U . . .
C7 C 1.181(7) 0.812(4) 0.337(9) 0.039(7) Uani 1 1 d D U . . .
H7A H 1.211313 0.716231 0.327239 0.047 Uiso 1 1 calc R U . . .
H7B H 1.176533 0.856900 0.430948 0.047 Uiso 1 1 calc R U . . .
C3 C 1.038(6) 0.027(4) 0.076(3) 0.04(3) Uani 1 1 d D U . . .
H3A H 1.127719 -0.017591 0.090842 0.046 Uiso 1 1 calc R U . . .
H3B H 0.965165 -0.016342 0.110747 0.046 Uiso 1 1 calc R U . . .
C4 C 0.676(8) 0.786(6) 0.082(11) 0.078(11) Uani 1 1 d D U . . .
H4C H 0.600350 0.699912 -0.000790 0.093 Uiso 0.5 1 calc R U P A 1
H4D H 0.778639 0.781024 0.074369 0.093 Uiso 0.5 1 calc R U P A 1
C11 C 0.536(11) 0.296(6) 0.380(14) 0.064(9) Uani 1 1 d D U . . .
H11A H 0.574053 0.248061 0.443371 0.077 Uiso 1 1 calc R U . . .
H11B H 0.457085 0.217558 0.294176 0.077 Uiso 1 1 calc R U . . .
N6 N 0.963(6) 0.808(4) 0.537(7) 0.054(6) Uani 1 1 d D U . . .
C2 C 1.097(6) 0.198(3) 0.168(9) 0.03(2) Uani 1 1 d D U . . .
H2A H 1.147554 0.211459 0.264623 0.041 Uiso 1 1 calc R U . . .
H2B H 1.176787 0.242822 0.139511 0.041 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8423(8) 0.5939(4) 0.2460(12) 0.054(5) Uani 1 1 d . U . . .
N3 N 1.031(7) 0.770(4) 0.248(9) 0.041(7) Uani 1 1 d D U . . .
H3C H 1.034166 0.737474 0.161210 0.049 Uiso 1 1 calc R U . . .
H H 0.997734 0.856702 0.263221 0.049 Uiso 1 1 calc R U . . .
O1 O 0.673(7) 0.423(4) 0.010(9) 0.067(8) Uani 1 1 d D U . . .
C5 C 0.646(8) 0.925(6) 0.063(11) 0.095(12) Uani 1 1 d D U . . .
H5A H 0.696386 1.013040 0.153925 0.114 Uiso 1 1 calc R U . . .
H5 H 0.697797 0.941364 0.000133 0.114 Uiso 1 1 calc R U . . .
O3 O 0.637(6) 0.422(5) -0.203(8) 0.064(7) Uani 1 1 d D U . . .
N2 N 0.674(8) 0.752(4) 0.192(10) 0.064(9) Uani 1 1 d D U . . .
H2C H 0.575774 0.704554 0.175390 0.076 Uiso 1 1 calc R U . . .
H2D H 0.700985 0.840648 0.267695 0.076 Uiso 1 1 calc R U . . .
N5 N 0.725(6) 0.457(5) -0.078(6) 0.061(9) Uani 1 1 d D U . . .
C8 C 1.320(5) 0.920(4) 0.338(8) 0.045(8) Uani 1 1 d D U . . .
H8A H 1.296899 1.020135 0.360038 0.054 Uiso 1 1 calc R U . . .
H8B H 1.317553 0.883194 0.241026 0.054 Uiso 1 1 calc R U . . .
O5 O 0.846(6) 0.855(4) 0.489(8) 0.054(6) Uani 1 1 d D U . . .
C1 C 0.971(7) 0.285(4) 0.163(10) 0.04(2) Uani 1 1 d D U . . .
H1A H 0.918952 0.261205 0.064581 0.050 Uiso 1 1 calc R U . . .
H1B H 0.895001 0.236227 0.192653 0.050 Uiso 1 1 calc R U . . .
C9 C 1.492(4) 0.950(3) 0.428(4) 0.033(8) Uani 1 1 d D U . . .
H9A H 1.517318 0.853679 0.424806 0.040 Uiso 1 1 calc R U . . .
H9B H 1.561424 1.000943 0.394892 0.040 Uiso 1 1 calc R U . . .
C12 C 0.462(5) 0.422(3) 0.448(5) 0.044(9) Uani 1 1 d D U . . .
H12A H 0.388567 0.432921 0.369682 0.053 Uiso 1 1 calc R U . . .
H12B H 0.397785 0.375843 0.488525 0.053 Uiso 1 1 calc R U . . .
C10 C 0.670(7) 0.360(5) 0.345(8) 0.064(9) Uani 1 1 d D U . . .
H10A H 0.756736 0.419782 0.432475 0.077 Uiso 1 1 calc R U . . .
H10B H 0.703312 0.273166 0.291115 0.077 Uiso 1 1 calc DR U . . .
O6 O 1.076(7) 0.912(4) 0.636(9) 0.054(6) Uani 1 1 d D U . . .
O2 O 0.866(7) 0.533(4) -0.021(8) 0.078(10) Uani 1 1 d D U . . .
N1 N 0.992(7) 0.435(3) 0.230(9) 0.04(2) Uani 1 1 d D U . . .
H1C H 1.064636 0.475840 0.203641 0.048 Uiso 1 1 calc R U . . .
H1D H 1.041507 0.452935 0.319919 0.048 Uiso 1 1 calc R U . . .


_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
O4 N6 1.30(4) . ?
O4 Cd1 2.28(12) . ?
C6 C6 1.49(5) 2_675 ?
C6 H6 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.45(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 Cd1 2.23(3) . ?
N4 C10 1.37(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N3 1.35(6) . ?
C7 C8 1.52(3) . ?
C3 C3 1.45(6) 2_755 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.50(4) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C5 1.46(2) . ?
C4 N2 1.34(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.51(3) . ?
C11 C10 1.49(4) . ?
N6 O5 1.26(4) . ?
N6 O6 1.25(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.50(4) . ?
Cd1 N3 2.23(3) . ?
Cd1 O1 2.40(8) . ?
Cd1 N2 2.39(6) . ?
Cd1 N1 2.16(3) . ?
N3 H3C 0.8900 . ?
N3 H 0.8900 . ?
O1 N5 1.29(4) . ?
C5 H5A 0.9700 . ?
C5 H5 0.9700 . ?
O3 N5 1.27(5) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N5 O2 1.25(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.52(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 N1 1.32(4) . ?
C9 C9 1.45(5) 2_876 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C12 C12 1.45(5) 2_666 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 O4 Cd1 103(7) . . ?
C6 C6 H6 112.7 2_675 . ?
C6 C6 H6B 112.7 2_675 . ?
H6 C6 H6B 110.2 . . ?
C5 C6 C6 95(6) . 2_675 ?
C5 C6 H6 112.7 . . ?
C5 C6 H6B 112.7 . . ?
H4A N4 H4B 106.4 . . ?
Cd1 N4 H4A 106.3 . . ?
Cd1 N4 H4B 106.3 . . ?
C10 N4 H4A 106.3 . . ?
C10 N4 H4B 106.3 . . ?
C10 N4 Cd1 124(3) . . ?
H7A C7 H7B 106.1 . . ?
N3 C7 H7A 105.6 . . ?
N3 C7 H7B 105.6 . . ?
N3 C7 C8 127(5) . . ?
C8 C7 H7A 105.6 . . ?
C8 C7 H7B 105.6 . . ?
C3 C3 H3A 107.2 2_755 . ?
C3 C3 H3B 107.2 2_755 . ?
C3 C3 C2 121(5) 2_755 . ?
H3A C3 H3B 106.8 . . ?
C2 C3 H3A 107.2 . . ?
C2 C3 H3B 107.2 . . ?
H4C C4 H4D 106.1 . . ?
C5 C4 H4C 105.7 . . ?
C5 C4 H4D 105.7 . . ?
N2 C4 H4C 105.7 . . ?
N2 C4 H4D 105.7 . . ?
N2 C4 C5 126(6) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C10 C11 C12 112(3) . . ?
O5 N6 O4 125(7) . . ?
O6 N6 O4 119(6) . . ?
O6 N6 O5 114(4) . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C1 C2 C3 114(4) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
O4 Cd1 O1 158.1(13) . . ?
O4 Cd1 N2 116(2) . . ?
N4 Cd1 O4 88.8(16) . . ?
N4 Cd1 N3 170.4(14) . . ?
N4 Cd1 O1 74.7(16) . . ?
N4 Cd1 N2 90.1(14) . . ?
N3 Cd1 O4 86(2) . . ?
N3 Cd1 O1 112(2) . . ?
N3 Cd1 N2 84.6(16) . . ?
N2 Cd1 O1 79(2) . . ?
N1 Cd1 O4 80(3) . . ?
N1 Cd1 N4 97.7(12) . . ?
N1 Cd1 N3 89.7(11) . . ?
N1 Cd1 O1 88(3) . . ?
N1 Cd1 N2 163(3) . . ?
C7 N3 Cd1 123(4) . . ?
C7 N3 H3C 106.7 . . ?
C7 N3 H 106.7 . . ?
Cd1 N3 H3C 106.7 . . ?
Cd1 N3 H 106.7 . . ?
H3C N3 H 106.6 . . ?
N5 O1 Cd1 109(4) . . ?
C6 C5 C4 116(5) . . ?
C6 C5 H5A 108.2 . . ?
C6 C5 H5 108.2 . . ?
C4 C5 H5A 108.2 . . ?
C4 C5 H5 108.2 . . ?
H5A C5 H5 107.3 . . ?
C4 N2 Cd1 116(3) . . ?
C4 N2 H2C 108.2 . . ?
C4 N2 H2D 108.2 . . ?
Cd1 N2 H2C 108.2 . . ?
Cd1 N2 H2D 108.2 . . ?
H2C N2 H2D 107.4 . . ?
O3 N5 O1 122(6) . . ?
O2 N5 O1 112(6) . . ?
O2 N5 O3 126(6) . . ?
C7 C8 H8A 106.0 . . ?
C7 C8 H8B 106.0 . . ?
C7 C8 C9 125(5) . . ?
H8A C8 H8B 106.3 . . ?
C9 C8 H8A 106.0 . . ?
C9 C8 H8B 106.0 . . ?
C2 C1 H1A 105.7 . . ?
C2 C1 H1B 105.7 . . ?
H1A C1 H1B 106.1 . . ?
N1 C1 C2 126(5) . . ?
N1 C1 H1A 105.7 . . ?
N1 C1 H1B 105.7 . . ?
C8 C9 H9A 110.4 . . ?
C8 C9 H9B 110.4 . . ?
C9 C9 C8 107(4) 2_876 . ?
C9 C9 H9A 110.4 2_876 . ?
C9 C9 H9B 110.4 2_876 . ?
H9A C9 H9B 108.6 . . ?
C11 C12 H12A 105.1 . . ?
C11 C12 H12B 105.1 . . ?
C12 C12 C11 129(6) 2_666 . ?
C12 C12 H12A 105.1 2_666 . ?
C12 C12 H12B 105.1 2_666 . ?
H12A C12 H12B 105.9 . . ?
N4 C10 C11 119(6) . . ?
N4 C10 H10A 107.5 . . ?
N4 C10 H10B 107.5 . . ?
C11 C10 H10A 107.5 . . ?
C11 C10 H10B 107.5 . . ?
H10A C10 H10B 107.0 . . ?
Cd1 N1 H1C 103.2 . . ?
Cd1 N1 H1D 103.2 . . ?
C1 N1 Cd1 136(5) . . ?
C1 N1 H1C 103.2 . . ?
C1 N1 H1D 103.2 . . ?
H1C N1 H1D 105.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C6 C5 C4 -172(8) 2_675 . . . ?
C7 C8 C9 C9 -74(6) . . . 2_876 ?
C3 C3 C2 C1 60(8) 2_755 . . . ?
C3 C2 C1 N1 -178(7) . . . . ?
C2 C1 N1 Cd1 180(5) . . . . ?
Cd1 O4 N6 O5 27(5) . . . . ?
Cd1 O4 N6 O6 -141(4) . . . . ?
Cd1 N4 C10 C11 167(6) . . . . ?
Cd1 O1 N5 O3 -157(5) . . . . ?
Cd1 O1 N5 O2 19(5) . . . . ?
N3 C7 C8 C9 -173(4) . . . . ?
C5 C4 N2 Cd1 -150(5) . . . . ?
N2 C4 C5 C6 -82(9) . . . . ?
C8 C7 N3 Cd1 174(3) . . . . ?
C12 C11 C10 N4 -50(13) . . . . ?
C10 C11 C12 C12 -41(14) . . . 2_666 ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999988 0.00000000 -0.00049271
omega rotation goniometer -1 . -0.71463000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.16291000 -0.76618634 0.00000000
0.64261846
phi rotation goniometer -1 kappa . 0.00013422 0.00000000 0.99999999
theta rotation goniometer -1 . -0.64400000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.412
_oxdiff_exptl_absorpt_empirical_full_min 0.710
####################################################################### 
# 
# 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_250_K_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262354'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-12
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         CdC6N6O6
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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   9.6193(2)
_cell_length_b                   9.6193(2)
_cell_length_c                   21.2771(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1968.79(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6040
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      28.2290
_cell_measurement_theta_min      3.5210
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.127
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12931
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.651
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  90.00   0.80    6.00    --   21.75  73.00  14.00  120
  2  ω      8.00  85.60   0.80    6.00    --   21.75-136.00-171.00   97
  3  ω     39.00  96.60   0.80    6.00    --   21.75 178.00 -90.00   72
  4  ω     39.00  96.60   0.80    6.00    --   21.75 178.00  30.00   72
  5  ω     -8.00  37.60   0.80    6.00    --   21.75  77.00-120.00   57
  6  ω    -39.00   6.60   0.80    6.00    --  -22.69 -77.00 -90.00   57
  7  ω    -47.00  42.60   0.80    6.00    --   21.75 -57.00  30.00  112
  8  ω      0.00  90.40   0.80    6.00    --   21.75  57.00 150.00  113
  9  ω    -95.00 -70.20   0.80    6.00    --  -22.69 -37.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394839000
_diffrn_orient_matrix_UB_12      -0.0558626000
_diffrn_orient_matrix_UB_13      0.0124299000
_diffrn_orient_matrix_UB_21      0.0459803000
_diffrn_orient_matrix_UB_22      -0.0481178000
_diffrn_orient_matrix_UB_23      -0.0143631000
_diffrn_orient_matrix_UB_31      0.0419907000
_diffrn_orient_matrix_UB_32      0.0001188000
_diffrn_orient_matrix_UB_33      0.0274031000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1247
_reflns_number_total             1449
_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       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0261
_refine_ls_restrained_S_all      1.071
_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)+(0.0278P)²+1.0456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0598
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2BC,H2BD), C2(H2AA,H2AB), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.03455(9) Uani 1 4 d S T P . .
N1 N 0.81493(18) 0.59671(18) 0.35981(8) 0.0447(4) Uani 1 1 d . . . . .
H1A H 0.790694 0.563383 0.397781 0.054 Uiso 1 1 calc R U . . .
H1B H 0.742455 0.646904 0.345645 0.054 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.52256(12) 0.0517(6) Uani 1 2 d S T P . .
O1 O 1.0703(2) 0.83457(19) 0.49225(9) 0.0741(5) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.57949(13) 0.1097(13) Uani 1 2 d S T P . .
C1 C 0.8312(2) 0.4777(2) 0.31776(11) 0.0518(5) Uani 1 1 d . . . . .
H1C H 0.916821 0.428329 0.328901 0.062 Uiso 1 1 calc R U . . .
H1D H 0.841576 0.511858 0.274629 0.062 Uiso 1 1 calc R U . . .
C2 C 0.7114(3) 0.3762(2) 0.31978(12) 0.0583(6) Uani 1 1 d . . . . .
H2BC H 0.629416 0.419538 0.300700 0.070 Uiso 0.704(10) 1 calc R U P A 2
H2BD H 0.689065 0.355265 0.363711 0.070 Uiso 0.704(10) 1 calc R U P A 2
H2AA H 0.625782 0.427354 0.329189 0.070 Uiso 0.296(10) 1 calc R U P A 1
H2AB H 0.727163 0.310125 0.354108 0.070 Uiso 0.296(10) 1 calc R U P A 1
C3B C 0.7438(4) 0.2391(3) 0.28491(17) 0.0491(12) Uani 0.704(10) 1 d . . P A 2
H3BA H 0.831104 0.200354 0.300986 0.059 Uiso 0.704(10) 1 calc R U P A 2
H3BB H 0.669725 0.171691 0.293329 0.059 Uiso 0.704(10) 1 calc R U P A 2
C3A C 0.6899(10) 0.2910(11) 0.2557(5) 0.061(3) Uani 0.296(10) 1 d . . P A 1
H3AA H 0.607971 0.230970 0.259203 0.074 Uiso 0.296(10) 1 calc R U P A 1
H3AB H 0.675108 0.355591 0.220734 0.074 Uiso 0.296(10) 1 calc R U 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
Cd1 N1 2.3341(17) . ?
Cd1 N1 2.3342(16) 11_676 ?
Cd1 N1 2.3342(16) 16_756 ?
Cd1 N1 2.3342(17) 6_664 ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 C1 1.461(2) . ?
N2 O1 1.239(2) 6_664 ?
N2 O1 1.239(2) . ?
N2 O2 1.211(4) . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C1 C2 1.511(3) . ?
C2 H2BC 0.9800 . ?
C2 H2BD 0.9800 . ?
C2 H2AA 0.9800 . ?
C2 H2AB 0.9800 . ?
C2 C3B 1.545(4) . ?
C2 C3A 1.604(10) . ?
C3B C3B 1.505(7) 13_655 ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3A C3A 1.42(2) 13_655 ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 164.08(8) . 6_664 ?
N1 Cd1 N1 164.07(8) 11_676 16_756 ?
N1 Cd1 N1 91.100(12) . 16_756 ?
N1 Cd1 N1 91.099(12) . 11_676 ?
N1 Cd1 N1 91.100(12) 6_664 11_676 ?
N1 Cd1 N1 91.100(12) 6_664 16_756 ?
Cd1 N1 H1A 107.4 . . ?
Cd1 N1 H1B 107.4 . . ?
H1A N1 H1B 106.9 . . ?
C1 N1 Cd1 119.88(12) . . ?
C1 N1 H1A 107.4 . . ?
C1 N1 H1B 107.4 . . ?
O1 N2 O1 117.3(3) 6_664 . ?
O2 N2 O1 121.37(14) . . ?
O2 N2 O1 121.36(14) . 6_664 ?
N1 C1 H1C 108.7 . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 C2 114.04(18) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.7 . . ?
C2 C1 H1D 108.7 . . ?
C1 C2 H2BC 109.1 . . ?
C1 C2 H2BD 109.1 . . ?
C1 C2 H2AA 108.8 . . ?
C1 C2 H2AB 108.8 . . ?
C1 C2 C3B 112.6(2) . . ?
C1 C2 C3A 113.8(4) . . ?
H2BC C2 H2BD 107.8 . . ?
H2AA C2 H2AB 107.7 . . ?
C3B C2 H2BC 109.1 . . ?
C3B C2 H2BD 109.1 . . ?
C3A C2 H2AA 108.8 . . ?
C3A C2 H2AB 108.8 . . ?
C2 C3B H3BA 109.3 . . ?
C2 C3B H3BB 109.3 . . ?
C3B C3B C2 111.8(4) 13_655 . ?
C3B C3B H3BA 109.3 13_655 . ?
C3B C3B H3BB 109.3 13_655 . ?
H3BA C3B H3BB 107.9 . . ?
C2 C3A H3AA 109.9 . . ?
C2 C3A H3AB 109.9 . . ?
C3A C3A C2 108.9(10) 13_655 . ?
C3A C3A H3AA 109.9 13_655 . ?
C3A C3A H3AB 109.9 13_655 . ?
H3AA C3A H3AB 108.3 . . ?

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
Cd1 N1 C1 C2 171.43(16) . . . . ?
N1 C1 C2 C3B -169.0(2) . . . . ?
N1 C1 C2 C3A 152.7(5) . . . . ?
C1 C2 C3B C3B -68.0(5) . . . 13_655 ?
C1 C2 C3A C3A 62.6(12) . . . 13_655 ?

_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 1.044
_oxdiff_exptl_absorpt_empirical_full_min 0.954
####################################################################### 
# 
# 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_200_K_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262355'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-12
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         CdC6N6O6
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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   9.5708(2)
_cell_length_b                   9.5708(2)
_cell_length_c                   21.3382(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1954.58(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7236
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      29.8800
_cell_measurement_theta_min      3.5270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.127
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.604
_diffrn_reflns_theta_min         2.332
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  90.00   0.80    6.00    --   21.75  73.00  14.00  120
  2  ω      8.00  85.60   0.80    6.00    --   21.75-136.00-171.00   97
  3  ω     39.00  96.60   0.80    6.00    --   21.75 178.00 -90.00   72
  4  ω     39.00  96.60   0.80    6.00    --   21.75 178.00  30.00   72
  5  ω     -8.00  37.60   0.80    6.00    --   21.75  77.00-120.00   57
  6  ω    -39.00   6.60   0.80    6.00    --  -22.69 -77.00 -90.00   57
  7  ω    -47.00  42.60   0.80    6.00    --   21.75 -57.00  30.00  112
  8  ω      0.00  90.40   0.80    6.00    --   21.75  57.00 150.00  113
  9  ω    -95.00 -70.20   0.80    6.00    --  -22.69 -37.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400082000
_diffrn_orient_matrix_UB_12      -0.0561420000
_diffrn_orient_matrix_UB_13      0.0121962000
_diffrn_orient_matrix_UB_21      0.0462074000
_diffrn_orient_matrix_UB_22      -0.0483780000
_diffrn_orient_matrix_UB_23      -0.0143016000
_diffrn_orient_matrix_UB_31      0.0418945000
_diffrn_orient_matrix_UB_32      -0.0002514000
_diffrn_orient_matrix_UB_33      0.0274223000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1281
_reflns_number_total             1444
_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       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.059
_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)+(0.0224P)²+1.0219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0486
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2BC,H2BD), C2(H2AA,H2AB), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.02612(7) Uani 1 4 d S T P . .
N1 N 0.81257(14) 0.59865(14) 0.35945(6) 0.0337(3) Uani 1 1 d . . . . .
H1A H 0.786476 0.565446 0.397656 0.040 Uiso 1 1 calc R U . . .
H1B H 0.739909 0.650231 0.344570 0.040 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.52160(9) 0.0400(4) Uani 1 2 d S T P . .
O1 O 1.07193(16) 0.83496(15) 0.49162(7) 0.0571(4) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.57887(10) 0.0832(9) Uani 1 2 d S T P . .
C1 C 0.82989(18) 0.47824(17) 0.31770(9) 0.0397(4) Uani 1 1 d . . . . .
H1C H 0.917011 0.428680 0.329162 0.048 Uiso 1 1 calc R U . . .
H1D H 0.840536 0.512435 0.274177 0.048 Uiso 1 1 calc R U . . .
C2 C 0.7098(2) 0.37579(19) 0.31990(9) 0.0458(4) Uani 1 1 d . . . . .
H2BC H 0.626130 0.419615 0.301015 0.055 Uiso 0.747(7) 1 calc R U P A 2
H2BD H 0.687942 0.353912 0.364168 0.055 Uiso 0.747(7) 1 calc R U P A 2
H2AA H 0.622950 0.427236 0.329965 0.055 Uiso 0.253(7) 1 calc R U P A 1
H2AB H 0.726855 0.308058 0.354124 0.055 Uiso 0.253(7) 1 calc R U P A 1
C3B C 0.7429(3) 0.2388(2) 0.28473(12) 0.0387(8) Uani 0.747(7) 1 d . . P A 2
H3BA H 0.830914 0.198972 0.301256 0.046 Uiso 0.747(7) 1 calc R U P A 2
H3BB H 0.667231 0.170500 0.292642 0.046 Uiso 0.747(7) 1 calc R U P A 2
C3A C 0.6874(8) 0.2919(8) 0.2560(4) 0.041(2) Uani 0.253(7) 1 d . . P A 1
H3AA H 0.604633 0.230427 0.259532 0.049 Uiso 0.253(7) 1 calc R U P A 1
H3AB H 0.671717 0.358072 0.221075 0.049 Uiso 0.253(7) 1 calc R U 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
Cd1 N1 2.3294(13) . ?
Cd1 N1 2.3294(13) 16_756 ?
Cd1 N1 2.3294(13) 11_676 ?
Cd1 N1 2.3295(13) 6_664 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.466(2) . ?
N2 O1 1.2427(17) 6_664 ?
N2 O1 1.2427(17) . ?
N2 O2 1.222(3) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C1 C2 1.511(2) . ?
C2 H2BC 0.9900 . ?
C2 H2BD 0.9900 . ?
C2 H2AA 0.9900 . ?
C2 H2AB 0.9900 . ?
C2 C3B 1.543(3) . ?
C2 C3A 1.596(8) . ?
C3B C3B 1.504(5) 13_655 ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3A C3A 1.464(16) 13_655 ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?

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 Cd1 N1 163.62(7) . 6_664 ?
N1 Cd1 N1 163.62(7) 16_756 11_676 ?
N1 Cd1 N1 91.163(10) . 11_676 ?
N1 Cd1 N1 91.163(9) . 16_756 ?
N1 Cd1 N1 91.163(10) 6_664 16_756 ?
N1 Cd1 N1 91.163(10) 6_664 11_676 ?
Cd1 N1 H1A 107.5 . . ?
Cd1 N1 H1B 107.5 . . ?
H1A N1 H1B 107.0 . . ?
C1 N1 Cd1 119.23(10) . . ?
C1 N1 H1A 107.5 . . ?
C1 N1 H1B 107.5 . . ?
O1 N2 O1 118.0(2) 6_664 . ?
O2 N2 O1 120.98(11) . . ?
O2 N2 O1 120.98(11) . 6_664 ?
N1 C1 H1C 108.8 . . ?
N1 C1 H1D 108.8 . . ?
N1 C1 C2 113.91(14) . . ?
H1C C1 H1D 107.7 . . ?
C2 C1 H1C 108.8 . . ?
C2 C1 H1D 108.8 . . ?
C1 C2 H2BC 109.1 . . ?
C1 C2 H2BD 109.1 . . ?
C1 C2 H2AA 108.8 . . ?
C1 C2 H2AB 108.8 . . ?
C1 C2 C3B 112.36(16) . . ?
C1 C2 C3A 113.7(3) . . ?
H2BC C2 H2BD 107.9 . . ?
H2AA C2 H2AB 107.7 . . ?
C3B C2 H2BC 109.1 . . ?
C3B C2 H2BD 109.1 . . ?
C3A C2 H2AA 108.8 . . ?
C3A C2 H2AB 108.8 . . ?
C2 C3B H3BA 109.2 . . ?
C2 C3B H3BB 109.2 . . ?
C3B C3B C2 112.2(3) 13_655 . ?
C3B C3B H3BA 109.2 13_655 . ?
C3B C3B H3BB 109.2 13_655 . ?
H3BA C3B H3BB 107.9 . . ?
C2 C3A H3AA 110.0 . . ?
C2 C3A H3AB 110.0 . . ?
C3A C3A C2 108.4(7) 13_655 . ?
C3A C3A H3AA 110.0 13_655 . ?
C3A C3A H3AB 110.0 13_655 . ?
H3AA C3A H3AB 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
Cd1 N1 C1 C2 170.41(12) . . . . ?
N1 C1 C2 C3B -169.86(18) . . . . ?
N1 C1 C2 C3A 151.6(4) . . . . ?
C1 C2 C3B C3B -66.9(3) . . . 13_655 ?
C1 C2 C3A C3A 62.7(8) . . . 13_655 ?

_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 1.050
_oxdiff_exptl_absorpt_empirical_full_min 0.951
####################################################################### 
# 
# 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_150_K_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262356'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_150_K_Cd_HDA_2_NO3_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.97Ang From Cd1'            4.04 eA-3
RESPONSE: The crystals all showed strong diffuse scattering in the form of
 diffuse Bragg peaks and scattering between them. As the model does not account
 for this type of disorder this is believe to be the source of the high electron
 density on the Cd cation.
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From Cd1             3.12 eA-3
RESPONSE: The crystals all showed strong diffuse scattering in the form of 
diffuse Bragg peaks and scattering between them. As the model does not account
 for this type of disorder this is believe to be the source of the high electron
 density on the Cd cation.
;
_vrf_PLAT973_150_K_Cd_HDA_2_NO3_2 
;
PROBLEM: Check Calcd Positive Resid. Density on      Cd1'       1.62 eA-3
RESPONSE: The crystals all showed strong diffuse scattering in the form of 
diffuse Bragg peaks and scattering between them. As the model does not account
 for this type of disorder this is believe to be the source of the high electron
 density on the Cd cation.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2023-05-09
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N5.5 O4.5, 0.5(N O3)'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         CdC6N6O6
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'
Cd Cd -0.8075 1.2024 '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      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                   9.9696(8)
_cell_length_b                   12.2010(9)
_cell_length_c                   18.1134(16)
_cell_angle_alpha                74.552(7)
_cell_angle_beta                 74.701(7)
_cell_angle_gamma                68.229(7)
_cell_volume                     1938.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4230
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      24.7130
_cell_measurement_theta_min      2.7680
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.714
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 9 8 0.1099
-10 -13 4 0.0823
11 12 -4 0.0477
-11 5 -8 0.1292
3 7 25 0.0220
-3 -7 -25 0.1253
4 17 1 0.0476
1 -16 -5 0.1216

_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.127
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.8722 8.5901 7.6515 0.0208 -0.0008 0.9998
-10.3206 -12.5673 4.0447 -0.9615 0.1797 0.2079
10.6624 11.8806 -4.4556 0.9476 -0.1773 -0.2658
-10.8611 4.6234 -7.5818 0.1027 0.5672 0.8172
3.1140 6.9250 25.1567 -0.1660 -0.8829 0.4392
-2.9909 -6.9923 -25.1125 0.1651 0.8778 -0.4497
4.4169 16.7778 1.2117 0.8827 -0.1659 0.4397
0.9661 -16.0055 -5.0287 -0.6153 0.1240 -0.8193

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19863
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.711
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  90.00   0.80    6.00    --   21.75  73.00  14.00  120
  2  ω      8.00  85.60   0.80    6.00    --   21.75-136.00-171.00   97
  3  ω     39.00  96.60   0.80    6.00    --   21.75 178.00 -90.00   72
  4  ω     39.00  96.60   0.80    6.00    --   21.75 178.00  30.00   72
  5  ω     -8.00  37.60   0.80    6.00    --   21.75  77.00-120.00   57
  6  ω    -39.00   6.60   0.80    6.00    --  -22.69 -77.00 -90.00   57
  7  ω    -47.00  42.60   0.80    6.00    --   21.75 -57.00  30.00  112
  8  ω      0.00  90.40   0.80    6.00    --   21.75  57.00 150.00  113
  9  ω    -95.00 -70.20   0.80    6.00    --  -22.69 -37.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0266508000
_diffrn_orient_matrix_UB_12      0.0472494000
_diffrn_orient_matrix_UB_13      -0.0229059000
_diffrn_orient_matrix_UB_21      -0.0301293000
_diffrn_orient_matrix_UB_22      0.0003181000
_diffrn_orient_matrix_UB_23      -0.0314538000
_diffrn_orient_matrix_UB_31      -0.0667658000
_diffrn_orient_matrix_UB_32      0.0427765000
_diffrn_orient_matrix_UB_33      0.0139494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5241
_reflns_number_total             7845
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.810
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0862
_refine_ls_restrained_S_all      1.087
_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)+(0.1123P)²+10.6345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2468
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cd1) \\sim Ueq, Uanis(Cd1') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N2'(H2'A,H2'B), N2(H2A,H2B), N1'(H1'A,H1'B), N1(H1A,
 H1B), N3'(H3'A,H3'B), N4'(H4'A,H4'B), C7(H7A,H7B), C2(H2C,H2D), C10(H10A,H10B),
  C4(H4C,H4D), C6'(H6'A,H6'B), C11'(H11A,H11B), C8(H8A,H8B), C5(H5A,H5B),
 C8'(H8'A,H8'B), C11(H11C,H11D), C5'(H5'A,H5'B), C2'(H2'C,H2'D), C1'(H1'C,H1'D),
  C1(H1C,H1D), C3(H3C,H3D), C7'(H7'A,H7'B), C4'(H4'C,H4'D), C12(H12A,H12B),
 C12'(H12C,H12D), C6(H6A,H6B), C3'(H3'C,H3'D), C9(H9A,H9B), C10'(H10C,H10D),
 C9'(H9'A,H9'B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 1.11691(8) 0.44979(7) 0.31295(4) 0.0289(2) Uani 1 1 d . U . . .
Cd1' Cd -0.08790(8) 1.05968(6) 0.18932(4) 0.0293(2) Uani 1 1 d . U . . .
O4 O 1.1784(8) 0.2926(7) 0.2368(5) 0.0411(19) Uani 1 1 d . . . . .
O2' O -0.0565(9) 0.8455(7) 0.1818(5) 0.0456(19) Uani 1 1 d . . . . .
O1 O 0.9490(9) 0.5788(7) 0.4094(5) 0.046(2) Uani 1 1 d . . . . .
O3 O 0.9290(10) 0.7448(7) 0.4389(5) 0.053(2) Uani 1 1 d . . . . .
O1' O 0.0695(8) 0.9393(7) 0.0893(5) 0.0456(19) Uani 1 1 d . . . . .
O2 O 1.0765(9) 0.6889(8) 0.3348(5) 0.052(2) Uani 1 1 d . . . . .
N3 N 1.2982(9) 0.5177(8) 0.2281(5) 0.0322(19) Uani 1 1 d . . . . .
H3A H 1.273625 0.597172 0.228562 0.039 Uiso 1 1 calc R U . . .
H3B H 1.382546 0.479350 0.247667 0.039 Uiso 1 1 calc R U . . .
N4 N 0.9544(9) 0.3485(8) 0.3875(5) 0.035(2) Uani 1 1 d . . . . .
H4A H 0.916093 0.377764 0.432528 0.042 Uiso 1 1 calc R U . . .
H4B H 0.878941 0.370788 0.361521 0.042 Uiso 1 1 calc R U . . .
N2' N -0.2381(9) 1.1342(8) 0.0970(5) 0.0310(19) Uani 1 1 d . . . . .
H2'A H -0.308211 1.204127 0.107651 0.037 Uiso 1 1 calc R U . . .
H2'B H -0.183353 1.151024 0.049172 0.037 Uiso 1 1 calc R U . . .
N5 N 0.9848(9) 0.6719(8) 0.3948(5) 0.034(2) Uani 1 1 d . . . . .
N2 N 1.2625(9) 0.3699(8) 0.4078(5) 0.037(2) Uani 1 1 d . . . . .
H2A H 1.213679 0.330415 0.449601 0.044 Uiso 1 1 calc R U . . .
H2B H 1.345621 0.313655 0.388845 0.044 Uiso 1 1 calc R U . . .
N1' N 0.0709(9) 0.9515(8) 0.2772(5) 0.037(2) Uani 1 1 d . . . . .
H1'A H 0.063089 1.000595 0.309202 0.044 Uiso 1 1 calc R U . . .
H1'B H 0.039188 0.889940 0.307311 0.044 Uiso 1 1 calc R U . . .
N6 N 1.3065(11) 0.2158(8) 0.2372(5) 0.039(2) Uani 1 1 d . . . . .
O3' O 0.0774(10) 0.7612(8) 0.0841(6) 0.057(2) Uani 1 1 d . . . . .
N5' N 0.0316(10) 0.8471(9) 0.1177(6) 0.039(2) Uani 1 1 d . . . . .
N1 N 0.9554(9) 0.5568(8) 0.2252(5) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.989728 0.615935 0.193269 0.045 Uiso 1 1 calc R U . . .
H1B H 0.961749 0.505756 0.194857 0.045 Uiso 1 1 calc R U . . .
N3' N -0.2885(9) 1.0740(8) 0.2894(6) 0.041(2) Uani 1 1 d . . . . .
H3'A H -0.278511 1.110293 0.324630 0.049 Uiso 1 1 calc R U . . .
H3'B H -0.370564 1.122339 0.269759 0.049 Uiso 1 1 calc R U . . .
N6' N -0.3151(10) 1.3503(9) 0.2574(6) 0.043(2) Uani 1 1 d . . . . .
O5 O 1.3881(10) 0.2279(8) 0.2736(6) 0.070(3) Uani 1 1 d . . . . .
O6' O -0.4256(9) 1.3871(10) 0.3030(5) 0.065(3) Uani 1 1 d . . . . .
O5' O -0.3166(9) 1.3538(9) 0.1883(5) 0.063(3) Uani 1 1 d . . . . .
N4' N 0.0125(9) 1.2084(8) 0.1457(5) 0.036(2) Uani 1 1 d . . . . .
H4'A H -0.062684 1.279176 0.146058 0.044 Uiso 1 1 calc R U . . .
H4'B H 0.065276 1.202742 0.181372 0.044 Uiso 1 1 calc R U . . .
O6 O 1.3470(13) 0.1364(10) 0.2019(7) 0.088(4) Uani 1 1 d . . . . .
C7 C 1.3323(11) 0.5042(9) 0.1457(6) 0.031(2) Uani 1 1 d . . . . .
H7A H 1.238614 0.528184 0.127146 0.037 Uiso 1 1 calc R U . . .
H7B H 1.383791 0.418274 0.143053 0.037 Uiso 1 1 calc R U . . .
C2 C 0.7052(11) 0.6657(11) 0.1928(6) 0.039(3) Uani 1 1 d . . . . .
H2C H 0.726999 0.604204 0.161192 0.047 Uiso 1 1 calc R U . . .
H2D H 0.733732 0.734303 0.157938 0.047 Uiso 1 1 calc R U . . .
C10 C 1.0015(11) 0.2165(9) 0.4096(6) 0.034(2) Uani 1 1 d . . . . .
H10A H 1.091201 0.188456 0.432390 0.041 Uiso 1 1 calc R U . . .
H10B H 1.027111 0.181918 0.362072 0.041 Uiso 1 1 calc R U . . .
C4 C 1.3084(11) 0.4510(10) 0.4368(6) 0.032(2) Uani 1 1 d . . . . .
H4C H 1.219941 0.509081 0.461703 0.039 Uiso 1 1 calc R U . . .
H4D H 1.359120 0.497163 0.392069 0.039 Uiso 1 1 calc R U . . .
C6' C -0.4653(11) 0.9892(10) 0.0343(6) 0.036(2) Uani 1 1 d . . . . .
H6'A H -0.384607 0.911397 0.036115 0.043 Uiso 1 1 calc R U . . .
H6'B H -0.539377 0.982953 0.082544 0.043 Uiso 1 1 calc R U . . .
C11' C 0.1308(12) 1.3390(9) 0.0356(6) 0.035(2) Uani 1 1 d . . . . .
H11A H 0.207122 1.332457 -0.012275 0.042 Uiso 1 1 calc R U . . .
H11B H 0.167187 1.360789 0.073700 0.042 Uiso 1 1 calc R U . . .
C8 C 1.4250(11) 0.5763(9) 0.0912(6) 0.032(2) Uani 1 1 d . . . . .
H8A H 1.520343 0.550487 0.108262 0.038 Uiso 1 1 calc R U . . .
H8B H 1.375246 0.662145 0.094660 0.038 Uiso 1 1 calc R U . . .
O4' O -0.1969(10) 1.3070(13) 0.2790(7) 0.098(5) Uani 1 1 d . . . . .
C5 C 1.4107(11) 0.3823(10) 0.4955(7) 0.037(2) Uani 1 1 d . . . . .
H5A H 1.500871 0.326828 0.469638 0.044 Uiso 1 1 calc R U . . .
H5B H 1.361532 0.333081 0.538741 0.044 Uiso 1 1 calc R U . . .
C8' C -0.4460(12) 0.9677(11) 0.3957(6) 0.038(3) Uani 1 1 d . . . . .
H8'A H -0.533523 1.027493 0.375593 0.046 Uiso 1 1 calc R U . . .
H8'B H -0.461824 0.888597 0.410737 0.046 Uiso 1 1 calc R U . . .
C11 C 0.8864(11) 0.1708(9) 0.4668(7) 0.036(2) Uani 1 1 d . . . . .
H11C H 0.794392 0.204849 0.445641 0.043 Uiso 1 1 calc R U . . .
H11D H 0.866782 0.200633 0.515651 0.043 Uiso 1 1 calc R U . . .
C5' C -0.4039(12) 1.0882(10) 0.0324(7) 0.037(2) Uani 1 1 d . . . . .
H5'A H -0.343542 1.105323 -0.019534 0.045 Uiso 1 1 calc R U . . .
H5'B H -0.486013 1.162724 0.041347 0.045 Uiso 1 1 calc R U . . .
C2' C 0.3250(10) 0.8441(11) 0.3041(7) 0.039(3) Uani 1 1 d . . . . .
H2'C H 0.298719 0.773547 0.337458 0.047 Uiso 1 1 calc R U . . .
H2'D H 0.304648 0.902453 0.337836 0.047 Uiso 1 1 calc R U . . .
C1' C 0.2276(10) 0.9009(10) 0.2439(6) 0.034(2) Uani 1 1 d . . . . .
H1'C H 0.260837 0.965743 0.206837 0.041 Uiso 1 1 calc R U . . .
H1'D H 0.238827 0.839726 0.214154 0.041 Uiso 1 1 calc R U . . .
C1 C 0.7974(11) 0.6133(10) 0.2554(6) 0.038(2) Uani 1 1 d . . . . .
H1C H 0.786682 0.677799 0.282175 0.045 Uiso 1 1 calc R U . . .
H1D H 0.759886 0.552279 0.294403 0.045 Uiso 1 1 calc R U . . .
C3 C 0.5405(10) 0.7087(10) 0.2238(7) 0.040(3) Uani 1 1 d . . . . .
H3C H 0.488871 0.738836 0.179050 0.048 Uiso 1 1 calc R U . . .
H3D H 0.511762 0.638703 0.256151 0.048 Uiso 1 1 calc R U . . .
C7' C -0.3101(12) 0.9610(10) 0.3297(7) 0.041(3) Uani 1 1 d . . . . .
H7'A H -0.221544 0.909589 0.352146 0.049 Uiso 1 1 calc R U . . .
H7'B H -0.317485 0.920704 0.290952 0.049 Uiso 1 1 calc R U . . .
C4' C -0.3107(12) 1.0488(10) 0.0947(7) 0.041(3) Uani 1 1 d . . . . .
H4'C H -0.373836 1.034439 0.146115 0.049 Uiso 1 1 calc R U . . .
H4'D H -0.233793 0.971238 0.086879 0.049 Uiso 1 1 calc R U . . .
C12 C 0.9273(12) 0.0324(10) 0.4864(7) 0.040(3) Uani 1 1 d . . . . .
H12A H 0.848774 0.010732 0.527625 0.048 Uiso 1 1 calc R U . . .
H12B H 0.930564 0.003768 0.439526 0.048 Uiso 1 1 calc R U . . .
C12' C -0.0097(13) 1.4387(10) 0.0160(7) 0.042(3) Uani 1 1 d . . . . .
H12C H -0.044650 1.417247 -0.022855 0.050 Uiso 1 1 calc R U . . .
H12D H -0.086478 1.443448 0.063677 0.050 Uiso 1 1 calc R U . . .
C6 C 1.4549(13) 0.4653(11) 0.5297(6) 0.044(3) Uani 1 1 d . . . . .
H6A H 1.364529 0.522612 0.553806 0.052 Uiso 1 1 calc R U . . .
H6B H 1.511401 0.415553 0.571251 0.052 Uiso 1 1 calc R U . . .
C3' C 0.4887(10) 0.8038(11) 0.2708(6) 0.038(3) Uani 1 1 d . . . . .
H3'C H 0.514540 0.874698 0.237897 0.045 Uiso 1 1 calc R U . . .
H3'D H 0.542905 0.774615 0.314553 0.045 Uiso 1 1 calc R U . . .
C9 C 1.4536(12) 0.5635(9) 0.0066(7) 0.038(3) Uani 1 1 d . . . . .
H9A H 1.504572 0.620456 -0.026509 0.046 Uiso 1 1 calc R U . . .
H9B H 1.358343 0.585482 -0.009803 0.046 Uiso 1 1 calc R U . . .
C10' C 0.1074(12) 1.2173(10) 0.0693(6) 0.039(3) Uani 1 1 d . . . . .
H10C H 0.064747 1.198970 0.032296 0.047 Uiso 1 1 calc R U . . .
H10D H 0.204412 1.155042 0.073039 0.047 Uiso 1 1 calc R U . . .
C9' C -0.4335(11) 1.0008(11) 0.4663(6) 0.043(3) Uani 1 1 d . . . . .
H9'A H -0.424513 1.082280 0.452134 0.052 Uiso 1 1 calc R U . . .
H9'B H -0.342737 0.944112 0.484612 0.052 Uiso 1 1 calc R U . . .


_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
Cd1 O4 2.458(7) . ?
Cd1 O1 2.510(8) . ?
Cd1 N3 2.298(8) . ?
Cd1 N4 2.327(8) . ?
Cd1 N2 2.320(8) . ?
Cd1 N1 2.348(9) . ?
Cd1' O2' 2.550(8) . ?
Cd1' O1' 2.472(8) . ?
Cd1' N2' 2.317(8) . ?
Cd1' N1' 2.333(9) . ?
Cd1' N3' 2.305(9) . ?
Cd1' N4' 2.254(9) . ?
O4 N6 1.274(12) . ?
O2' N5' 1.259(12) . ?
O1 N5 1.256(11) . ?
O3 N5 1.231(11) . ?
O1' N5' 1.256(12) . ?
O2 N5 1.248(11) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C7 1.481(12) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C10 1.473(13) . ?
N2' H2'A 0.9100 . ?
N2' H2'B 0.9100 . ?
N2' C4' 1.487(13) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C4 1.485(13) . ?
N1' H1'A 0.9100 . ?
N1' H1'B 0.9100 . ?
N1' C1' 1.474(12) . ?
N6 O5 1.242(12) . ?
N6 O6 1.189(12) . ?
O3' N5' 1.232(12) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.482(12) . ?
N3' H3'A 0.9100 . ?
N3' H3'B 0.9100 . ?
N3' C7' 1.442(14) . ?
N6' O6' 1.203(12) . ?
N6' O5' 1.246(12) . ?
N6' O4' 1.221(13) . ?
N4' H4'A 0.9100 . ?
N4' H4'B 0.9100 . ?
N4' C10' 1.459(13) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.504(14) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C1 1.506(14) . ?
C2 C3 1.522(14) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.497(14) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C4 C5 1.529(13) . ?
C6' C6' 1.49(2) 2_475 ?
C6' H6'A 0.9900 . ?
C6' H6'B 0.9900 . ?
C6' C5' 1.533(14) . ?
C11' H11A 0.9900 . ?
C11' H11B 0.9900 . ?
C11' C12' 1.528(15) . ?
C11' C10' 1.527(15) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.522(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.552(15) . ?
C8' H8'A 0.9900 . ?
C8' H8'B 0.9900 . ?
C8' C7' 1.545(14) . ?
C8' C9' 1.486(15) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 C12 1.546(15) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C5' C4' 1.517(15) . ?
C2' H2'C 0.9900 . ?
C2' H2'D 0.9900 . ?
C2' C1' 1.507(14) . ?
C2' C3' 1.521(13) . ?
C1' H1'C 0.9900 . ?
C1' H1'D 0.9900 . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C3' 1.479(16) . ?
C7' H7'A 0.9900 . ?
C7' H7'B 0.9900 . ?
C4' H4'C 0.9900 . ?
C4' H4'D 0.9900 . ?
C12 C12 1.51(2) 2_756 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12' C12' 1.52(2) 2_585 ?
C12' H12C 0.9900 . ?
C12' H12D 0.9900 . ?
C6 C6 1.50(2) 2_866 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3' H3'C 0.9900 . ?
C3' H3'D 0.9900 . ?
C9 C9 1.53(2) 2_865 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C9' C9' 1.55(2) 2_476 ?
C9' H9'A 0.9900 . ?
C9' H9'B 0.9900 . ?

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 Cd1 O1 152.7(2) . . ?
N3 Cd1 O4 88.8(3) . . ?
N3 Cd1 O1 116.9(3) . . ?
N3 Cd1 N4 168.9(3) . . ?
N3 Cd1 N2 90.2(3) . . ?
N3 Cd1 N1 90.0(3) . . ?
N4 Cd1 O4 80.4(3) . . ?
N4 Cd1 O1 74.2(3) . . ?
N4 Cd1 N1 91.0(3) . . ?
N2 Cd1 O4 106.6(3) . . ?
N2 Cd1 O1 83.4(3) . . ?
N2 Cd1 N4 90.4(3) . . ?
N2 Cd1 N1 171.4(3) . . ?
N1 Cd1 O4 82.0(3) . . ?
N1 Cd1 O1 88.8(3) . . ?
O1' Cd1' O2' 50.7(3) . . ?
N2' Cd1' O2' 90.1(3) . . ?
N2' Cd1' O1' 80.7(3) . . ?
N2' Cd1' N1' 169.8(3) . . ?
N1' Cd1' O2' 79.8(3) . . ?
N1' Cd1' O1' 91.7(3) . . ?
N3' Cd1' O2' 94.1(3) . . ?
N3' Cd1' O1' 143.4(3) . . ?
N3' Cd1' N2' 91.3(3) . . ?
N3' Cd1' N1' 90.8(3) . . ?
N4' Cd1' O2' 144.8(3) . . ?
N4' Cd1' O1' 95.4(3) . . ?
N4' Cd1' N2' 93.6(3) . . ?
N4' Cd1' N1' 93.9(3) . . ?
N4' Cd1' N3' 120.8(3) . . ?
N6 O4 Cd1 115.1(6) . . ?
N5' O2' Cd1' 93.8(6) . . ?
N5 O1 Cd1 107.2(6) . . ?
N5' O1' Cd1' 97.7(6) . . ?
Cd1 N3 H3A 107.5 . . ?
Cd1 N3 H3B 107.5 . . ?
H3A N3 H3B 107.0 . . ?
C7 N3 Cd1 119.1(6) . . ?
C7 N3 H3A 107.5 . . ?
C7 N3 H3B 107.5 . . ?
Cd1 N4 H4A 106.9 . . ?
Cd1 N4 H4B 106.9 . . ?
H4A N4 H4B 106.7 . . ?
C10 N4 Cd1 121.8(6) . . ?
C10 N4 H4A 106.9 . . ?
C10 N4 H4B 106.9 . . ?
Cd1' N2' H2'A 109.0 . . ?
Cd1' N2' H2'B 109.0 . . ?
H2'A N2' H2'B 107.8 . . ?
C4' N2' Cd1' 112.7(6) . . ?
C4' N2' H2'A 109.0 . . ?
C4' N2' H2'B 109.0 . . ?
O3 N5 O1 120.2(9) . . ?
O3 N5 O2 121.1(10) . . ?
O2 N5 O1 118.7(9) . . ?
Cd1 N2 H2A 107.5 . . ?
Cd1 N2 H2B 107.5 . . ?
H2A N2 H2B 107.0 . . ?
C4 N2 Cd1 119.4(6) . . ?
C4 N2 H2A 107.5 . . ?
C4 N2 H2B 107.5 . . ?
Cd1' N1' H1'A 108.1 . . ?
Cd1' N1' H1'B 108.1 . . ?
H1'A N1' H1'B 107.3 . . ?
C1' N1' Cd1' 116.9(7) . . ?
C1' N1' H1'A 108.1 . . ?
C1' N1' H1'B 108.1 . . ?
O5 N6 O4 118.4(9) . . ?
O6 N6 O4 120.3(10) . . ?
O6 N6 O5 121.4(11) . . ?
O1' N5' O2' 117.7(9) . . ?
O3' N5' O2' 120.7(10) . . ?
O3' N5' O1' 121.6(10) . . ?
Cd1 N1 H1A 107.4 . . ?
Cd1 N1 H1B 107.4 . . ?
H1A N1 H1B 107.0 . . ?
C1 N1 Cd1 119.6(6) . . ?
C1 N1 H1A 107.4 . . ?
C1 N1 H1B 107.4 . . ?
Cd1' N3' H3'A 108.5 . . ?
Cd1' N3' H3'B 108.5 . . ?
H3'A N3' H3'B 107.5 . . ?
C7' N3' Cd1' 114.9(7) . . ?
C7' N3' H3'A 108.5 . . ?
C7' N3' H3'B 108.5 . . ?
O6' N6' O5' 122.1(10) . . ?
O6' N6' O4' 119.7(11) . . ?
O4' N6' O5' 118.2(10) . . ?
Cd1' N4' H4'A 107.2 . . ?
Cd1' N4' H4'B 107.2 . . ?
H4'A N4' H4'B 106.9 . . ?
C10' N4' Cd1' 120.3(7) . . ?
C10' N4' H4'A 107.2 . . ?
C10' N4' H4'B 107.2 . . ?
N3 C7 H7A 108.5 . . ?
N3 C7 H7B 108.5 . . ?
N3 C7 C8 114.9(8) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H2C C2 H2D 107.7 . . ?
C1 C2 H2C 108.8 . . ?
C1 C2 H2D 108.8 . . ?
C1 C2 C3 113.9(9) . . ?
C3 C2 H2C 108.8 . . ?
C3 C2 H2D 108.8 . . ?
N4 C10 H10A 109.0 . . ?
N4 C10 H10B 109.0 . . ?
N4 C10 C11 113.1(9) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
N2 C4 H4C 109.2 . . ?
N2 C4 H4D 109.2 . . ?
N2 C4 C5 112.2(9) . . ?
H4C C4 H4D 107.9 . . ?
C5 C4 H4C 109.2 . . ?
C5 C4 H4D 109.2 . . ?
C6' C6' H6'A 108.9 2_475 . ?
C6' C6' H6'B 108.9 2_475 . ?
C6' C6' C5' 113.3(12) 2_475 . ?
H6'A C6' H6'B 107.7 . . ?
C5' C6' H6'A 108.9 . . ?
C5' C6' H6'B 108.9 . . ?
H11A C11' H11B 107.8 . . ?
C12' C11' H11A 109.1 . . ?
C12' C11' H11B 109.1 . . ?
C10' C11' H11A 109.1 . . ?
C10' C11' H11B 109.1 . . ?
C10' C11' C12' 112.5(9) . . ?
C7 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
C7 C8 C9 113.5(8) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113.4(9) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H8'A C8' H8'B 107.7 . . ?
C7' C8' H8'A 108.8 . . ?
C7' C8' H8'B 108.8 . . ?
C9' C8' H8'A 108.8 . . ?
C9' C8' H8'B 108.8 . . ?
C9' C8' C7' 113.9(9) . . ?
C10 C11 H11C 108.6 . . ?
C10 C11 H11D 108.6 . . ?
C10 C11 C12 114.5(9) . . ?
H11C C11 H11D 107.6 . . ?
C12 C11 H11C 108.6 . . ?
C12 C11 H11D 108.6 . . ?
C6' C5' H5'A 109.6 . . ?
C6' C5' H5'B 109.6 . . ?
H5'A C5' H5'B 108.2 . . ?
C4' C5' C6' 110.1(9) . . ?
C4' C5' H5'A 109.6 . . ?
C4' C5' H5'B 109.6 . . ?
H2'C C2' H2'D 107.6 . . ?
C1' C2' H2'C 108.6 . . ?
C1' C2' H2'D 108.6 . . ?
C1' C2' C3' 114.6(9) . . ?
C3' C2' H2'C 108.6 . . ?
C3' C2' H2'D 108.6 . . ?
N1' C1' C2' 113.6(9) . . ?
N1' C1' H1'C 108.8 . . ?
N1' C1' H1'D 108.8 . . ?
C2' C1' H1'C 108.8 . . ?
C2' C1' H1'D 108.8 . . ?
H1'C C1' H1'D 107.7 . . ?
N1 C1 C2 113.3(9) . . ?
N1 C1 H1C 108.9 . . ?
N1 C1 H1D 108.9 . . ?
C2 C1 H1C 108.9 . . ?
C2 C1 H1D 108.9 . . ?
H1C C1 H1D 107.7 . . ?
C2 C3 H3C 108.4 . . ?
C2 C3 H3D 108.4 . . ?
H3C C3 H3D 107.4 . . ?
C3' C3 C2 115.7(9) . . ?
C3' C3 H3C 108.4 . . ?
C3' C3 H3D 108.4 . . ?
N3' C7' C8' 116.3(9) . . ?
N3' C7' H7'A 108.2 . . ?
N3' C7' H7'B 108.2 . . ?
C8' C7' H7'A 108.2 . . ?
C8' C7' H7'B 108.2 . . ?
H7'A C7' H7'B 107.4 . . ?
N2' C4' C5' 115.9(9) . . ?
N2' C4' H4'C 108.3 . . ?
N2' C4' H4'D 108.3 . . ?
C5' C4' H4'C 108.3 . . ?
C5' C4' H4'D 108.3 . . ?
H4'C C4' H4'D 107.4 . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C12 C12 C11 114.4(11) 2_756 . ?
C12 C12 H12A 108.7 2_756 . ?
C12 C12 H12B 108.7 2_756 . ?
H12A C12 H12B 107.6 . . ?
C11' C12' H12C 108.8 . . ?
C11' C12' H12D 108.8 . . ?
C12' C12' C11' 113.7(12) 2_585 . ?
C12' C12' H12C 108.8 2_585 . ?
C12' C12' H12D 108.8 2_585 . ?
H12C C12' H12D 107.7 . . ?
C5 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
C6 C6 C5 113.7(12) 2_866 . ?
C6 C6 H6A 108.8 2_866 . ?
C6 C6 H6B 108.8 2_866 . ?
H6A C6 H6B 107.7 . . ?
C2' C3' H3'C 108.3 . . ?
C2' C3' H3'D 108.3 . . ?
C3 C3' C2' 115.9(9) . . ?
C3 C3' H3'C 108.3 . . ?
C3 C3' H3'D 108.3 . . ?
H3'C C3' H3'D 107.4 . . ?
C8 C9 C9 113.0(12) . 2_865 ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C9 C9 H9A 109.0 2_865 . ?
C9 C9 H9B 109.0 2_865 . ?
H9A C9 H9B 107.8 . . ?
N4' C10' C11' 115.4(9) . . ?
N4' C10' H10C 108.4 . . ?
N4' C10' H10D 108.4 . . ?
C11' C10' H10C 108.4 . . ?
C11' C10' H10D 108.4 . . ?
H10C C10' H10D 107.5 . . ?
C8' C9' C9' 113.2(12) . 2_476 ?
C8' C9' H9'A 108.9 . . ?
C8' C9' H9'B 108.9 . . ?
C9' C9' H9'A 108.9 2_476 . ?
C9' C9' H9'B 108.9 2_476 . ?
H9'A C9' H9'B 107.8 . . ?

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
Cd1 O4 N6 O5 -1.5(13) . . . . ?
Cd1 O4 N6 O6 -179.7(10) . . . . ?
Cd1 O1 N5 O3 -172.6(8) . . . . ?
Cd1 O1 N5 O2 8.0(11) . . . . ?
Cd1 N3 C7 C8 166.1(7) . . . . ?
Cd1 N4 C10 C11 171.6(7) . . . . ?
Cd1 N2 C4 C5 -176.7(6) . . . . ?
Cd1 N1 C1 C2 -173.1(7) . . . . ?
Cd1' O2' N5' O1' 3.4(9) . . . . ?
Cd1' O2' N5' O3' -176.0(9) . . . . ?
Cd1' O1' N5' O2' -3.5(10) . . . . ?
Cd1' O1' N5' O3' 175.8(9) . . . . ?
Cd1' N2' C4' C5' -176.5(7) . . . . ?
Cd1' N1' C1' C2' 173.7(7) . . . . ?
Cd1' N3' C7' C8' -178.4(7) . . . . ?
Cd1' N4' C10' C11' 162.2(7) . . . . ?
N3 C7 C8 C9 -178.1(8) . . . . ?
N4 C10 C11 C12 175.4(9) . . . . ?
N2 C4 C5 C6 -177.4(9) . . . . ?
C7 C8 C9 C9 -65.5(15) . . . 2_865 ?
C2 C3 C3' C2' -178.1(9) . . . . ?
C10 C11 C12 C12 53.8(16) . . . 2_756 ?
C4 C5 C6 C6 -64.9(16) . . . 2_866 ?
C6' C6' C5' C4' -169.2(11) 2_475 . . . ?
C6' C5' C4' N2' 177.2(9) . . . . ?
C1' C2' C3' C3 -63.1(14) . . . . ?
C1 C2 C3 C3' 60.1(14) . . . . ?
C3 C2 C1 N1 172.1(9) . . . . ?
C7' C8' C9' C9' -176.3(12) . . . 2_476 ?
C12' C11' C10' N4' -66.8(12) . . . . ?
C3' C2' C1' N1' -173.5(9) . . . . ?
C10' C11' C12' C12' 178.7(12) . . . 2_585 ?
C9' C8' C7' N3' -71.0(14) . . . . ?

_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 1.099
_oxdiff_exptl_absorpt_empirical_full_min 0.859
####################################################################### 
# 
# 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_100_K_Cd_HDA_2_NO3_2_fast_cooling
_database_code_depnum_ccdc_archive 'CCDC 2262358'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd N4 O4 C12'
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'
Cd Cd -0.8075 1.2024 '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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   9.5843(7)
_cell_length_b                   9.5843(7)
_cell_length_c                   20.900(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1919.9(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2963
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      26.6730
_cell_measurement_theta_min      3.5520
_shelx_estimated_absorpt_T_max   0.793
_shelx_estimated_absorpt_T_min   0.675
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -4 18 0.1001
3 -12 -14 0.0904
-2 11 15 0.1112
-10 5 -17 0.1765
11 1 -17 0.1838
-11 -1 17 0.0199

_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.198
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
9.7666 -4.3860 17.9992 0.1836 0.7530 0.6318
2.5389 -11.5584 -14.2618 0.1664 0.6994 -0.6950
-2.1706 11.4813 14.8367 -0.1656 -0.6752 0.7188
-9.8696 5.0096 -16.9242 -0.1879 -0.7890 -0.5849
11.0374 0.7214 -16.8333 -0.7853 0.6044 -0.1342
-10.8886 -0.5879 17.3133 0.7827 -0.6025 0.1560

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5245
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_min         3.583
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  91.00   1.00    5.00    --   17.63   0.00   0.00  146
  2  ω    -25.00  23.00   1.00    5.00    --  -18.80 -99.00 -30.00   48
  3  ω    -40.00  36.00   1.00    5.00    --  -18.80  57.00 -90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0382800000
_diffrn_orient_matrix_UB_12      -0.0469153000
_diffrn_orient_matrix_UB_13      0.0195400000
_diffrn_orient_matrix_UB_21      0.0569550000
_diffrn_orient_matrix_UB_22      -0.0472786000
_diffrn_orient_matrix_UB_23      -0.0005872000
_diffrn_orient_matrix_UB_31      0.0280167000
_diffrn_orient_matrix_UB_32      0.0320851000
_diffrn_orient_matrix_UB_33      0.0277194000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1077
_reflns_number_total             1155
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1155
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0713
_refine_ls_restrained_S_all      1.309
_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)+(0.0317P)²+35.1579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1613
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C3B, Cd1, N1, H1A, H1B, C1, H1C, H1D, C2, H2BC, H2BD, H2AA, H2AB, C3A, H3AA,
 H3AB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2BC,H2BD), C2(H2AA,H2AB), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_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
Cd1 Cd 1.000000 0.750000 0.375000 0.0235(3) Uani 1 4 d S T P . .
N1 N 0.8178(7) 0.5964(7) 0.3598(4) 0.054(2) Uani 1 1 d . . . . .
H1A H 0.797004 0.559265 0.398758 0.064 Uiso 1 1 calc R U . . .
H1B H 0.742554 0.647833 0.347660 0.064 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.5249(5) 0.056(3) Uani 1 2 d S T P . .
O1 O 1.0722(7) 0.8355(7) 0.4941(4) 0.0608(18) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.5820(5) 0.130(7) Uani 1 2 d S TU P . .
C1 C 0.8287(11) 0.4835(10) 0.3162(6) 0.063(3) Uani 1 1 d . . . . .
H1C H 0.917423 0.433602 0.324387 0.076 Uiso 1 1 calc R U . . .
H1D H 0.832771 0.521264 0.272188 0.076 Uiso 1 1 calc R U . . .
C2 C 0.7064(9) 0.3773(8) 0.3204(4) 0.045(2) Uani 1 1 d . . . . .
H2BC H 0.688114 0.350449 0.365408 0.054 Uiso 0.61(3) 1 calc R U P A 2
H2BD H 0.620097 0.416796 0.301786 0.054 Uiso 0.61(3) 1 calc R U P A 2
H2AA H 0.619247 0.428889 0.329710 0.054 Uiso 0.39(3) 1 calc R U P A 1
H2AB H 0.723986 0.313343 0.356757 0.054 Uiso 0.39(3) 1 calc R U P A 1
C3B C 0.757(2) 0.252(2) 0.2816(9) 0.077(7) Uani 0.61(3) 1 d . . P A 2
H3BA H 0.858294 0.241715 0.290656 0.092 Uiso 0.61(3) 1 calc R U P A 2
H3BB H 0.710598 0.168751 0.299180 0.092 Uiso 0.61(3) 1 calc R U P A 2
C3A C 0.685(2) 0.288(2) 0.2581(11) 0.034(6) Uani 0.39(3) 1 d . . P A 1
H3AA H 0.607915 0.220345 0.264927 0.040 Uiso 0.39(3) 1 calc R U P A 1
H3AB H 0.658022 0.349945 0.222189 0.040 Uiso 0.39(3) 1 calc R U 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
Cd1 N1 2.306(7) 3_765 ?
Cd1 N1 2.306(7) 12_756 ?
Cd1 N1 2.306(7) 10_676 ?
Cd1 N1 2.306(7) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.418(11) . ?
N2 O1 1.250(8) . ?
N2 O1 1.250(8) 3_765 ?
N2 O2 1.194(15) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C1 C2 1.555(12) . ?
C2 H2BC 0.9900 . ?
C2 H2BD 0.9900 . ?
C2 H2AA 0.9900 . ?
C2 H2AB 0.9900 . ?
C2 C3B 1.527(18) . ?
C2 C3A 1.57(2) . ?
C3B C3B 1.33(4) 13_655 ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3A C3A 1.49(4) 13_655 ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?

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 Cd1 N1 91.08(6) 3_765 12_756 ?
N1 Cd1 N1 91.08(6) 12_756 . ?
N1 Cd1 N1 91.08(6) 3_765 10_676 ?
N1 Cd1 N1 91.08(6) 10_676 . ?
N1 Cd1 N1 164.2(4) 3_765 . ?
N1 Cd1 N1 164.2(4) 12_756 10_676 ?
Cd1 N1 H1A 107.0 . . ?
Cd1 N1 H1B 107.0 . . ?
H1A N1 H1B 106.7 . . ?
C1 N1 Cd1 121.3(6) . . ?
C1 N1 H1A 107.0 . . ?
C1 N1 H1B 107.0 . . ?
O1 N2 O1 118.1(12) . 3_765 ?
O2 N2 O1 120.9(6) . . ?
O2 N2 O1 120.9(6) . 3_765 ?
N1 C1 H1C 108.7 . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 C2 114.0(8) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.7 . . ?
C2 C1 H1D 108.7 . . ?
C1 C2 H2BC 111.0 . . ?
C1 C2 H2BD 111.0 . . ?
C1 C2 H2AA 108.7 . . ?
C1 C2 H2AB 108.7 . . ?
C1 C2 C3A 114.2(10) . . ?
H2BC C2 H2BD 109.0 . . ?
H2AA C2 H2AB 107.6 . . ?
C3B C2 C1 104.0(11) . . ?
C3B C2 H2BC 111.0 . . ?
C3B C2 H2BD 111.0 . . ?
C3A C2 H2AA 108.7 . . ?
C3A C2 H2AB 108.7 . . ?
C2 C3B H3BA 107.0 . . ?
C2 C3B H3BB 107.0 . . ?
C3B C3B C2 121(2) 13_655 . ?
C3B C3B H3BA 107.0 13_655 . ?
C3B C3B H3BB 107.0 13_655 . ?
H3BA C3B H3BB 106.7 . . ?
C2 C3A H3AA 109.7 . . ?
C2 C3A H3AB 109.7 . . ?
C3A C3A C2 110(2) 13_655 . ?
C3A C3A H3AA 109.7 13_655 . ?
C3A C3A H3AB 109.7 13_655 . ?
H3AA C3A H3AB 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 N1 C1 C2 170.4(7) . . . . ?
N1 C1 C2 C3B -167.4(12) . . . . ?
N1 C1 C2 C3A 157.6(12) . . . . ?
C1 C2 C3B C3B -85(3) . . . 13_655 ?
C1 C2 C3A C3A 57(2) . . . 13_655 ?

_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 1.041
_oxdiff_exptl_absorpt_empirical_full_min 0.969
####################################################################### 
# 
# 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_100_K_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262357'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_100_K_Cd_HDA_2_NO3_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.97Ang From Cd1'            4.86 eA-3 
RESPONSE: The crystals all showed strong diffuse scattering in the form
 of diffuse Bragg peaks and scattering between them. As the model
 does not account for this type of disorder this is
 believe to be the source of the high electron density on the Cd cation.
 PROBLEM: Check Calcd Resid. Dens.  0.87Ang From Cd1             3.53 eA-3 
RESPONSE: The crystals all showed strong diffuse scattering in the form
 of diffuse Bragg peaks and scattering between them. As the model
 does not account for this type of disorder this is
 believe to be the source of the high electron density on the Cd cation.
;
_vrf_PLAT973_100_K_Cd_HDA_2_NO3_2 
;
PROBLEM: Check Calcd Positive Resid. Density on       Cd1       2.21 eA-3
RESPONSE: The crystals all showed strong diffuse scattering in the form
 of diffuse Bragg peaks and scattering between them. As the model
 does not account for this type of disorder this is
 believe to be the source of the high electron density on the Cd cation.
;
_vrf_PLAT097_100_K_Cd_HDA_2_NO3_2 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       4.95 eA-3  
RESPONSE: The crystals all showed strong diffuse scattering in the form
 of diffuse Bragg peaks and scattering between them. As the model
 does not account for this type of disorder this is
 believe to be the source of the high electron density on the Cd cation.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:18 PM
# end Validation Reply Form

_audit_creation_date             2022-11-07
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cd N5.5 O4.5, 0.5(N O3)'
_chemical_formula_sum            'C12 H32 Cd N6 O6'
_chemical_formula_weight         468.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         CdC6N6O6
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'
Cd Cd -0.8075 1.2024 '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      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                   9.9729(8)
_cell_length_b                   12.1703(10)
_cell_length_c                   18.0586(17)
_cell_angle_alpha                74.687(7)
_cell_angle_beta                 74.744(7)
_cell_angle_gamma                68.239(7)
_cell_volume                     1929.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      25.2810
_cell_measurement_theta_min      2.7670
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.713
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 9 8 0.1099
-10 -13 4 0.0823
11 12 -5 0.0477
-11 5 -8 0.1292
3 7 25 0.0220
-3 -7 -25 0.1253
4 17 1 0.0476
1 -16 -5 0.1216

_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.127
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.8510 8.6109 7.5884 0.0208 -0.0008 0.9998
-10.3410 -12.5025 4.1000 -0.9615 0.1797 0.2079
10.6812 11.8155 -4.5064 0.9476 -0.1773 -0.2658
-10.8448 4.6460 -7.5924 0.1027 0.5672 0.8172
3.1238 6.9280 25.0676 -0.1660 -0.8829 0.4392
-3.0010 -6.9955 -25.0231 0.1651 0.8778 -0.4497
4.4487 16.7322 1.1218 0.8827 -0.1659 0.4397
0.9332 -15.9849 -4.9337 -0.6153 0.1240 -0.8193

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.1344
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23553
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         2.332
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  90.00   0.80    6.00    --   21.75  73.00  14.00  120
  2  ω      8.00  85.60   0.80    6.00    --   21.75-136.00-171.00   97
  3  ω     39.00  96.60   0.80    6.00    --   21.75 178.00 -90.00   72
  4  ω     39.00  96.60   0.80    6.00    --   21.75 178.00  30.00   72
  5  ω     -8.00  37.60   0.80    6.00    --   21.75  77.00-120.00   57
  6  ω    -39.00   6.60   0.80    6.00    --  -22.69 -77.00 -90.00   57
  7  ω    -47.00  42.60   0.80    6.00    --   21.75 -57.00  30.00  112
  8  ω      0.00  90.40   0.80    6.00    --   21.75  57.00 150.00  113
  9  ω    -95.00 -70.20   0.80    6.00    --  -22.69 -37.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268409000
_diffrn_orient_matrix_UB_12      0.0471603000
_diffrn_orient_matrix_UB_13      -0.0230024000
_diffrn_orient_matrix_UB_21      -0.0301385000
_diffrn_orient_matrix_UB_22      0.0002145000
_diffrn_orient_matrix_UB_23      -0.0315239000
_diffrn_orient_matrix_UB_31      -0.0666507000
_diffrn_orient_matrix_UB_32      0.0430660000
_diffrn_orient_matrix_UB_33      0.0139259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6417
_reflns_number_total             10332
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.946
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1538
_refine_ls_R_factor_gt           0.0939
_refine_ls_restrained_S_all      1.088
_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)+(0.1073P)²+12.3753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2613
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N2'(H2'A,H2'B), N2(H2A,H2B), N1'(H1'A,H1'B), N1(H1A,
 H1B), N3'(H3'A,H3'B), N4'(H4'A,H4'B), C7(H7A,H7B), C2(H2C,H2D), C10(H10A,H10B),
  C4(H4C,H4D), C6'(H6'A,H6'B), C11'(H11A,H11B), C8(H8A,H8B), C5(H5A,H5B),
 C8'(H8'A,H8'B), C11(H11C,H11D), C5'(H5'A,H5'B), C2'(H2'C,H2'D), C1'(H1'C,H1'D),
  C1(H1C,H1D), C3(H3C,H3D), C7'(H7'A,H7'B), C4'(H4'C,H4'D), C12(H12A,H12B),
 C12'(H12C,H12D), C6(H6A,H6B), C3'(H3'C,H3'D), C9(H9A,H9B), C10'(H10C,H10D),
 C9'(H9'A,H9'B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 1.11614(7) 0.44991(6) 0.31294(4) 0.02045(19) Uani 1 1 d . . . . .
Cd1' Cd -0.08710(7) 1.05966(6) 0.18939(4) 0.02078(19) Uani 1 1 d . . . . .
O4 O 1.1799(7) 0.2917(7) 0.2380(4) 0.0307(16) Uani 1 1 d . . . . .
O2' O -0.0564(8) 0.8456(7) 0.1817(4) 0.0329(17) Uani 1 1 d . . . . .
O1 O 0.9492(8) 0.5798(7) 0.4081(4) 0.0329(17) Uani 1 1 d . . . . .
O3 O 0.9292(8) 0.7444(7) 0.4404(4) 0.0344(17) Uani 1 1 d . . . . .
O1' O 0.0711(8) 0.9389(7) 0.0891(4) 0.0316(16) Uani 1 1 d . . . . .
O2 O 1.0767(8) 0.6908(7) 0.3356(4) 0.0363(18) Uani 1 1 d . . . . .
N3 N 1.2979(8) 0.5187(7) 0.2285(5) 0.0235(17) Uani 1 1 d . . . . .
H3A H 1.272953 0.598446 0.229016 0.028 Uiso 1 1 calc R U . . .
H3B H 1.382114 0.480509 0.248186 0.028 Uiso 1 1 calc R U . . .
N4 N 0.9533(9) 0.3491(7) 0.3877(5) 0.0253(17) Uani 1 1 d . . . . .
H4A H 0.916162 0.377514 0.433205 0.030 Uiso 1 1 calc R U . . .
H4B H 0.877198 0.371989 0.362047 0.030 Uiso 1 1 calc R U . . .
N2' N -0.2370(8) 1.1347(7) 0.0958(5) 0.0247(17) Uani 1 1 d . . . . .
H2'A H -0.307285 1.204860 0.106326 0.030 Uiso 1 1 calc R U . . .
H2'B H -0.182107 1.150960 0.047943 0.030 Uiso 1 1 calc R U . . .
N5 N 0.9848(8) 0.6727(7) 0.3943(5) 0.0222(17) Uani 1 1 d . . . . .
N2 N 1.2612(8) 0.3703(8) 0.4092(5) 0.0238(17) Uani 1 1 d . . . . .
H2A H 1.211572 0.331678 0.451239 0.029 Uiso 1 1 calc R U . . .
H2B H 1.344084 0.313252 0.390741 0.029 Uiso 1 1 calc R U . . .
N1' N 0.0698(8) 0.9517(7) 0.2775(5) 0.0233(17) Uani 1 1 d . . . . .
H1'A H 0.061863 1.000764 0.309803 0.028 Uiso 1 1 calc R U . . .
H1'B H 0.038382 0.889835 0.307368 0.028 Uiso 1 1 calc R U . . .
N6 N 1.3090(9) 0.2165(8) 0.2363(5) 0.0286(19) Uani 1 1 d . . . . .
O3' O 0.0777(9) 0.7600(7) 0.0841(5) 0.041(2) Uani 1 1 d . . . . .
N5' N 0.0310(9) 0.8472(7) 0.1172(5) 0.0249(17) Uani 1 1 d . . . . .
N1 N 0.9554(8) 0.5559(8) 0.2244(5) 0.0244(17) Uani 1 1 d . . . . .
H1A H 0.989578 0.615067 0.192262 0.029 Uiso 1 1 calc R U . . .
H1B H 0.961947 0.504299 0.194158 0.029 Uiso 1 1 calc R U . . .
N3' N -0.2883(9) 1.0745(7) 0.2903(5) 0.0293(19) Uani 1 1 d . . . . .
H3'A H -0.277897 1.110285 0.325844 0.035 Uiso 1 1 calc R U . . .
H3'B H -0.370434 1.123339 0.270776 0.035 Uiso 1 1 calc R U . . .
N6' N -0.3146(9) 1.3506(8) 0.2573(5) 0.0299(19) Uani 1 1 d . . . . .
O5 O 1.3926(9) 0.2308(8) 0.2715(6) 0.050(2) Uani 1 1 d . . . . .
O6' O -0.4285(8) 1.3888(8) 0.3028(5) 0.043(2) Uani 1 1 d . . . . .
O5' O -0.3154(8) 1.3573(8) 0.1865(5) 0.041(2) Uani 1 1 d . . . . .
N4' N 0.0132(9) 1.2095(8) 0.1463(5) 0.0284(19) Uani 1 1 d . . . . .
H4'A H -0.061976 1.280506 0.146083 0.034 Uiso 1 1 calc R U . . .
H4'B H 0.065050 1.204407 0.182365 0.034 Uiso 1 1 calc R U . . .
O6 O 1.3504(11) 0.1351(9) 0.2007(7) 0.066(3) Uani 1 1 d . . . . .
C7 C 1.3320(10) 0.5049(8) 0.1460(5) 0.0199(18) Uani 1 1 d . . . . .
H7A H 1.238349 0.527937 0.127620 0.024 Uiso 1 1 calc R U . . .
H7B H 1.384340 0.418819 0.143383 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7045(9) 0.6658(9) 0.1923(5) 0.024(2) Uani 1 1 d . . . . .
H2C H 0.726660 0.604881 0.159957 0.029 Uiso 1 1 calc R U . . .
H2D H 0.732387 0.735150 0.158005 0.029 Uiso 1 1 calc R U . . .
C10 C 1.0021(11) 0.2160(8) 0.4084(5) 0.0230(19) Uani 1 1 d . . . . .
H10A H 1.093100 0.187236 0.430187 0.028 Uiso 1 1 calc R U . . .
H10B H 1.024945 0.182126 0.360656 0.028 Uiso 1 1 calc R U . . .
C4 C 1.3069(10) 0.4516(9) 0.4375(6) 0.024(2) Uani 1 1 d . . . . .
H4C H 1.218561 0.510663 0.461862 0.029 Uiso 1 1 calc R U . . .
H4D H 1.358631 0.496658 0.392569 0.029 Uiso 1 1 calc R U . . .
C6' C -0.4644(10) 0.9897(8) 0.0341(6) 0.023(2) Uani 1 1 d . . . . .
H6'A H -0.383068 0.912104 0.035419 0.028 Uiso 1 1 calc R U . . .
H6'B H -0.537344 0.982790 0.082839 0.028 Uiso 1 1 calc R U . . .
C11' C 0.1312(11) 1.3387(9) 0.0369(6) 0.027(2) Uani 1 1 d . . . . .
H11A H 0.209373 1.332896 -0.010261 0.032 Uiso 1 1 calc R U . . .
H11B H 0.164282 1.361197 0.076190 0.032 Uiso 1 1 calc R U . . .
C8 C 1.4233(10) 0.5775(9) 0.0909(6) 0.0222(19) Uani 1 1 d . . . . .
H8A H 1.518736 0.552351 0.107734 0.027 Uiso 1 1 calc R U . . .
H8B H 1.372892 0.663440 0.094563 0.027 Uiso 1 1 calc R U . . .
O4' O -0.1967(9) 1.3067(11) 0.2803(6) 0.071(4) Uani 1 1 d . . . . .
C5 C 1.4084(10) 0.3830(9) 0.4973(6) 0.026(2) Uani 1 1 d . . . . .
H5A H 1.357144 0.336286 0.541371 0.032 Uiso 1 1 calc R U . . .
H5B H 1.497255 0.324992 0.472343 0.032 Uiso 1 1 calc R U . . .
C8' C -0.4445(10) 0.9673(9) 0.3950(5) 0.025(2) Uani 1 1 d . . . . .
H8'A H -0.531639 1.027341 0.374642 0.030 Uiso 1 1 calc R U . . .
H8'B H -0.460470 0.888097 0.409702 0.030 Uiso 1 1 calc R U . . .
C11 C 0.8857(10) 0.1712(8) 0.4676(6) 0.0232(19) Uani 1 1 d . . . . .
H11C H 0.792396 0.206298 0.447575 0.028 Uiso 1 1 calc R U . . .
H11D H 0.868976 0.200097 0.516702 0.028 Uiso 1 1 calc R U . . .
C5' C -0.4044(11) 1.0882(10) 0.0322(6) 0.029(2) Uani 1 1 d . . . . .
H5'A H -0.486738 1.162431 0.041983 0.035 Uiso 1 1 calc R U . . .
H5'B H -0.345341 1.106251 -0.020088 0.035 Uiso 1 1 calc R U . . .
C2' C 0.3264(10) 0.8438(10) 0.3046(6) 0.028(2) Uani 1 1 d . . . . .
H2'C H 0.305952 0.901994 0.338677 0.033 Uiso 1 1 calc R U . . .
H2'D H 0.301292 0.772582 0.337690 0.033 Uiso 1 1 calc R U . . .
C1' C 0.2264(9) 0.9017(10) 0.2435(6) 0.028(2) Uani 1 1 d . . . . .
H1'C H 0.258922 0.966975 0.206448 0.033 Uiso 1 1 calc R U . . .
H1'D H 0.237658 0.840459 0.213516 0.033 Uiso 1 1 calc R U . . .
C1 C 0.7972(9) 0.6124(9) 0.2549(6) 0.026(2) Uani 1 1 d . . . . .
H1C H 0.786626 0.676644 0.282214 0.031 Uiso 1 1 calc R U . . .
H1D H 0.759853 0.551055 0.293674 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5397(10) 0.7079(10) 0.2238(6) 0.028(2) Uani 1 1 d . . . . .
H3C H 0.487431 0.737280 0.179165 0.033 Uiso 1 1 calc R U . . .
H3D H 0.511701 0.637853 0.256732 0.033 Uiso 1 1 calc R U . . .
C7' C -0.3098(10) 0.9606(10) 0.3301(6) 0.029(2) Uani 1 1 d . . . . .
H7'A H -0.221531 0.908829 0.352721 0.035 Uiso 1 1 calc R U . . .
H7'B H -0.316747 0.920461 0.290826 0.035 Uiso 1 1 calc R U . . .
C4' C -0.3086(11) 1.0485(10) 0.0943(7) 0.034(2) Uani 1 1 d . . . . .
H4'C H -0.370246 1.033518 0.146231 0.041 Uiso 1 1 calc R U . . .
H4'D H -0.231222 0.971191 0.085846 0.041 Uiso 1 1 calc R U . . .
C12 C 0.9266(11) 0.0322(9) 0.4860(6) 0.028(2) Uani 1 1 d . . . . .
H12A H 0.848079 0.009612 0.526819 0.033 Uiso 1 1 calc R U . . .
H12B H 0.931159 0.004102 0.438452 0.033 Uiso 1 1 calc R U . . .
C12' C -0.0087(12) 1.4380(9) 0.0156(6) 0.028(2) Uani 1 1 d . . . . .
H12C H -0.040732 1.415876 -0.024237 0.034 Uiso 1 1 calc R U . . .
H12D H -0.087313 1.442454 0.062626 0.034 Uiso 1 1 calc R U . . .
C6 C 1.4550(12) 0.4645(11) 0.5290(6) 0.033(2) Uani 1 1 d . . . . .
H6A H 1.365378 0.521848 0.553948 0.040 Uiso 1 1 calc R U . . .
H6B H 1.512010 0.414267 0.570398 0.040 Uiso 1 1 calc R U . . .
C3' C 0.4886(10) 0.8050(9) 0.2707(6) 0.027(2) Uani 1 1 d . . . . .
H3'C H 0.513247 0.876129 0.237066 0.032 Uiso 1 1 calc R U . . .
H3'D H 0.543863 0.776780 0.314053 0.032 Uiso 1 1 calc R U . . .
C9 C 1.4520(11) 0.5649(8) 0.0056(6) 0.024(2) Uani 1 1 d . . . . .
H9A H 1.502406 0.622209 -0.027764 0.029 Uiso 1 1 calc R U . . .
H9B H 1.357203 0.585453 -0.010964 0.029 Uiso 1 1 calc R U . . .
C10' C 0.1106(11) 1.2173(9) 0.0690(6) 0.029(2) Uani 1 1 d . . . . .
H10C H 0.069382 1.198231 0.031594 0.034 Uiso 1 1 calc R U . . .
H10D H 0.207930 1.155603 0.073278 0.034 Uiso 1 1 calc R U . . .
C9' C -0.4331(10) 1.0002(11) 0.4662(6) 0.030(2) Uani 1 1 d . . . . .
H9'A H -0.423135 1.081485 0.452253 0.036 Uiso 1 1 calc R U . . .
H9'B H -0.342948 0.942892 0.484967 0.036 Uiso 1 1 calc R U . . .


_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
Cd1 O4 2.441(7) . ?
Cd1 O1 2.490(7) . ?
Cd1 N3 2.305(8) . ?
Cd1 N4 2.326(8) . ?
Cd1 N2 2.334(8) . ?
Cd1 N1 2.349(8) . ?
Cd1' O2' 2.545(7) . ?
Cd1' O1' 2.472(7) . ?
Cd1' N2' 2.329(8) . ?
Cd1' N1' 2.321(8) . ?
Cd1' N3' 2.316(9) . ?
Cd1' N4' 2.264(9) . ?
O4 N6 1.271(11) . ?
O2' N5' 1.258(11) . ?
O1 N5 1.252(10) . ?
O3 N5 1.243(10) . ?
O1' N5' 1.261(11) . ?
O2 N5 1.236(10) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C7 1.479(11) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C10 1.481(12) . ?
N2' H2'A 0.9100 . ?
N2' H2'B 0.9100 . ?
N2' C4' 1.479(13) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C4 1.474(12) . ?
N1' H1'A 0.9100 . ?
N1' H1'B 0.9100 . ?
N1' C1' 1.475(11) . ?
N6 O5 1.254(11) . ?
N6 O6 1.209(12) . ?
O3' N5' 1.234(10) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.484(11) . ?
N3' H3'A 0.9100 . ?
N3' H3'B 0.9100 . ?
N3' C7' 1.449(13) . ?
N6' O6' 1.225(11) . ?
N6' O5' 1.262(11) . ?
N6' O4' 1.231(11) . ?
N4' H4'A 0.9100 . ?
N4' H4'B 0.9100 . ?
N4' C10' 1.477(13) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.501(12) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C1 1.507(13) . ?
C2 C3 1.525(12) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.516(13) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C4 C5 1.536(13) . ?
C6' C6' 1.499(18) 2_475 ?
C6' H6'A 0.9900 . ?
C6' H6'B 0.9900 . ?
C6' C5' 1.516(13) . ?
C11' H11A 0.9900 . ?
C11' H11B 0.9900 . ?
C11' C12' 1.530(14) . ?
C11' C10' 1.507(14) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.529(13) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.521(14) . ?
C8' H8'A 0.9900 . ?
C8' H8'B 0.9900 . ?
C8' C7' 1.526(13) . ?
C8' C9' 1.487(14) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C11 C12 1.549(13) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C5' C4' 1.530(14) . ?
C2' H2'C 0.9900 . ?
C2' H2'D 0.9900 . ?
C2' C1' 1.535(13) . ?
C2' C3' 1.510(12) . ?
C1' H1'C 0.9900 . ?
C1' H1'D 0.9900 . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C3' 1.492(14) . ?
C7' H7'A 0.9900 . ?
C7' H7'B 0.9900 . ?
C4' H4'C 0.9900 . ?
C4' H4'D 0.9900 . ?
C12 C12 1.530(19) 2_756 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12' C12' 1.522(19) 2_585 ?
C12' H12C 0.9900 . ?
C12' H12D 0.9900 . ?
C6 C6 1.50(2) 2_866 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3' H3'C 0.9900 . ?
C3' H3'D 0.9900 . ?
C9 C9 1.550(18) 2_865 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C9' C9' 1.553(18) 2_476 ?
C9' H9'A 0.9900 . ?
C9' H9'B 0.9900 . ?

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 Cd1 O1 153.2(2) . . ?
N3 Cd1 O4 89.1(3) . . ?
N3 Cd1 O1 116.3(3) . . ?
N3 Cd1 N4 169.4(3) . . ?
N3 Cd1 N2 90.2(3) . . ?
N3 Cd1 N1 90.1(3) . . ?
N4 Cd1 O4 80.6(3) . . ?
N4 Cd1 O1 74.3(3) . . ?
N4 Cd1 N2 90.3(3) . . ?
N4 Cd1 N1 91.0(3) . . ?
N2 Cd1 O4 106.2(3) . . ?
N2 Cd1 O1 83.4(3) . . ?
N2 Cd1 N1 171.5(3) . . ?
N1 Cd1 O4 82.3(3) . . ?
N1 Cd1 O1 88.9(3) . . ?
O1' Cd1' O2' 50.9(2) . . ?
N2' Cd1' O2' 90.1(3) . . ?
N2' Cd1' O1' 80.6(3) . . ?
N1' Cd1' O2' 79.8(3) . . ?
N1' Cd1' O1' 91.8(3) . . ?
N1' Cd1' N2' 169.8(3) . . ?
N3' Cd1' O2' 94.1(3) . . ?
N3' Cd1' O1' 143.7(3) . . ?
N3' Cd1' N2' 91.7(3) . . ?
N3' Cd1' N1' 90.5(3) . . ?
N4' Cd1' O2' 145.1(3) . . ?
N4' Cd1' O1' 95.5(3) . . ?
N4' Cd1' N2' 93.6(3) . . ?
N4' Cd1' N1' 94.0(3) . . ?
N4' Cd1' N3' 120.4(3) . . ?
N6 O4 Cd1 116.1(6) . . ?
N5' O2' Cd1' 93.8(5) . . ?
N5 O1 Cd1 107.9(6) . . ?
N5' O1' Cd1' 97.2(5) . . ?
Cd1 N3 H3A 107.7 . . ?
Cd1 N3 H3B 107.7 . . ?
H3A N3 H3B 107.1 . . ?
C7 N3 Cd1 118.6(5) . . ?
C7 N3 H3A 107.7 . . ?
C7 N3 H3B 107.7 . . ?
Cd1 N4 H4A 107.1 . . ?
Cd1 N4 H4B 107.1 . . ?
H4A N4 H4B 106.8 . . ?
C10 N4 Cd1 120.9(6) . . ?
C10 N4 H4A 107.1 . . ?
C10 N4 H4B 107.1 . . ?
Cd1' N2' H2'A 109.2 . . ?
Cd1' N2' H2'B 109.2 . . ?
H2'A N2' H2'B 107.9 . . ?
C4' N2' Cd1' 111.9(6) . . ?
C4' N2' H2'A 109.2 . . ?
C4' N2' H2'B 109.2 . . ?
O3 N5 O1 119.7(8) . . ?
O2 N5 O1 119.4(8) . . ?
O2 N5 O3 120.9(9) . . ?
Cd1 N2 H2A 107.5 . . ?
Cd1 N2 H2B 107.5 . . ?
H2A N2 H2B 107.0 . . ?
C4 N2 Cd1 119.3(6) . . ?
C4 N2 H2A 107.5 . . ?
C4 N2 H2B 107.5 . . ?
Cd1' N1' H1'A 108.2 . . ?
Cd1' N1' H1'B 108.2 . . ?
H1'A N1' H1'B 107.4 . . ?
C1' N1' Cd1' 116.2(6) . . ?
C1' N1' H1'A 108.2 . . ?
C1' N1' H1'B 108.2 . . ?
O5 N6 O4 118.1(8) . . ?
O6 N6 O4 120.8(9) . . ?
O6 N6 O5 121.1(9) . . ?
O2' N5' O1' 117.8(8) . . ?
O3' N5' O2' 120.5(9) . . ?
O3' N5' O1' 121.7(9) . . ?
Cd1 N1 H1A 107.5 . . ?
Cd1 N1 H1B 107.5 . . ?
H1A N1 H1B 107.0 . . ?
C1 N1 Cd1 119.2(6) . . ?
C1 N1 H1A 107.5 . . ?
C1 N1 H1B 107.5 . . ?
Cd1' N3' H3'A 108.6 . . ?
Cd1' N3' H3'B 108.6 . . ?
H3'A N3' H3'B 107.6 . . ?
C7' N3' Cd1' 114.5(6) . . ?
C7' N3' H3'A 108.6 . . ?
C7' N3' H3'B 108.6 . . ?
O6' N6' O5' 121.1(8) . . ?
O6' N6' O4' 119.8(9) . . ?
O4' N6' O5' 119.0(9) . . ?
Cd1' N4' H4'A 107.4 . . ?
Cd1' N4' H4'B 107.4 . . ?
H4'A N4' H4'B 106.9 . . ?
C10' N4' Cd1' 119.8(6) . . ?
C10' N4' H4'A 107.4 . . ?
C10' N4' H4'B 107.4 . . ?
N3 C7 H7A 108.5 . . ?
N3 C7 H7B 108.5 . . ?
N3 C7 C8 115.3(7) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H2C C2 H2D 107.7 . . ?
C1 C2 H2C 108.8 . . ?
C1 C2 H2D 108.8 . . ?
C1 C2 C3 114.0(8) . . ?
C3 C2 H2C 108.8 . . ?
C3 C2 H2D 108.8 . . ?
N4 C10 H10A 109.3 . . ?
N4 C10 H10B 109.3 . . ?
N4 C10 C11 111.7(8) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
N2 C4 H4C 109.2 . . ?
N2 C4 H4D 109.2 . . ?
N2 C4 C5 112.1(8) . . ?
H4C C4 H4D 107.9 . . ?
C5 C4 H4C 109.2 . . ?
C5 C4 H4D 109.2 . . ?
C6' C6' H6'A 108.8 2_475 . ?
C6' C6' H6'B 108.8 2_475 . ?
C6' C6' C5' 113.9(10) 2_475 . ?
H6'A C6' H6'B 107.7 . . ?
C5' C6' H6'A 108.8 . . ?
C5' C6' H6'B 108.8 . . ?
H11A C11' H11B 107.8 . . ?
C12' C11' H11A 108.9 . . ?
C12' C11' H11B 108.9 . . ?
C10' C11' H11A 108.9 . . ?
C10' C11' H11B 108.9 . . ?
C10' C11' C12' 113.2(8) . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C7 C8 C9 114.1(8) . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 C4 113.5(9) . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H8'A C8' H8'B 107.6 . . ?
C7' C8' H8'A 108.7 . . ?
C7' C8' H8'B 108.7 . . ?
C9' C8' H8'A 108.7 . . ?
C9' C8' H8'B 108.7 . . ?
C9' C8' C7' 114.0(8) . . ?
C10 C11 H11C 108.9 . . ?
C10 C11 H11D 108.9 . . ?
C10 C11 C12 113.5(8) . . ?
H11C C11 H11D 107.7 . . ?
C12 C11 H11C 108.9 . . ?
C12 C11 H11D 108.9 . . ?
C6' C5' H5'A 109.6 . . ?
C6' C5' H5'B 109.6 . . ?
C6' C5' C4' 110.2(9) . . ?
H5'A C5' H5'B 108.1 . . ?
C4' C5' H5'A 109.6 . . ?
C4' C5' H5'B 109.6 . . ?
H2'C C2' H2'D 107.6 . . ?
C1' C2' H2'C 108.6 . . ?
C1' C2' H2'D 108.6 . . ?
C3' C2' H2'C 108.6 . . ?
C3' C2' H2'D 108.6 . . ?
C3' C2' C1' 114.5(8) . . ?
N1' C1' C2' 113.6(8) . . ?
N1' C1' H1'C 108.8 . . ?
N1' C1' H1'D 108.8 . . ?
C2' C1' H1'C 108.8 . . ?
C2' C1' H1'D 108.8 . . ?
H1'C C1' H1'D 107.7 . . ?
N1 C1 C2 113.5(8) . . ?
N1 C1 H1C 108.9 . . ?
N1 C1 H1D 108.9 . . ?
C2 C1 H1C 108.9 . . ?
C2 C1 H1D 108.9 . . ?
H1C C1 H1D 107.7 . . ?
C2 C3 H3C 108.6 . . ?
C2 C3 H3D 108.6 . . ?
H3C C3 H3D 107.5 . . ?
C3' C3 C2 114.9(8) . . ?
C3' C3 H3C 108.6 . . ?
C3' C3 H3D 108.6 . . ?
N3' C7' C8' 116.0(8) . . ?
N3' C7' H7'A 108.3 . . ?
N3' C7' H7'B 108.3 . . ?
C8' C7' H7'A 108.3 . . ?
C8' C7' H7'B 108.3 . . ?
H7'A C7' H7'B 107.4 . . ?
N2' C4' C5' 115.5(9) . . ?
N2' C4' H4'C 108.4 . . ?
N2' C4' H4'D 108.4 . . ?
C5' C4' H4'C 108.4 . . ?
C5' C4' H4'D 108.4 . . ?
H4'C C4' H4'D 107.5 . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C12 C12 C11 113.4(10) 2_756 . ?
C12 C12 H12A 108.9 2_756 . ?
C12 C12 H12B 108.9 2_756 . ?
H12A C12 H12B 107.7 . . ?
C11' C12' H12C 108.7 . . ?
C11' C12' H12D 108.7 . . ?
C12' C12' C11' 114.1(11) 2_585 . ?
C12' C12' H12C 108.7 2_585 . ?
C12' C12' H12D 108.7 2_585 . ?
H12C C12' H12D 107.6 . . ?
C5 C6 H6A 108.2 . . ?
C5 C6 H6B 108.2 . . ?
C6 C6 C5 116.4(11) 2_866 . ?
C6 C6 H6A 108.2 2_866 . ?
C6 C6 H6B 108.2 2_866 . ?
H6A C6 H6B 107.3 . . ?
C2' C3' H3'C 108.5 . . ?
C2' C3' H3'D 108.5 . . ?
C3 C3' C2' 115.1(8) . . ?
C3 C3' H3'C 108.5 . . ?
C3 C3' H3'D 108.5 . . ?
H3'C C3' H3'D 107.5 . . ?
C8 C9 C9 111.1(10) . 2_865 ?
C8 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
C9 C9 H9A 109.4 2_865 . ?
C9 C9 H9B 109.4 2_865 . ?
H9A C9 H9B 108.0 . . ?
N4' C10' C11' 114.0(8) . . ?
N4' C10' H10C 108.8 . . ?
N4' C10' H10D 108.8 . . ?
C11' C10' H10C 108.8 . . ?
C11' C10' H10D 108.8 . . ?
H10C C10' H10D 107.7 . . ?
C8' C9' C9' 113.7(11) . 2_476 ?
C8' C9' H9'A 108.8 . . ?
C8' C9' H9'B 108.8 . . ?
C9' C9' H9'A 108.8 2_476 . ?
C9' C9' H9'B 108.8 2_476 . ?
H9'A C9' H9'B 107.7 . . ?

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
Cd1 O4 N6 O5 -1.3(11) . . . . ?
Cd1 O4 N6 O6 -180.0(9) . . . . ?
Cd1 O1 N5 O3 -171.0(6) . . . . ?
Cd1 O1 N5 O2 7.8(10) . . . . ?
Cd1 N3 C7 C8 165.6(6) . . . . ?
Cd1 N4 C10 C11 170.8(6) . . . . ?
Cd1 N2 C4 C5 -176.9(6) . . . . ?
Cd1 N1 C1 C2 -173.8(7) . . . . ?
Cd1' O2' N5' O1' 4.6(8) . . . . ?
Cd1' O2' N5' O3' -177.1(8) . . . . ?
Cd1' O1' N5' O2' -4.7(9) . . . . ?
Cd1' O1' N5' O3' 176.9(8) . . . . ?
Cd1' N2' C4' C5' -177.6(7) . . . . ?
Cd1' N1' C1' C2' 173.5(7) . . . . ?
Cd1' N3' C7' C8' -177.9(7) . . . . ?
Cd1' N4' C10' C11' 161.9(7) . . . . ?
N3 C7 C8 C9 -177.9(8) . . . . ?
N4 C10 C11 C12 175.2(8) . . . . ?
N2 C4 C5 C6 -178.8(8) . . . . ?
C7 C8 C9 C9 -65.7(12) . . . 2_865 ?
C2 C3 C3' C2' -177.8(9) . . . . ?
C10 C11 C12 C12 55.9(14) . . . 2_756 ?
C4 C5 C6 C6 -63.2(15) . . . 2_866 ?
C6' C6' C5' C4' -169.0(10) 2_475 . . . ?
C6' C5' C4' N2' 177.1(8) . . . . ?
C1' C2' C3' C3 -64.0(13) . . . . ?
C1 C2 C3 C3' 61.4(13) . . . . ?
C3 C2 C1 N1 171.7(8) . . . . ?
C7' C8' C9' C9' -176.7(11) . . . 2_476 ?
C12' C11' C10' N4' -67.7(11) . . . . ?
C3' C2' C1' N1' -173.2(9) . . . . ?
C10' C11' C12' C12' 179.0(10) . . . 2_585 ?
C9' C8' C7' N3' -71.0(12) . . . . ?

_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 1.120
_oxdiff_exptl_absorpt_empirical_full_min 0.876
####################################################################### 
# 
# 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_1_2_GPa_Cd2_HDA_3_NO3_4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262361'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_2_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.350 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_2_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.27 Note
RESPONSE: The data/parameter ratio is affected by the access limits
 of the DAC.
;
_vrf_PLAT342_1_2_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02875 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_1_2_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        878 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C10 H10 N4 O4'
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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.276(14)
_cell_length_b                   6.7318(5)
_cell_length_c                   15.218(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.72(4)
_cell_angle_gamma                90
_cell_volume                     1452.5(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3637
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9000
_cell_measurement_theta_min      2.6790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.08
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.350
_diffrn_reflns_Laue_measured_fraction_max 0.327
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11532
_diffrn_reflns_point_group_measured_fraction_full 0.350
_diffrn_reflns_point_group_measured_fraction_max 0.327
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.667
_diffrn_reflns_theta_min         1.851
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.350
_diffrn_measured_fraction_theta_max 0.327
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.20(2) GPa
 (1200000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
 17  ω    -23.00   9.00   1.00   25.00    --    0.12 -13.00   3.00   32
 18  ω    -22.00  11.00   1.00   25.00    --   30.76  53.00 -17.00   33
 19  ω     89.00 114.00   1.00   25.00    --   30.76 134.00 -57.00   25
 20  ω     -9.00  19.00   1.00   25.00    --  -30.53 -81.00-151.00   28
 21  ω      7.00  33.00   1.00   25.00    --  -30.53-114.00-135.00   26
 22  ω     58.00  90.00   1.00   25.00    --    0.12-178.00-120.00   32
 23  ω    -21.00   5.00   1.00   25.00    --    0.12  82.00 153.00   26
 24  ω    -25.00   0.00   1.00   25.00    --   30.76  53.00 162.00   25
 25  ω    -68.00 -15.00   1.00   25.00    --  -30.53  82.00 153.00   53
 26  ω    -24.00  18.00   1.00   25.00    --   30.76   0.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0491566000
_diffrn_orient_matrix_UB_12      -0.0035675000
_diffrn_orient_matrix_UB_13      0.0132718000
_diffrn_orient_matrix_UB_21      -0.0026423000
_diffrn_orient_matrix_UB_22      0.0917109000
_diffrn_orient_matrix_UB_23      0.0226222000
_diffrn_orient_matrix_UB_31      -0.0082095000
_diffrn_orient_matrix_UB_32      -0.0520650000
_diffrn_orient_matrix_UB_33      0.0389524000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                699
_reflns_number_total             1001
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1001
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      0.996
_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)+(0.0870P)²+1.7272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1518
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C2-C1 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C8-C7 \\sim C9-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O1, Cd1, N1, N3, O4, N4, C1, C7, N5, O2, O3, C2, C8, O6, O5, C3, C9, C4, C5,
 C6, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), N3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C8(H8A,H8B),
 C7(H7A,H7B), C6(H6A,H6B), C1(H1C,H1D), C2(H2C,H2D), C4(H4A,H4B), C3(H3C,H3D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 0.57974(17) 0.32827(11) 0.34721(6) 0.078(2) Uani 1 1 d . . . . .
O2 O 0.7147(15) -0.2075(9) 0.2883(7) 0.101(11) Uani 1 1 d . . . . .
O6 O 0.4268(14) 0.7794(10) 0.4762(6) 0.094(12) Uani 1 1 d . . . . .
N4 N 0.667(2) -0.0576(13) 0.3020(9) 0.082(9) Uani 1 1 d . . . . .
O1 O 0.6804(17) 0.0352(11) 0.3714(7) 0.105(8) Uani 1 1 d . . . . .
N2 N -0.091(2) -0.0345(13) 0.2870(9) 0.084(11) Uani 1 1 d . . . . .
H2A H -0.099948 0.095573 0.279342 0.101 Uiso 1 1 calc R U . . .
H2B H -0.143347 -0.082434 0.306569 0.101 Uiso 1 1 calc R U . . .
N1 N 0.458(2) 0.1341(14) 0.3584(8) 0.086(7) Uani 1 1 d . . . . .
H1A H 0.480900 0.012772 0.370573 0.103 Uiso 1 1 calc R U . . .
H1B H 0.432127 0.174308 0.405681 0.103 Uiso 1 1 calc R U . . .
N5 N 0.4435(19) 0.6598(12) 0.4201(7) 0.065(7) Uani 1 1 d . . . . .
N3 N 0.699(2) 0.4916(12) 0.4291(9) 0.075(7) Uani 1 1 d . . . . .
H3A H 0.700660 0.614956 0.408379 0.089 Uiso 1 1 calc R U . . .
H3B H 0.684311 0.499978 0.484421 0.089 Uiso 1 1 calc R U . . .
O3 O 0.607(2) 0.0023(15) 0.2470(8) 0.114(9) Uani 1 1 d . . . . .
O4 O 0.514(2) 0.6791(14) 0.3797(10) 0.110(5) Uani 1 1 d . U . . .
C5 C 0.0712(16) 0.0523(14) 0.3367(9) 0.073(11) Uani 1 1 d D . . . .
H5A H 0.083951 0.028266 0.276407 0.088 Uiso 1 1 calc R U . . .
H5B H 0.059457 0.193325 0.342719 0.088 Uiso 1 1 calc R U . . .
C9 C 0.9622(19) 0.4458(16) 0.4734(8) 0.075(9) Uani 1 1 d D . . . .
H9A H 0.964554 0.307126 0.490841 0.090 Uiso 1 1 calc R U . . .
H9B H 0.972425 0.452542 0.411549 0.090 Uiso 1 1 calc R U . . .
C8 C 0.8656(16) 0.5281(15) 0.4838(9) 0.072(9) Uani 1 1 d D . . . .
H8A H 0.862234 0.665156 0.463923 0.086 Uiso 1 1 calc R U . . .
H8B H 0.856278 0.526479 0.545895 0.086 Uiso 1 1 calc R U . . .
C7 C 0.787(2) 0.410(2) 0.4315(9) 0.076(8) Uani 1 1 d D . . . .
H7A H 0.802259 0.395879 0.371247 0.091 Uiso 1 1 calc R U . . .
H7B H 0.786211 0.277957 0.456817 0.091 Uiso 1 1 calc R U . . .
C6 C -0.016(2) -0.0622(16) 0.3538(10) 0.078(11) Uani 1 1 d D . . . .
H6A H -0.001145 -0.202534 0.358318 0.094 Uiso 1 1 calc R U . . .
H6B H -0.035597 -0.019986 0.409864 0.094 Uiso 1 1 calc R U . . .
O5 O 0.3952(16) 0.5217(13) 0.4032(7) 0.116(8) Uani 1 1 d . . . . .
C1 C 0.3815(18) 0.1137(15) 0.2857(9) 0.071(8) Uani 1 1 d D . . . .
H1C H 0.406397 0.045134 0.237363 0.086 Uiso 1 1 calc R U . . .
H1D H 0.363277 0.245855 0.264804 0.086 Uiso 1 1 calc R U . . .
C2 C 0.2932(16) 0.0054(12) 0.3055(8) 0.071(8) Uani 1 1 d D . . . .
H2C H 0.308754 -0.132817 0.317949 0.085 Uiso 1 1 calc R U . . .
H2D H 0.247134 0.009490 0.253373 0.085 Uiso 1 1 calc R U . . .
C4 C 0.1570(16) -0.0051(15) 0.3995(8) 0.076(10) Uani 1 1 d D . . . .
H4A H 0.165135 -0.147842 0.396049 0.091 Uiso 1 1 calc R U . . .
H4B H 0.144451 0.025700 0.459246 0.091 Uiso 1 1 calc R U . . .
C3 C 0.2491(17) 0.0933(16) 0.3838(8) 0.079(10) Uani 1 1 d D . . . .
H3C H 0.293537 0.080112 0.436817 0.095 Uiso 1 1 calc R U . . .
H3D H 0.238007 0.233931 0.373332 0.095 Uiso 1 1 calc R U . . .


_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
Cd1 O1 2.443(16) . ?
Cd1 N2 2.266(10) 2 ?
Cd1 N1 2.19(2) . ?
Cd1 N3 2.27(3) . ?
Cd1 O4 2.610(13) . ?
O2 N4 1.249(19) . ?
O6 N5 1.217(11) . ?
N4 O1 1.223(17) . ?
N4 O3 1.20(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C6 1.40(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.47(3) . ?
N5 O4 1.25(3) . ?
N5 O5 1.17(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.38(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.515(16) . ?
C5 C4 1.513(15) . ?
C9 C9 1.47(4) 3_766 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.512(17) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.518(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.516(16) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.531(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.516(15) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?

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 Cd1 O4 156.9(7) . . ?
N2 Cd1 O1 111.2(5) 2 . ?
N2 Cd1 N3 99.7(7) 2 . ?
N2 Cd1 O4 82.4(4) 2 . ?
N1 Cd1 O1 87.9(7) . . ?
N1 Cd1 N2 117.1(9) . 2 ?
N1 Cd1 N3 142.5(5) . . ?
N1 Cd1 O4 102.7(7) . . ?
N3 Cd1 O1 85.4(6) . . ?
N3 Cd1 O4 73.7(9) . . ?
O1 N4 O2 122(2) . . ?
O3 N4 O2 121.1(14) . . ?
O3 N4 O1 117.3(17) . . ?
N4 O1 Cd1 104.6(15) . . ?
Cd1 N2 H2A 107.8 2_545 . ?
Cd1 N2 H2B 107.8 2_545 . ?
H2A N2 H2B 107.2 . . ?
C6 N2 Cd1 117.9(15) . 2_545 ?
C6 N2 H2A 107.8 . . ?
C6 N2 H2B 107.8 . . ?
Cd1 N1 H1A 106.9 . . ?
Cd1 N1 H1B 106.9 . . ?
H1A N1 H1B 106.7 . . ?
C1 N1 Cd1 121.6(7) . . ?
C1 N1 H1A 106.9 . . ?
C1 N1 H1B 106.9 . . ?
O6 N5 O4 120.8(18) . . ?
O5 N5 O6 121.5(19) . . ?
O5 N5 O4 117.7(12) . . ?
Cd1 N3 H3A 108.1 . . ?
Cd1 N3 H3B 108.1 . . ?
H3A N3 H3B 107.3 . . ?
C7 N3 Cd1 116.6(8) . . ?
C7 N3 H3A 108.1 . . ?
C7 N3 H3B 108.1 . . ?
N5 O4 Cd1 109.2(8) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C4 C5 C6 112.6(10) . . ?
C9 C9 H9A 109.1 3_766 . ?
C9 C9 H9B 109.1 3_766 . ?
C9 C9 C8 112.4(15) 3_766 . ?
H9A C9 H9B 107.9 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C9 C8 C7 112.2(11) . . ?
H8A C8 H8B 107.9 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
N3 C7 C8 115.0(12) . . ?
N3 C7 H7A 108.5 . . ?
N3 C7 H7B 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
N2 C6 C5 112.7(13) . . ?
N2 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N1 C1 H1C 108.0 . . ?
N1 C1 H1D 108.0 . . ?
N1 C1 C2 117.3(11) . . ?
H1C C1 H1D 107.2 . . ?
C2 C1 H1C 108.0 . . ?
C2 C1 H1D 108.0 . . ?
C1 C2 H2C 108.9 . . ?
C1 C2 H2D 108.9 . . ?
C1 C2 C3 113.3(11) . . ?
H2C C2 H2D 107.7 . . ?
C3 C2 H2C 108.9 . . ?
C3 C2 H2D 108.9 . . ?
C5 C4 H4A 108.2 . . ?
C5 C4 H4B 108.2 . . ?
C5 C4 C3 116.3(9) . . ?
H4A C4 H4B 107.4 . . ?
C3 C4 H4A 108.2 . . ?
C3 C4 H4B 108.2 . . ?
C2 C3 H3C 108.9 . . ?
C2 C3 H3D 108.9 . . ?
C4 C3 C2 113.4(12) . . ?
C4 C3 H3C 108.9 . . ?
C4 C3 H3D 108.9 . . ?
H3C C3 H3D 107.7 . . ?

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
Cd1 N2 C6 C5 70.2(11) 2_545 . . . ?
Cd1 N1 C1 C2 -169.5(8) . . . . ?
Cd1 N3 C7 C8 177.5(7) . . . . ?
O2 N4 O1 Cd1 172.8(13) . . . . ?
O6 N5 O4 Cd1 145.4(14) . . . . ?
N1 C1 C2 C3 55.2(16) . . . . ?
O3 N4 O1 Cd1 -6(2) . . . . ?
C5 C4 C3 C2 -76.5(14) . . . . ?
C9 C9 C8 C7 -177.6(11) 3_766 . . . ?
C9 C8 C7 N3 -172.2(10) . . . . ?
C6 C5 C4 C3 176.5(8) . . . . ?
O5 N5 O4 Cd1 -33(2) . . . . ?
C1 C2 C3 C4 175.7(11) . . . . ?
C4 C5 C6 N2 -169.8(11) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999925 0.00000000 0.00122348
omega rotation goniometer -1 . -0.88992000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -2.28590000 -0.76675894 0.00000000
0.64193514
phi rotation goniometer -1 kappa . 0.00018850 0.00000000 0.99999998
theta rotation goniometer -1 . -0.75634000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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_0_0001_GPa_Cd2_HDA_3_NO3_4
_database_code_depnum_ccdc_archive 'CCDC 2262359'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.3304(4)
_cell_length_b                   7.0034(2)
_cell_length_c                   16.3600(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.033(3)
_cell_angle_gamma                90
_cell_volume                     1629.56(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9480
_cell_measurement_theta_min      2.8630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.193
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         2.864
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  41.00   1.00    6.29    --   16.56 -69.00-147.00   93
  2  ω     -8.00  83.00   1.00    6.29    --   16.56  69.00 -15.00   91
  3  ω      6.00  57.00   1.00    6.29    --   16.56 -99.00  90.00   51
  4  ω      1.00  30.00   1.00    6.29    --   16.56  77.00  90.00   29
  5  ω     -2.00  58.00   1.00    6.29    --   16.56 -99.00 150.00   60
  6  ω    -39.00   9.00   1.00    6.29    --  -17.42 -77.00  90.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0445667000
_diffrn_orient_matrix_UB_12      -0.0120823000
_diffrn_orient_matrix_UB_13      0.0235330000
_diffrn_orient_matrix_UB_21      0.0177305000
_diffrn_orient_matrix_UB_22      0.0786366000
_diffrn_orient_matrix_UB_23      -0.0206787000
_diffrn_orient_matrix_UB_31      -0.0136021000
_diffrn_orient_matrix_UB_32      0.0627080000
_diffrn_orient_matrix_UB_33      0.0304552000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2780
_reflns_number_total             3524
_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       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3524
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.036
_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)+(0.0328P)²+2.6627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0885
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O4, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), N3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C8(H8A,H8B),
 C7(H7A,H7B), C6(H6A,H6B), C1(H1C,H1D), C2(H2C,H2D), C4(H4A,H4B), C3(H3C,H3D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 0.57798(2) 0.30838(4) 0.34967(2) 0.04447(11) Uani 1 1 d . . . . .
O2 O 0.7072(2) -0.2146(4) 0.2938(2) 0.0601(8) Uani 1 1 d . . . . .
O6 O 0.4356(3) 0.7656(5) 0.4727(2) 0.0737(10) Uani 1 1 d . . . . .
N4 N 0.6614(2) -0.0658(5) 0.3034(2) 0.0483(8) Uani 1 1 d . . . . .
O1 O 0.6813(2) 0.0327(5) 0.3654(3) 0.0827(12) Uani 1 1 d . . . . .
N2 N -0.0934(2) -0.0597(5) 0.2750(2) 0.0472(8) Uani 1 1 d . . . . .
H2A H -0.104205 0.064423 0.266726 0.057 Uiso 1 1 calc R U . . .
H2B H -0.145125 -0.108865 0.291727 0.057 Uiso 1 1 calc R U . . .
N1 N 0.4530(2) 0.1346(5) 0.3674(2) 0.0497(8) Uani 1 1 d . . . . .
H1A H 0.473026 0.018704 0.383473 0.060 Uiso 1 1 calc R U . . .
H1B H 0.426632 0.185830 0.408730 0.060 Uiso 1 1 calc R U . . .
N5 N 0.4454(3) 0.6422(5) 0.4224(2) 0.0530(9) Uani 1 1 d . . . . .
N3 N 0.6940(2) 0.4677(5) 0.4234(2) 0.0441(8) Uani 1 1 d . . . . .
H3A H 0.693387 0.586666 0.404255 0.053 Uiso 1 1 calc R U . . .
H3B H 0.680405 0.474080 0.475020 0.053 Uiso 1 1 calc R U . . .
O3 O 0.5971(3) -0.0137(6) 0.2513(2) 0.0787(11) Uani 1 1 d . . . . .
O4 O 0.5059(3) 0.6410(7) 0.3779(3) 0.0986(13) Uani 1 1 d . U . . .
C5 C 0.0692(2) 0.0366(5) 0.3299(3) 0.0436(9) Uani 1 1 d . . . . .
H5A H 0.087534 0.003759 0.276552 0.052 Uiso 1 1 calc R U . . .
H5B H 0.054277 0.171755 0.329463 0.052 Uiso 1 1 calc R U . . .
C9 C 0.9630(2) 0.4427(6) 0.4732(2) 0.0422(9) Uani 1 1 d . . . . .
H9A H 0.966423 0.310386 0.490800 0.051 Uiso 1 1 calc R U . . .
H9B H 0.976653 0.447125 0.416580 0.051 Uiso 1 1 calc R U . . .
C8 C 0.8634(2) 0.5162(6) 0.4767(3) 0.0456(9) Uani 1 1 d . . . . .
H8A H 0.850500 0.517254 0.533566 0.055 Uiso 1 1 calc R U . . .
H8B H 0.858898 0.646537 0.456533 0.055 Uiso 1 1 calc R U . . .
C7 C 0.7903(2) 0.3949(6) 0.4261(3) 0.0437(9) Uani 1 1 d . . . . .
H7A H 0.806218 0.386841 0.370211 0.052 Uiso 1 1 calc R U . . .
H7B H 0.792662 0.266667 0.448615 0.052 Uiso 1 1 calc R U . . .
C6 C -0.0175(3) -0.0772(6) 0.3441(3) 0.0460(9) Uani 1 1 d . . . . .
H6A H -0.000521 -0.210641 0.351599 0.055 Uiso 1 1 calc R U . . .
H6B H -0.040350 -0.032829 0.394172 0.055 Uiso 1 1 calc R U . . .
O5 O 0.3808(4) 0.5162(6) 0.4117(3) 0.1104(16) Uani 1 1 d . . . . .
C1 C 0.3795(3) 0.1115(6) 0.2976(3) 0.0493(10) Uani 1 1 d . . . . .
H1C H 0.405920 0.043148 0.254288 0.059 Uiso 1 1 calc R U . . .
H1D H 0.361114 0.237122 0.276448 0.059 Uiso 1 1 calc R U . . .
C2 C 0.2915(3) 0.0063(6) 0.3163(3) 0.0474(10) Uani 1 1 d . . . . .
H2C H 0.247692 -0.000374 0.266299 0.057 Uiso 1 1 calc R U . . .
H2D H 0.308674 -0.123388 0.332616 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1506(3) -0.0024(7) 0.3961(3) 0.0542(11) Uani 1 1 d . . . . .
H4A H 0.161616 -0.138984 0.398940 0.065 Uiso 1 1 calc R U . . .
H4B H 0.132628 0.037533 0.448797 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2424(3) 0.0971(7) 0.3832(3) 0.0528(11) Uani 1 1 d . . . . .
H3C H 0.229223 0.229745 0.369060 0.063 Uiso 1 1 calc R U . . .
H3D H 0.284257 0.094648 0.434464 0.063 Uiso 1 1 calc R U . . .


_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
Cd1 O1 2.427(3) . ?
Cd1 N2 2.274(3) 2 ?
Cd1 N1 2.213(3) . ?
Cd1 N3 2.230(3) . ?
Cd1 O4 2.612(4) . ?
O2 N4 1.252(4) . ?
O6 N5 1.213(5) . ?
N4 O1 1.231(5) . ?
N4 O3 1.232(5) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C6 1.475(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.465(5) . ?
N5 O4 1.199(5) . ?
N5 O5 1.275(5) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.467(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.517(5) . ?
C5 C4 1.516(5) . ?
C9 C9 1.521(7) 3_766 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.524(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.515(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.523(5) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.512(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.526(5) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?

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 Cd1 O4 160.01(13) . . ?
N2 Cd1 O1 107.03(13) 2 . ?
N2 Cd1 O4 83.11(13) 2 . ?
N1 Cd1 O1 92.39(13) . . ?
N1 Cd1 N2 120.67(12) . 2 ?
N1 Cd1 N3 139.97(13) . . ?
N1 Cd1 O4 97.11(14) . . ?
N3 Cd1 O1 86.33(11) . . ?
N3 Cd1 N2 97.69(12) . 2 ?
N3 Cd1 O4 75.08(13) . . ?
O1 N4 O2 119.9(4) . . ?
O1 N4 O3 118.9(4) . . ?
O3 N4 O2 121.3(4) . . ?
N4 O1 Cd1 106.4(3) . . ?
Cd1 N2 H2A 107.2 2_545 . ?
Cd1 N2 H2B 107.2 2_545 . ?
H2A N2 H2B 106.8 . . ?
C6 N2 Cd1 120.6(2) . 2_545 ?
C6 N2 H2A 107.2 . . ?
C6 N2 H2B 107.2 . . ?
Cd1 N1 H1A 107.7 . . ?
Cd1 N1 H1B 107.7 . . ?
H1A N1 H1B 107.1 . . ?
C1 N1 Cd1 118.4(3) . . ?
C1 N1 H1A 107.7 . . ?
C1 N1 H1B 107.7 . . ?
O6 N5 O5 116.3(4) . . ?
O4 N5 O6 124.7(5) . . ?
O4 N5 O5 118.7(4) . . ?
Cd1 N3 H3A 107.7 . . ?
Cd1 N3 H3B 107.7 . . ?
H3A N3 H3B 107.1 . . ?
C7 N3 Cd1 118.6(2) . . ?
C7 N3 H3A 107.7 . . ?
C7 N3 H3B 107.7 . . ?
N5 O4 Cd1 116.4(4) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C4 C5 C6 111.7(3) . . ?
C9 C9 H9A 109.0 3_766 . ?
C9 C9 H9B 109.0 3_766 . ?
C9 C9 C8 112.9(4) 3_766 . ?
H9A C9 H9B 107.8 . . ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C7 C8 C9 112.2(3) . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
N3 C7 C8 114.0(3) . . ?
N3 C7 H7A 108.8 . . ?
N3 C7 H7B 108.8 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N2 C6 C5 112.3(3) . . ?
N2 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N1 C1 H1C 108.4 . . ?
N1 C1 H1D 108.4 . . ?
N1 C1 C2 115.5(4) . . ?
H1C C1 H1D 107.5 . . ?
C2 C1 H1C 108.4 . . ?
C2 C1 H1D 108.4 . . ?
C1 C2 H2C 108.7 . . ?
C1 C2 H2D 108.7 . . ?
H2C C2 H2D 107.6 . . ?
C3 C2 C1 114.4(3) . . ?
C3 C2 H2C 108.7 . . ?
C3 C2 H2D 108.7 . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
C5 C4 C3 114.8(4) . . ?
H4A C4 H4B 107.5 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C2 C3 C4 113.2(3) . . ?
C2 C3 H3C 108.9 . . ?
C2 C3 H3D 108.9 . . ?
C4 C3 H3C 108.9 . . ?
C4 C3 H3D 108.9 . . ?
H3C C3 H3D 107.7 . . ?

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
Cd1 N2 C6 C5 68.7(4) 2_545 . . . ?
Cd1 N1 C1 C2 -174.4(3) . . . . ?
Cd1 N3 C7 C8 179.0(3) . . . . ?
O2 N4 O1 Cd1 177.1(3) . . . . ?
O6 N5 O4 Cd1 142.3(4) . . . . ?
N1 C1 C2 C3 58.2(5) . . . . ?
O3 N4 O1 Cd1 -1.8(5) . . . . ?
C5 C4 C3 C2 -74.7(5) . . . . ?
C9 C9 C8 C7 -177.4(4) 3_766 . . . ?
C9 C8 C7 N3 -176.3(3) . . . . ?
C6 C5 C4 C3 176.2(4) . . . . ?
O5 N5 O4 Cd1 -44.7(5) . . . . ?
C1 C2 C3 C4 175.6(4) . . . . ?
C4 C5 C6 N2 -172.8(3) . . . . ?

_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 1.162
_oxdiff_exptl_absorpt_empirical_full_min 0.929
####################################################################### 
# 
# 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_3_1_GPa_Cd2_HDA_3_NO3_4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262363'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.329 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT090_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.49 Note
RESPONSE: The data/parameter ratio is affected by the access limits of
 the DAC.
;
_vrf_PLAT342_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.10333 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT780_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !
RESPONSE: Coordinates Form a Properly Connected Set in the Unit Cell 
after symmetry operation. 
;
_vrf_PLAT911_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        757 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT915_3_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         30 %
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd N4 O4 C10 H10'
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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.188(11)
_cell_length_b                   6.5088(3)
_cell_length_c                   14.7051(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.70(3)
_cell_angle_gamma                90
_cell_volume                     1351.2(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5017
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1190
_cell_measurement_theta_min      2.7700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.08
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.329
_diffrn_reflns_Laue_measured_fraction_max 0.303
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10939
_diffrn_reflns_point_group_measured_fraction_full 0.333
_diffrn_reflns_point_group_measured_fraction_max 0.302
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.660
_diffrn_reflns_theta_min         2.784
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.329
_diffrn_measured_fraction_theta_max 0.303
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 3.10(2) GPa
 (3100000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
 17  ω    -23.00   9.00   1.00   25.00    --    0.12 -13.00   3.00   32
 18  ω    -22.00  11.00   1.00   25.00    --   30.76  53.00 -17.00   33
 19  ω     89.00 114.00   1.00   25.00    --   30.76 134.00 -57.00   25
 20  ω     -9.00  19.00   1.00   25.00    --  -30.53 -81.00-151.00   28
 21  ω      7.00  33.00   1.00   25.00    --  -30.53-114.00-135.00   26
 22  ω     58.00  90.00   1.00   25.00    --    0.12-178.00-120.00   32
 23  ω    -21.00   5.00   1.00   25.00    --    0.12  82.00 153.00   26
 24  ω    -25.00   0.00   1.00   25.00    --   30.76  53.00 162.00   25
 25  ω    -68.00 -15.00   1.00   25.00    --  -30.53  82.00 153.00   53
 26  ω    -24.00  18.00   1.00   25.00    --   30.76   0.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0497199000
_diffrn_orient_matrix_UB_12      0.0014518000
_diffrn_orient_matrix_UB_13      -0.0113566000
_diffrn_orient_matrix_UB_21      0.0040225000
_diffrn_orient_matrix_UB_22      0.0935935000
_diffrn_orient_matrix_UB_23      -0.0240923000
_diffrn_orient_matrix_UB_31      0.0055109000
_diffrn_orient_matrix_UB_32      -0.0560066000
_diffrn_orient_matrix_UB_33      -0.0405158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.337
_reflns_Friedel_fraction_max     0.300
_reflns_number_gt                1412
_reflns_number_total             1726
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.226
_refine_ls_abs_structure_details 
;
 Flack x determined using 560 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     716
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      0.967
_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)+(0.1901P)²+4.9460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2495
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C7'-N3'
 1.42 with sigma of 0.02
 N3-C7
 1.42 with sigma of 0.02
 C6'-C5' \\sim C4'-C5' \\sim C3'-C4' \\sim C1'-C2' \\sim C7'-C8' \\sim C8'-C9'
\\sim C9-C9' \\sim C8-C9 ~
 C8-C7 \\sim C2'-C3' \\sim C5-C6 \\sim C2-C3 \\sim C2-C1 \\sim C4-C3
 with sigma of 0.02
 O2'-N4' \\sim O1'-N4' \\sim O3'-N4' \\sim O6'-N5' \\sim O4'-N5' \\sim O5'-N5'
\\sim O3-N4 \\sim O1-N4 ~
 O2-N4 \\sim O5-N5 \\sim O4-N5 \\sim O6-N5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cd1' \\sim Cd1 \\sim N1 \\sim O4 \\sim O3 \\sim N2 \\sim O1 \\sim N3 \\sim C1
\\sim N5 \\sim N4 \\sim C6 \\sim C7 \\sim C2 \\sim O6 \\sim O5 \\sim O2 \\sim
C5 \\sim C8 \\sim C3 \\sim C9 \\sim C4 \\sim C9' \\sim C8' \\sim C7' \\sim N3'
\\sim O4' \\sim O1' \\sim N2' \\sim N1' \\sim N5' \\sim N4' \\sim C1' \\sim O6'
\\sim O5' \\sim O3' \\sim O2' \\sim C2' \\sim C3' \\sim C4' \\sim C5' \\sim
C6': within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C5') \\sim Ueq, Uanis(C6') \\sim Ueq, Uanis(N2') \\sim Ueq, Uanis(N3')
\\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq: with sigma of 0.03 and
sigma for terminal atoms of 0.06
Uanis(C7') \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C6') \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N5') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cd1, N1, O4, O3, N2, O1, N3, C1, N5, N4, C6, C7, C2, O6, O5, O2, C5, C8, C3,
 C9, C4, C9', C8', C7', N3', Cd1', O4', O1', N2', N1', N5', N4', C1', O6', O5',
 O3', O2', C2', C3', C4', C5', C6'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N3'(H3'A,H3'B), C5'(H5'A,H5'B), C4'(H4'A,H4'B), C1(H1A,H1B), C9'(H9'A,H9'B),
 C3(H3A,H3B), N1(H1C,H1D), C7(H7A,H7B), C2(H2A,H2B), N2(H2C,H2D), C6'(H6'A,
 H6'B), C6(H6A,H6B), N2'(H2'A,H2'B), C3'(H3'C,H3'D), N1'(H1'A,H1'B), N3(H3C,
 H3D), C9(H9A,H9B), C5(H5A,H5B), C8(H8A,H8B), C4(H4A,H4B), C1'(H1'C,H1'D),
 C2'(H2'C,H2'D), C7'(H7'A,H7'B), C8'(H8'A,H8'B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 0.3382(7) 0.0763(4) 0.0801(3) 0.095(6) Uani 1 1 d . . . . .
Cd1' Cd 1.1730(7) 0.4060(4) 0.3930(3) 0.098(6) Uani 1 1 d . U . . .
O2 O 0.477(5) -0.468(4) 0.020(2) 0.09(2) Uani 1 1 d D U . . .
N5' N 1.316(4) 0.079(5) 0.322(2) 0.035(8) Uani 1 1 d D U . . .
O6 O 0.182(7) 0.526(4) 0.218(2) 0.068(19) Uani 1 1 d D U . . .
O3' O 1.149(5) 0.740(8) 0.497(2) 0.10(2) Uani 1 1 d D U . . .
N3' N 1.034(7) 0.248(6) 0.306(2) 0.043(8) Uani 1 1 d D U . . .
H3'A H 1.040718 0.267564 0.247118 0.052 Uiso 1 1 calc R U . . .
H3'B H 1.038652 0.112730 0.315748 0.052 Uiso 1 1 calc R U . . .
O5 O 0.135(5) 0.277(5) 0.136(2) 0.059(11) Uani 1 1 d D U . . .
C5' C 1.663(6) 0.678(6) 0.411(3) 0.031(8) Uani 1 1 d D U . . .
H5'A H 1.672519 0.532826 0.399305 0.037 Uiso 1 1 calc R U . . .
H5'B H 1.647497 0.690765 0.473438 0.037 Uiso 1 1 calc R U . . .
C4' C 1.580(6) 0.750(6) 0.349(3) 0.040(8) Uani 1 1 d D U . . .
H4'A H 1.593185 0.726993 0.286238 0.049 Uiso 1 1 calc R U . . .
H4'B H 1.572598 0.896168 0.357491 0.049 Uiso 1 1 calc R U . . .
O6' O 1.345(6) -0.038(4) 0.265(2) 0.038(12) Uani 1 1 d D U . . .
C1 C 0.120(6) -0.154(5) 0.017(3) 0.067(17) Uani 1 1 d D U . . .
H1A H 0.102619 -0.019996 -0.007539 0.080 Uiso 1 1 calc R U . . .
H1B H 0.140472 -0.234939 -0.032893 0.080 Uiso 1 1 calc R U . . .
N4' N 1.088(4) 0.804(5) 0.440(2) 0.074(17) Uani 1 1 d D U . . .
O2' O 1.041(5) 0.955(4) 0.456(2) 0.09(2) Uani 1 1 d D U . . .
C9' C 0.768(6) 0.279(6) 0.283(3) 0.036(8) Uani 1 1 d D U . . .
H9'A H 0.761376 0.256314 0.347449 0.044 Uiso 1 1 calc R U . . .
H9'B H 0.764215 0.426065 0.272384 0.044 Uiso 1 1 calc R U . . .
C3 C 0.019(7) -0.162(6) 0.135(3) 0.065(19) Uani 1 1 d D U . . .
H3A H 0.072202 -0.194073 0.179448 0.078 Uiso 1 1 calc R U . . .
H3B H 0.011421 -0.014126 0.131428 0.078 Uiso 1 1 calc R U . . .
N1 N 0.221(8) -0.120(6) 0.098(3) 0.074(16) Uani 1 1 d . U . . .
H1C H 0.245275 -0.244347 0.108508 0.089 Uiso 1 1 calc R U . . .
H1D H 0.198720 -0.079322 0.149251 0.089 Uiso 1 1 calc R U . . .
O4' O 1.245(5) 0.055(6) 0.361(3) 0.061(10) Uani 1 1 d D U . . .
C7 C 0.522(5) 0.129(4) 0.192(2) 0.029(8) Uani 1 1 d D U . . .
H7A H 0.545926 0.070646 0.138313 0.034 Uiso 1 1 calc R U . . .
H7B H 0.504478 0.016678 0.230738 0.034 Uiso 1 1 calc R U . . .
O4 O 0.253(5) 0.407(6) 0.101(2) 0.056(8) Uani 1 1 d D U . . .
N4 N 0.431(4) -0.322(4) 0.0436(19) 0.076(19) Uani 1 1 d D U . . .
O1' O 1.073(6) 0.719(5) 0.365(2) 0.085(14) Uani 1 1 d D U . . .
C2 C 0.033(6) -0.251(6) 0.044(2) 0.062(17) Uani 1 1 d D U . . .
H2A H 0.039681 -0.399238 0.047902 0.074 Uiso 1 1 calc R U . . .
H2B H -0.020971 -0.219353 -0.000077 0.074 Uiso 1 1 calc R U . . .
O3 O 0.373(5) -0.248(5) -0.014(2) 0.09(2) Uani 1 1 d D U . . .
N2 N 0.331(7) 0.223(6) -0.061(3) 0.040(10) Uani 1 1 d . U . . .
H2C H 0.335478 0.358936 -0.054015 0.048 Uiso 1 1 calc R U . . .
H2D H 0.381577 0.182609 -0.087887 0.048 Uiso 1 1 calc R U . . .
C6' C 1.753(7) 0.789(5) 0.402(3) 0.037(9) Uani 1 1 d D U . . .
H6'A H 1.738762 0.934388 0.404601 0.044 Uiso 1 1 calc R U . . .
H6'B H 1.769414 0.762512 0.340285 0.044 Uiso 1 1 calc R U . . .
C6 C 0.240(7) 0.175(6) -0.127(3) 0.033(11) Uani 1 1 d D U . . .
H6A H 0.251575 0.209633 -0.189373 0.040 Uiso 1 1 calc R U . . .
H6B H 0.226597 0.028896 -0.125366 0.040 Uiso 1 1 calc R U . . .
N2' N 1.145(9) 0.249(8) 0.526(3) 0.066(18) Uani 1 1 d . U . . .
H2'A H 1.094675 0.305441 0.548496 0.079 Uiso 1 1 calc R U . . .
H2'B H 1.133747 0.115903 0.516862 0.079 Uiso 1 1 calc R U . . .
C3' C 1.491(6) 0.644(5) 0.365(3) 0.044(9) Uani 1 1 d D U . . .
H3'C H 1.502255 0.498447 0.376527 0.053 Uiso 1 1 calc R U . . .
H3'D H 1.444709 0.657425 0.312163 0.053 Uiso 1 1 calc R U . . .
N1' N 1.266(8) 0.619(5) 0.379(3) 0.069(10) Uani 1 1 d . U . . .
H1'A H 1.288791 0.600552 0.325295 0.083 Uiso 1 1 calc R U . . .
H1'B H 1.236139 0.739625 0.376355 0.083 Uiso 1 1 calc R U . . .
O1 O 0.447(6) -0.235(4) 0.1189(19) 0.078(18) Uani 1 1 d D U . . .
N3 N 0.442(6) 0.251(5) 0.166(3) 0.042(8) Uani 1 1 d D U . . .
H3C H 0.458802 0.360912 0.135919 0.051 Uiso 1 1 calc R U . . .
H3D H 0.416061 0.293360 0.215671 0.051 Uiso 1 1 calc R U . . .
N5 N 0.194(5) 0.412(5) 0.155(2) 0.050(8) Uani 1 1 d D U . . .
C9 C 0.689(6) 0.179(6) 0.229(3) 0.035(8) Uani 1 1 d D U . . .
H9A H 0.690179 0.033278 0.242926 0.042 Uiso 1 1 calc R U . . .
H9B H 0.698366 0.192558 0.164435 0.042 Uiso 1 1 calc R U . . .
C5 C 0.157(8) 0.291(6) -0.102(3) 0.034(11) Uani 1 1 d D U . . .
H5A H 0.168976 0.437366 -0.107279 0.041 Uiso 1 1 calc R U . . .
H5B H 0.147680 0.262877 -0.038713 0.041 Uiso 1 1 calc R U . . .
O5' O 1.368(5) 0.222(4) 0.342(2) 0.047(12) Uani 1 1 d D U . . .
C8 C 0.594(6) 0.259(6) 0.242(3) 0.039(9) Uani 1 1 d D U . . .
H8A H 0.588128 0.399232 0.219837 0.047 Uiso 1 1 calc R U . . .
H8B H 0.585467 0.259313 0.306691 0.047 Uiso 1 1 calc R U . . .
C4 C -0.069(7) -0.261(7) 0.160(3) 0.07(2) Uani 1 1 d D U . . .
H4A H -0.077169 -0.223954 0.222918 0.080 Uiso 1 1 calc R U . . .
H4B H -0.060112 -0.408886 0.158674 0.080 Uiso 1 1 calc R U . . .
C1' C 1.366(6) 0.638(4) 0.466(3) 0.051(10) Uani 1 1 d D U . . .
H1'C H 1.343901 0.706057 0.518705 0.061 Uiso 1 1 calc R U . . .
H1'D H 1.383204 0.498686 0.485391 0.061 Uiso 1 1 calc R U . . .
C2' C 1.454(6) 0.742(5) 0.447(3) 0.049(10) Uani 1 1 d D U . . .
H2'C H 1.501449 0.731256 0.498885 0.059 Uiso 1 1 calc R U . . .
H2'D H 1.441960 0.886459 0.434427 0.059 Uiso 1 1 calc R U . . .
C7' C 0.942(6) 0.306(5) 0.320(3) 0.031(8) Uani 1 1 d D U . . .
H7'A H 0.936485 0.453386 0.311030 0.038 Uiso 1 1 calc R U . . .
H7'B H 0.933175 0.280124 0.384072 0.038 Uiso 1 1 calc R U . . .
C8' C 0.863(6) 0.207(5) 0.264(3) 0.034(8) Uani 1 1 d D U . . .
H8'A H 0.866796 0.060152 0.273698 0.041 Uiso 1 1 calc R U . . .
H8'B H 0.870595 0.233069 0.200116 0.041 Uiso 1 1 calc R U . . .


_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
Cd1 N1 2.13(8) . ?
Cd1 O4 2.50(5) . ?
Cd1 O3 2.60(3) . ?
Cd1 N2 2.28(4) . ?
Cd1 O1 2.58(6) . ?
Cd1 N3 2.16(7) . ?
Cd1' N3' 2.46(8) . ?
Cd1' O4' 2.57(4) . ?
Cd1' O1' 2.50(6) . ?
Cd1' N2' 2.27(4) . ?
Cd1' N1' 1.94(8) . ?
O2 N4 1.22(3) . ?
N5' O6' 1.23(3) . ?
N5' O4' 1.22(3) . ?
N5' O5' 1.21(3) . ?
O6 N5 1.21(2) . ?
O3' N4' 1.21(3) . ?
N3' H3'A 0.8900 . ?
N3' H3'B 0.8900 . ?
N3' C7' 1.41(3) . ?
O5 N5 1.22(3) . ?
C5' H5'A 0.9700 . ?
C5' H5'B 0.9700 . ?
C5' C4' 1.48(3) . ?
C5' C6' 1.49(3) . ?
C4' H4'A 0.9700 . ?
C4' H4'B 0.9700 . ?
C4' C3' 1.49(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 N1 1.78(13) . ?
C1 C2 1.48(3) . ?
N4' O2' 1.23(3) . ?
N4' O1' 1.23(3) . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C9' C9 1.47(3) . ?
C9' C8' 1.48(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.49(3) . ?
C3 C4 1.48(3) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N3 1.41(3) . ?
C7 C8 1.47(3) . ?
O4 N5 1.21(3) . ?
N4 O3 1.22(3) . ?
N4 O1 1.24(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 C6 1.57(12) . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?
C6' N2' 1.73(14) 2_856 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.48(3) . ?
N2' H2'A 0.8900 . ?
N2' H2'B 0.8900 . ?
C3' H3'C 0.9700 . ?
C3' H3'D 0.9700 . ?
C3' C2' 1.49(3) . ?
N1' H1'A 0.8900 . ?
N1' H1'B 0.8900 . ?
N1' C1' 1.82(13) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.47(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.48(12) 2 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C1' H1'C 0.9700 . ?
C1' H1'D 0.9700 . ?
C1' C2' 1.48(3) . ?
C2' H2'C 0.9700 . ?
C2' H2'D 0.9700 . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C7' C8' 1.47(3) . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?

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 Cd1 O4 96(2) . . ?
N1 Cd1 O3 76.7(19) . . ?
N1 Cd1 N2 113(3) . . ?
N1 Cd1 O1 88(3) . . ?
N1 Cd1 N3 137.4(16) . . ?
O4 Cd1 O3 152.0(17) . . ?
O4 Cd1 O1 159.3(13) . . ?
N2 Cd1 O4 76.9(17) . . ?
N2 Cd1 O3 81.3(13) . . ?
N2 Cd1 O1 120(2) . . ?
O1 Cd1 O3 48.5(12) . . ?
N3 Cd1 O4 77.6(19) . . ?
N3 Cd1 O3 126(2) . . ?
N3 Cd1 N2 106(2) . . ?
N3 Cd1 O1 85.9(18) . . ?
N3' Cd1' O4' 81.0(19) . . ?
N3' Cd1' O1' 81(2) . . ?
O1' Cd1' O4' 158.1(16) . . ?
N2' Cd1' N3' 93(3) . . ?
N2' Cd1' O4' 82.5(19) . . ?
N2' Cd1' O1' 111(3) . . ?
N1' Cd1' N3' 140(2) . . ?
N1' Cd1' O4' 109(3) . . ?
N1' Cd1' O1' 77(3) . . ?
N1' Cd1' N2' 126(3) . . ?
O4' N5' O6' 126(5) . . ?
O5' N5' O6' 115(5) . . ?
O5' N5' O4' 120(4) . . ?
Cd1' N3' H3'A 107.0 . . ?
Cd1' N3' H3'B 107.0 . . ?
H3'A N3' H3'B 106.8 . . ?
C7' N3' Cd1' 121(3) . . ?
C7' N3' H3'A 107.0 . . ?
C7' N3' H3'B 107.0 . . ?
H5'A C5' H5'B 107.5 . . ?
C4' C5' H5'A 108.5 . . ?
C4' C5' H5'B 108.5 . . ?
C4' C5' C6' 115(3) . . ?
C6' C5' H5'A 108.5 . . ?
C6' C5' H5'B 108.5 . . ?
C5' C4' H4'A 109.0 . . ?
C5' C4' H4'B 109.0 . . ?
C5' C4' C3' 113(4) . . ?
H4'A C4' H4'B 107.8 . . ?
C3' C4' H4'A 109.0 . . ?
C3' C4' H4'B 109.0 . . ?
H1A C1 H1B 106.8 . . ?
N1 C1 H1A 107.0 . . ?
N1 C1 H1B 107.0 . . ?
C2 C1 H1A 107.0 . . ?
C2 C1 H1B 107.0 . . ?
C2 C1 N1 121(4) . . ?
O3' N4' O2' 120(4) . . ?
O3' N4' O1' 121(5) . . ?
O2' N4' O1' 119(5) . . ?
H9'A C9' H9'B 107.6 . . ?
C9 C9' H9'A 108.6 . . ?
C9 C9' H9'B 108.6 . . ?
C9 C9' C8' 115(3) . . ?
C8' C9' H9'A 108.6 . . ?
C8' C9' H9'B 108.6 . . ?
H3A C3 H3B 109.0 . . ?
C2 C3 H3A 110.9 . . ?
C2 C3 H3B 110.9 . . ?
C4 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
C4 C3 C2 104(5) . . ?
Cd1 N1 H1C 105.9 . . ?
Cd1 N1 H1D 105.9 . . ?
C1 N1 Cd1 126(2) . . ?
C1 N1 H1C 105.9 . . ?
C1 N1 H1D 105.9 . . ?
H1C N1 H1D 106.3 . . ?
N5' O4' Cd1' 110(3) . . ?
H7A C7 H7B 108.4 . . ?
N3 C7 H7A 110.0 . . ?
N3 C7 H7B 110.0 . . ?
N3 C7 C8 108(3) . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
N5 O4 Cd1 119(3) . . ?
O2 N4 O3 117(4) . . ?
O2 N4 O1 124(4) . . ?
O3 N4 O1 119(4) . . ?
N4' O1' Cd1' 100(4) . . ?
C1 C2 C3 105(5) . . ?
C1 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
C3 C2 H2A 110.7 . . ?
C3 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N4 O3 Cd1 96(2) . . ?
Cd1 N2 H2C 108.3 . . ?
Cd1 N2 H2D 108.3 . . ?
H2C N2 H2D 107.4 . . ?
C6 N2 Cd1 116(4) . . ?
C6 N2 H2C 108.3 . . ?
C6 N2 H2D 108.3 . . ?
C5' C6' H6'A 106.5 . . ?
C5' C6' H6'B 106.5 . . ?
C5' C6' N2' 123(4) . 2_856 ?
H6'A C6' H6'B 106.5 . . ?
N2' C6' H6'A 106.5 2_856 . ?
N2' C6' H6'B 106.5 2_856 . ?
N2 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C5 C6 N2 112(4) . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
Cd1' N2' H2'A 110.8 . . ?
Cd1' N2' H2'B 110.8 . . ?
C6' N2' Cd1' 105(5) 2_846 . ?
C6' N2' H2'A 110.8 2_846 . ?
C6' N2' H2'B 110.8 2_846 . ?
H2'A N2' H2'B 108.9 . . ?
C4' C3' H3'C 110.3 . . ?
C4' C3' H3'D 110.3 . . ?
C4' C3' C2' 107(5) . . ?
H3'C C3' H3'D 108.5 . . ?
C2' C3' H3'C 110.3 . . ?
C2' C3' H3'D 110.3 . . ?
Cd1' N1' H1'A 107.9 . . ?
Cd1' N1' H1'B 107.9 . . ?
H1'A N1' H1'B 107.2 . . ?
C1' N1' Cd1' 118(2) . . ?
C1' N1' H1'A 107.9 . . ?
C1' N1' H1'B 107.9 . . ?
N4 O1 Cd1 96(3) . . ?
Cd1 N3 H3C 109.6 . . ?
Cd1 N3 H3D 109.6 . . ?
C7 N3 Cd1 110(2) . . ?
C7 N3 H3C 109.6 . . ?
C7 N3 H3D 109.6 . . ?
H3C N3 H3D 108.2 . . ?
O6 N5 O5 118(5) . . ?
O6 N5 O4 132(5) . . ?
O4 N5 O5 109(4) . . ?
C9' C9 H9A 108.4 . . ?
C9' C9 H9B 108.4 . . ?
C9' C9 C8 115(3) . . ?
H9A C9 H9B 107.5 . . ?
C8 C9 H9A 108.4 . . ?
C8 C9 H9B 108.4 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
C6 C5 C4 113(4) . 2 ?
H5A C5 H5B 107.8 . . ?
C4 C5 H5A 109.1 2 . ?
C4 C5 H5B 109.1 2 . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C9 C8 C7 109(4) . . ?
C9 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C3 C4 C5 116(4) . 2_545 ?
C3 C4 H4A 108.3 . . ?
C3 C4 H4B 108.3 . . ?
C5 C4 H4A 108.3 2_545 . ?
C5 C4 H4B 108.3 2_545 . ?
H4A C4 H4B 107.4 . . ?
N1' C1' H1'C 107.2 . . ?
N1' C1' H1'D 107.2 . . ?
H1'C C1' H1'D 106.8 . . ?
C2' C1' N1' 121(3) . . ?
C2' C1' H1'C 107.2 . . ?
C2' C1' H1'D 107.2 . . ?
C3' C2' H2'C 109.9 . . ?
C3' C2' H2'D 109.9 . . ?
C1' C2' C3' 109(4) . . ?
C1' C2' H2'C 109.9 . . ?
C1' C2' H2'D 109.9 . . ?
H2'C C2' H2'D 108.3 . . ?
N3' C7' H7'A 107.9 . . ?
N3' C7' H7'B 107.9 . . ?
N3' C7' C8' 118(3) . . ?
H7'A C7' H7'B 107.2 . . ?
C8' C7' H7'A 107.9 . . ?
C8' C7' H7'B 107.9 . . ?
C9' C8' H8'A 108.7 . . ?
C9' C8' H8'B 108.7 . . ?
C7' C8' C9' 114(3) . . ?
C7' C8' H8'A 108.7 . . ?
C7' C8' H8'B 108.7 . . ?
H8'A C8' H8'B 107.6 . . ?

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
Cd1 O4 N5 O6 129(7) . . . . ?
Cd1 O4 N5 O5 -55(5) . . . . ?
Cd1 N2 C6 C5 75(4) . . . . ?
Cd1' N3' C7' C8' 179(2) . . . . ?
Cd1' N1' C1' C2' 159(3) . . . . ?
O2 N4 O3 Cd1 -169(4) . . . . ?
O2 N4 O1 Cd1 169(4) . . . . ?
O3' N4' O1' Cd1' 9(6) . . . . ?
N3' C7' C8' C9' -180(3) . . . . ?
C5' C4' C3' C2' 80(5) . . . . ?
C4' C5' C6' N2' 173(4) . . . 2_856 ?
C4' C3' C2' C1' -179(3) . . . . ?
O6' N5' O4' Cd1' -148(4) . . . . ?
O2' N4' O1' Cd1' -172(4) . . . . ?
C9' C9 C8 C7 -173(3) . . . . ?
N1 C1 C2 C3 42(6) . . . . ?
C2 C1 N1 Cd1 -165(3) . . . . ?
C2 C3 C4 C5 -66(5) . . . 2_545 ?
O3 N4 O1 Cd1 -4(5) . . . . ?
N2 C6 C5 C4 -177(4) . . . 2 ?
C6' C5' C4' C3' -176(3) . . . . ?
N1' C1' C2' C3' -56(5) . . . . ?
O1 N4 O3 Cd1 4(5) . . . . ?
N3 C7 C8 C9 -151(3) . . . . ?
C9 C9' C8' C7' -179(3) . . . . ?
O5' N5' O4' Cd1' 37(5) . . . . ?
C8 C7 N3 Cd1 174(3) . . . . ?
C4 C3 C2 C1 -180(4) . . . . ?
C8' C9' C9 C8 -176(3) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999925 0.00000000 0.00122348
omega rotation goniometer -1 . -0.88992000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -2.28590000 -0.76675894 0.00000000
0.64193514
phi rotation goniometer -1 kappa . 0.00018850 0.00000000 0.99999998
theta rotation goniometer -1 . -0.75634000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.870
####################################################################### 
# 
# 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_2_1_GPa_Cd2_HDA_3_NO3_4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262362'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_2_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.333 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT090_2_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.63 Note
RESPONSE: The data/parameter ratio is affected by the access limits of
 the DAC.
;
_vrf_PLAT342_2_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.08067 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_2_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        758 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT915_2_1_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         31 %
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C10 N4 O4 '
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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.206(12)
_cell_length_b                   6.6183(4)
_cell_length_c                   14.9354(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.11(3)
_cell_angle_gamma                90
_cell_volume                     1396.2(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9020
_cell_measurement_theta_min      2.7290
_shelx_estimated_absorpt_T_max   0.751
_shelx_estimated_absorpt_T_min   0.007
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60999
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -9 4 0.2426
-4 1 21 0.0636
2 9 -3 0.0768
4 -1 -21 0.1275
-2 -9 7 0.0512
-4 2 20 0.0023
2 9 -3 0.2401

_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.08
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.8852 -9.0883 4.2707 -0.0191 -0.7369 0.6757
-4.4945 0.7606 20.8107 0.0146 0.5738 0.8189
1.7207 9.1563 -3.4900 0.0198 0.7621 -0.6471
4.4289 -1.1892 -20.7154 -0.0155 -0.6111 -0.7914
-2.3919 -8.7731 6.7877 -0.0162 -0.6469 0.7624
-4.2059 2.2715 20.2712 0.0185 0.7004 0.7135
1.5614 9.2060 -2.7921 0.0198 0.7836 -0.6209

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.333
_diffrn_reflns_Laue_measured_fraction_max 0.308
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11452
_diffrn_reflns_point_group_measured_fraction_full 0.338
_diffrn_reflns_point_group_measured_fraction_max 0.308
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.754
_diffrn_reflns_theta_min         2.743
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.333
_diffrn_measured_fraction_theta_max 0.308
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 2.10(2) GPa
 (2100000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
 17  ω    -23.00   9.00   1.00   25.00    --    0.12 -13.00   3.00   32
 18  ω    -22.00  11.00   1.00   25.00    --   30.76  53.00 -17.00   33
 19  ω     89.00 114.00   1.00   25.00    --   30.76 134.00 -57.00   25
 20  ω     -9.00  19.00   1.00   25.00    --  -30.53 -81.00-151.00   28
 21  ω      7.00  33.00   1.00   25.00    --  -30.53-114.00-135.00   26
 22  ω     58.00  90.00   1.00   25.00    --    0.12-178.00-120.00   32
 23  ω    -21.00   5.00   1.00   25.00    --    0.12  82.00 153.00   26
 24  ω    -25.00   0.00   1.00   25.00    --   30.76  53.00 162.00   25
 25  ω    -68.00 -15.00   1.00   25.00    --  -30.53  82.00 153.00   53
 26  ω    -24.00  18.00   1.00   25.00    --   30.76   0.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0495491000
_diffrn_orient_matrix_UB_12      -0.0027659000
_diffrn_orient_matrix_UB_13      0.0115023000
_diffrn_orient_matrix_UB_21      -0.0022870000
_diffrn_orient_matrix_UB_22      0.0926933000
_diffrn_orient_matrix_UB_23      0.0236909000
_diffrn_orient_matrix_UB_31      -0.0066075000
_diffrn_orient_matrix_UB_32      -0.0542257000
_diffrn_orient_matrix_UB_33      0.0399029000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.343
_reflns_Friedel_fraction_max     0.307
_reflns_number_gt                1453
_reflns_number_total             1834
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 
;
 Flack x determined using 543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(6)
_refine_ls_extinction_coef       0.008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         1834
_refine_ls_number_restraints     518
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      0.988
_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)+(0.0792P)²+5.5259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1579
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C7'-N3'
 1.45 with sigma of 0.02
 C7-N3
 1.45 with sigma of 0.02
 O6'-N5' \\sim O5'-N5' \\sim O4'-N5' \\sim O1'-N4' \\sim O3'-N4' \\sim O2'-N4'
\\sim O1-N4 \\sim O2-N4 ~
 O3-N4 \\sim O4-N5 \\sim O6-N5 \\sim O5-N5
 with sigma of 0.02
 C4-C3 \\sim C2-C3 \\sim C2-C1 \\sim C5-C6 \\sim C8-C7 \\sim C8-C9 \\sim C9-C9'
\\sim C8'-C9' \\sim C7'-C8' ~
 C6'-C5' \\sim C4'-C5' \\sim C3'-C4' \\sim C2'-C3' \\sim C1'-C2'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3') \\sim Ueq, Uanis(C9') \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq,
Uanis(N3) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5') \\sim Ueq, Uanis(O6') \\sim Ueq, Uanis(O4') \\sim Ueq, Uanis(O5')
\\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(O6') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C8, Cd1, N3, N1, N2, O1, O4, O3, C7, C1, C6, N4, N5, C2, C5, O2, O6, O5, C9,
 C3, C9', C4, C8', C7', N3', Cd1', O4', O1', N2', N1', N5', O5', N4', C1', O6',
 O3', O2', C2', C3', C4', C5', C6'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N3'(H3'A,H3'B), C5'(H5'A,H5'B), C4'(H4'A,H4'B), C1(H1A,H1B), C9'(H9'A,H9'B),
 C3(H3A,H3B), N1(H1C,H1D), C7(H7A,H7B), C2(H2A,H2B), N2(H2C,H2D), C6'(H6'A,
 H6'B), C6(H6A,H6B), N2'(H2'A,H2'B), C3'(H3'C,H3'D), N1'(H1'A,H1'B), N3(H3C,
 H3D), C9(H9A,H9B), C5(H5A,H5B), C8(H8A,H8B), C4(H4A,H4B), C1'(H1'C,H1'D),
 C2'(H2'C,H2'D), C7'(H7'A,H7'B), C8'(H8'A,H8'B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cd1 Cd 0.3354(5) 0.0740(3) 0.08669(19) 0.087(5) Uani 1 1 d . . . . .
Cd1' Cd 1.1723(5) 0.4083(3) 0.39632(19) 0.084(5) Uani 1 1 d . . . . .
O2 O 0.473(4) -0.466(3) 0.0272(16) 0.09(2) Uani 1 1 d D . . . .
N5' N 1.313(3) 0.080(4) 0.3235(14) 0.038(11) Uani 1 1 d D U . . .
O6 O 0.183(4) 0.524(3) 0.2217(15) 0.07(3) Uani 1 1 d D . . . .
O3' O 1.141(3) 0.743(4) 0.4976(14) 0.07(2) Uani 1 1 d D . . . .
N3' N 1.044(5) 0.243(5) 0.3105(17) 0.052(8) Uani 1 1 d D U . . .
H3'A H 1.054341 0.248201 0.252779 0.062 Uiso 1 1 calc R U . . .
H3'B H 1.045534 0.112778 0.326281 0.062 Uiso 1 1 calc R U . . .
O5 O 0.143(4) 0.271(4) 0.1440(16) 0.103(19) Uani 1 1 d D . . . .
C5' C 1.670(4) 0.685(5) 0.412(2) 0.07(2) Uani 1 1 d D . . . .
H5'A H 1.680533 0.541704 0.402821 0.079 Uiso 1 1 calc R U . . .
H5'B H 1.656515 0.703213 0.473507 0.079 Uiso 1 1 calc R U . . .
C4' C 1.586(4) 0.749(5) 0.351(2) 0.07(2) Uani 1 1 d D . . . .
H4'A H 1.598914 0.722766 0.289446 0.081 Uiso 1 1 calc R U . . .
H4'B H 1.578747 0.893386 0.357180 0.081 Uiso 1 1 calc R U . . .
O6' O 1.332(4) -0.044(3) 0.2669(15) 0.045(13) Uani 1 1 d D U . . .
C1 C 0.120(5) -0.147(5) 0.024(2) 0.076(18) Uani 1 1 d D . . . .
H1A H 0.100339 -0.012128 0.004830 0.092 Uiso 1 1 calc R U . . .
H1B H 0.140996 -0.214952 -0.028253 0.092 Uiso 1 1 calc R U . . .
N4' N 1.080(3) 0.796(4) 0.4391(15) 0.05(2) Uani 1 1 d D . . . .
O2' O 1.039(4) 0.948(3) 0.4592(16) 0.08(3) Uani 1 1 d D . . . .
C9' C 0.780(5) 0.289(5) 0.281(2) 0.047(9) Uani 1 1 d D U . . .
H9'A H 0.777968 0.430930 0.265057 0.057 Uiso 1 1 calc R U . . .
H9'B H 0.772445 0.279397 0.345001 0.057 Uiso 1 1 calc R U . . .
C3 C 0.007(5) -0.164(5) 0.135(2) 0.07(3) Uani 1 1 d D . . . .
H3A H 0.055955 -0.183844 0.185204 0.082 Uiso 1 1 calc R U . . .
H3B H -0.003403 -0.020317 0.127204 0.082 Uiso 1 1 calc R U . . .
N1 N 0.213(6) -0.125(5) 0.100(2) 0.079(15) Uani 1 1 d . . . . .
H1C H 0.236504 -0.248989 0.109252 0.095 Uiso 1 1 calc R U . . .
H1D H 0.190413 -0.088967 0.151241 0.095 Uiso 1 1 calc R U . . .
O4' O 1.246(4) 0.063(6) 0.366(2) 0.090(12) Uani 1 1 d D U . . .
C7 C 0.528(5) 0.136(5) 0.187(2) 0.044(9) Uani 1 1 d D U . . .
H7A H 0.548627 0.094413 0.129719 0.053 Uiso 1 1 calc R U . . .
H7B H 0.519519 0.015138 0.221726 0.053 Uiso 1 1 calc R U . . .
O4 O 0.267(4) 0.420(6) 0.119(2) 0.097(13) Uani 1 1 d D . . . .
N4 N 0.425(3) -0.318(3) 0.0439(16) 0.08(2) Uani 1 1 d D . . . .
O1' O 1.064(5) 0.710(4) 0.3673(16) 0.066(17) Uani 1 1 d D . . . .
C2 C 0.037(5) -0.256(5) 0.0510(18) 0.066(17) Uani 1 1 d D . . . .
H2A H 0.052845 -0.397585 0.061406 0.079 Uiso 1 1 calc R U . . .
H2B H -0.014597 -0.248668 0.003124 0.079 Uiso 1 1 calc R U . . .
O3 O 0.363(4) -0.250(4) -0.0110(15) 0.105(19) Uani 1 1 d D . . . .
N2 N 0.337(6) 0.216(4) -0.052(2) 0.05(2) Uani 1 1 d . . . . .
H2C H 0.343413 0.349290 -0.044525 0.064 Uiso 1 1 calc R U . . .
H2D H 0.388522 0.172106 -0.075126 0.064 Uiso 1 1 calc R U . . .
C6' C 1.759(5) 0.796(4) 0.399(2) 0.06(2) Uani 1 1 d D . . . .
H6'A H 1.743882 0.938998 0.396178 0.074 Uiso 1 1 calc R U . . .
H6'B H 1.776921 0.758521 0.340018 0.074 Uiso 1 1 calc R U . . .
C6 C 0.253(6) 0.177(5) -0.118(2) 0.05(3) Uani 1 1 d D . . . .
H6A H 0.267797 0.210370 -0.177876 0.056 Uiso 1 1 calc R U . . .
H6B H 0.237030 0.034138 -0.116911 0.056 Uiso 1 1 calc R U . . .
N2' N 1.155(6) 0.267(4) 0.532(2) 0.09(3) Uani 1 1 d . . . . .
H2'A H 1.104461 0.320960 0.553860 0.108 Uiso 1 1 calc R U . . .
H2'B H 1.143945 0.135096 0.524854 0.108 Uiso 1 1 calc R U . . .
C3' C 1.495(5) 0.651(4) 0.365(2) 0.07(2) Uani 1 1 d D . . . .
H3'C H 1.503835 0.506070 0.372926 0.089 Uiso 1 1 calc R U . . .
H3'D H 1.449072 0.672547 0.312983 0.089 Uiso 1 1 calc R U . . .
N1' N 1.286(5) 0.613(5) 0.3867(18) 0.061(15) Uani 1 1 d . . . . .
H1'A H 1.311771 0.581701 0.336973 0.073 Uiso 1 1 calc R U . . .
H1'B H 1.260232 0.735594 0.377815 0.073 Uiso 1 1 calc R U . . .
O1 O 0.429(5) -0.227(4) 0.1156(16) 0.078(17) Uani 1 1 d D . . . .
N3 N 0.439(5) 0.239(5) 0.170(2) 0.057(8) Uani 1 1 d D U . . .
H3C H 0.448903 0.357666 0.144567 0.068 Uiso 1 1 calc R U . . .
H3D H 0.417382 0.264033 0.222940 0.068 Uiso 1 1 calc R U . . .
N5 N 0.201(3) 0.403(4) 0.1646(16) 0.067(17) Uani 1 1 d D . . . .
C9 C 0.701(5) 0.182(5) 0.2289(19) 0.045(8) Uani 1 1 d D U . . .
H9A H 0.702390 0.041542 0.247856 0.054 Uiso 1 1 calc R U . . .
H9B H 0.712116 0.184026 0.165919 0.054 Uiso 1 1 calc R U . . .
C5 C 0.171(6) 0.298(5) -0.096(2) 0.04(3) Uani 1 1 d D . . . .
H5A H 0.182886 0.440290 -0.105123 0.049 Uiso 1 1 calc R U . . .
H5B H 0.161018 0.278678 -0.033112 0.049 Uiso 1 1 calc R U . . .
O5' O 1.359(4) 0.226(4) 0.3423(16) 0.069(15) Uani 1 1 d D U . . .
C8 C 0.604(5) 0.262(5) 0.236(2) 0.049(9) Uani 1 1 d D U . . .
H8A H 0.593331 0.268877 0.298932 0.059 Uiso 1 1 calc R U . . .
H8B H 0.599734 0.398182 0.211874 0.059 Uiso 1 1 calc R U . . .
C4 C -0.082(5) -0.266(5) 0.155(2) 0.06(3) Uani 1 1 d D . . . .
H4A H -0.092123 -0.238522 0.217428 0.071 Uiso 1 1 calc R U . . .
H4B H -0.074591 -0.410365 0.149226 0.071 Uiso 1 1 calc R U . . .
C1' C 1.370(5) 0.634(4) 0.4663(18) 0.050(16) Uani 1 1 d D . . . .
H1'C H 1.345803 0.704998 0.515751 0.060 Uiso 1 1 calc R U . . .
H1'D H 1.387488 0.499399 0.487433 0.060 Uiso 1 1 calc R U . . .
C2' C 1.459(4) 0.739(4) 0.4470(19) 0.048(16) Uani 1 1 d D . . . .
H2'C H 1.506393 0.724661 0.498099 0.057 Uiso 1 1 calc R U . . .
H2'D H 1.446153 0.881662 0.437457 0.057 Uiso 1 1 calc R U . . .
C7' C 0.951(5) 0.317(5) 0.318(2) 0.047(9) Uani 1 1 d D U . . .
H7'A H 0.948626 0.457129 0.298562 0.057 Uiso 1 1 calc R U . . .
H7'B H 0.940400 0.314825 0.380968 0.057 Uiso 1 1 calc R U . . .
C8' C 0.874(5) 0.206(5) 0.266(2) 0.052(9) Uani 1 1 d D U . . .
H8'A H 0.876975 0.064968 0.283379 0.062 Uiso 1 1 calc R U . . .
H8'B H 0.881812 0.214399 0.202429 0.062 Uiso 1 1 calc R U . . .


_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
Cd1 N1 2.21(6) . ?
Cd1 O4 2.56(4) . ?
Cd1 O3 2.65(2) . ?
Cd1 N2 2.27(3) . ?
Cd1 O1 2.41(4) . ?
Cd1 N3 2.13(5) . ?
Cd1' N3' 2.38(6) . ?
Cd1' O4' 2.58(4) . ?
Cd1' O1' 2.53(5) . ?
Cd1' N2' 2.28(3) . ?
Cd1' N1' 2.12(6) . ?
O2 N4 1.23(2) . ?
N5' O6' 1.23(2) . ?
N5' O4' 1.20(2) . ?
N5' O5' 1.19(2) . ?
O6 N5 1.22(2) . ?
O3' N4' 1.22(2) . ?
N3' H3'A 0.8900 . ?
N3' H3'B 0.8900 . ?
N3' C7' 1.42(3) . ?
O5 N5 1.21(2) . ?
C5' H5'A 0.9700 . ?
C5' H5'B 0.9700 . ?
C5' C4' 1.48(3) . ?
C5' C6' 1.49(3) . ?
C4' H4'A 0.9700 . ?
C4' H4'B 0.9700 . ?
C4' C3' 1.49(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 N1 1.65(9) . ?
C1 C2 1.48(3) . ?
N4' O2' 1.22(2) . ?
N4' O1' 1.22(2) . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C9' C9 1.48(2) . ?
C9' C8' 1.48(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.50(2) . ?
C3 C4 1.49(3) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N3 1.43(3) . ?
C7 C8 1.49(2) . ?
O4 N5 1.22(2) . ?
N4 O3 1.22(2) . ?
N4 O1 1.22(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 C6 1.49(9) . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?
C6' N2' 1.53(9) 2_856 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.48(3) . ?
N2' H2'A 0.8900 . ?
N2' H2'B 0.8900 . ?
C3' H3'C 0.9700 . ?
C3' H3'D 0.9700 . ?
C3' C2' 1.49(2) . ?
N1' H1'A 0.8900 . ?
N1' H1'B 0.8900 . ?
N1' C1' 1.60(8) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.49(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.52(8) 2 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C1' H1'C 0.9700 . ?
C1' H1'D 0.9700 . ?
C1' C2' 1.49(3) . ?
C2' H2'C 0.9700 . ?
C2' H2'D 0.9700 . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C7' C8' 1.47(2) . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?

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 Cd1 O4 101.4(17) . . ?
N1 Cd1 O3 74.4(14) . . ?
N1 Cd1 N2 115(2) . . ?
N1 Cd1 O1 85(2) . . ?
O4 Cd1 O3 156.0(13) . . ?
N2 Cd1 O4 81.0(12) . . ?
N2 Cd1 O3 79.5(9) . . ?
N2 Cd1 O1 116.5(15) . . ?
O1 Cd1 O4 157.1(12) . . ?
O1 Cd1 O3 46.9(10) . . ?
N3 Cd1 N1 139.0(12) . . ?
N3 Cd1 O4 71.5(18) . . ?
N3 Cd1 O3 127.2(17) . . ?
N3 Cd1 N2 104.2(18) . . ?
N3 Cd1 O1 89.2(17) . . ?
N3' Cd1' O4' 78.2(16) . . ?
N3' Cd1' O1' 81.6(15) . . ?
O1' Cd1' O4' 157.0(12) . . ?
N2' Cd1' N3' 98.1(19) . . ?
N2' Cd1' O4' 83.0(12) . . ?
N2' Cd1' O1' 110.8(16) . . ?
N1' Cd1' N3' 143.2(11) . . ?
N1' Cd1' O4' 103.4(18) . . ?
N1' Cd1' O1' 86.4(18) . . ?
N1' Cd1' N2' 119(2) . . ?
O4' N5' O6' 123(4) . . ?
O5' N5' O6' 123(3) . . ?
O5' N5' O4' 114(3) . . ?
Cd1' N3' H3'A 108.0 . . ?
Cd1' N3' H3'B 108.0 . . ?
H3'A N3' H3'B 107.2 . . ?
C7' N3' Cd1' 117(2) . . ?
C7' N3' H3'A 108.0 . . ?
C7' N3' H3'B 108.0 . . ?
H5'A C5' H5'B 107.6 . . ?
C4' C5' H5'A 108.6 . . ?
C4' C5' H5'B 108.6 . . ?
C4' C5' C6' 115(3) . . ?
C6' C5' H5'A 108.6 . . ?
C6' C5' H5'B 108.6 . . ?
C5' C4' H4'A 108.2 . . ?
C5' C4' H4'B 108.2 . . ?
C5' C4' C3' 117(3) . . ?
H4'A C4' H4'B 107.3 . . ?
C3' C4' H4'A 108.2 . . ?
C3' C4' H4'B 108.2 . . ?
H1A C1 H1B 107.3 . . ?
N1 C1 H1A 108.0 . . ?
N1 C1 H1B 108.0 . . ?
C2 C1 H1A 108.0 . . ?
C2 C1 H1B 108.0 . . ?
C2 C1 N1 117(3) . . ?
O3' N4' O2' 113(3) . . ?
O1' N4' O3' 124(3) . . ?
O1' N4' O2' 124(4) . . ?
H9'A C9' H9'B 107.8 . . ?
C9 C9' H9'A 109.1 . . ?
C9 C9' H9'B 109.1 . . ?
C8' C9' H9'A 109.1 . . ?
C8' C9' H9'B 109.1 . . ?
C8' C9' C9 113(3) . . ?
H3A C3 H3B 108.4 . . ?
C2 C3 H3A 110.1 . . ?
C2 C3 H3B 110.1 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
C4 C3 C2 108(3) . . ?
Cd1 N1 H1C 106.2 . . ?
Cd1 N1 H1D 106.2 . . ?
C1 N1 Cd1 124.4(17) . . ?
C1 N1 H1C 106.2 . . ?
C1 N1 H1D 106.2 . . ?
H1C N1 H1D 106.4 . . ?
N5' O4' Cd1' 112(3) . . ?
H7A C7 H7B 107.8 . . ?
N3 C7 H7A 108.9 . . ?
N3 C7 H7B 108.9 . . ?
N3 C7 C8 113(3) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
N5 O4 Cd1 111(3) . . ?
O3 N4 O2 122(3) . . ?
O3 N4 O1 112(3) . . ?
O1 N4 O2 126(4) . . ?
N4' O1' Cd1' 99(3) . . ?
C1 C2 C3 110(3) . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N4 O3 Cd1 93.8(17) . . ?
Cd1 N2 H2C 108.2 . . ?
Cd1 N2 H2D 108.2 . . ?
H2C N2 H2D 107.4 . . ?
C6 N2 Cd1 116(3) . . ?
C6 N2 H2C 108.2 . . ?
C6 N2 H2D 108.2 . . ?
C5' C6' H6'A 107.7 . . ?
C5' C6' H6'B 107.7 . . ?
C5' C6' N2' 119(3) . 2_856 ?
H6'A C6' H6'B 107.1 . . ?
N2' C6' H6'A 107.7 2_856 . ?
N2' C6' H6'B 107.7 2_856 . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 N2 111(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
Cd1' N2' H2'A 108.9 . . ?
Cd1' N2' H2'B 108.9 . . ?
C6' N2' Cd1' 113(4) 2_846 . ?
C6' N2' H2'A 108.9 2_846 . ?
C6' N2' H2'B 108.9 2_846 . ?
H2'A N2' H2'B 107.8 . . ?
C4' C3' H3'C 109.9 . . ?
C4' C3' H3'D 109.9 . . ?
C4' C3' C2' 109(4) . . ?
H3'C C3' H3'D 108.3 . . ?
C2' C3' H3'C 109.9 . . ?
C2' C3' H3'D 109.9 . . ?
Cd1' N1' H1'A 107.0 . . ?
Cd1' N1' H1'B 107.0 . . ?
H1'A N1' H1'B 106.7 . . ?
C1' N1' Cd1' 121.3(18) . . ?
C1' N1' H1'A 107.0 . . ?
C1' N1' H1'B 107.0 . . ?
N4 O1 Cd1 106(3) . . ?
Cd1 N3 H3C 108.9 . . ?
Cd1 N3 H3D 108.9 . . ?
C7 N3 Cd1 113(2) . . ?
C7 N3 H3C 108.9 . . ?
C7 N3 H3D 108.9 . . ?
H3C N3 H3D 107.7 . . ?
O5 N5 O6 118(4) . . ?
O5 N5 O4 118(3) . . ?
O4 N5 O6 124(4) . . ?
C9' C9 H9A 108.1 . . ?
C9' C9 H9B 108.1 . . ?
C9' C9 C8 117(3) . . ?
H9A C9 H9B 107.3 . . ?
C8 C9 H9A 108.1 . . ?
C8 C9 H9B 108.1 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
C6 C5 C4 110(3) . 2 ?
H5A C5 H5B 108.2 . . ?
C4 C5 H5A 109.7 2 . ?
C4 C5 H5B 109.7 2 . ?
C7 C8 C9 113(3) . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C3 C4 C5 115(3) . 2_545 ?
C3 C4 H4A 108.4 . . ?
C3 C4 H4B 108.4 . . ?
C5 C4 H4A 108.4 2_545 . ?
C5 C4 H4B 108.4 2_545 . ?
H4A C4 H4B 107.5 . . ?
N1' C1' H1'C 107.7 . . ?
N1' C1' H1'D 107.7 . . ?
H1'C C1' H1'D 107.1 . . ?
C2' C1' N1' 119(3) . . ?
C2' C1' H1'C 107.7 . . ?
C2' C1' H1'D 107.7 . . ?
C3' C2' H2'C 109.6 . . ?
C3' C2' H2'D 109.6 . . ?
C1' C2' C3' 110(3) . . ?
C1' C2' H2'C 109.6 . . ?
C1' C2' H2'D 109.6 . . ?
H2'C C2' H2'D 108.1 . . ?
N3' C7' H7'A 108.4 . . ?
N3' C7' H7'B 108.4 . . ?
N3' C7' C8' 116(3) . . ?
H7'A C7' H7'B 107.4 . . ?
C8' C7' H7'A 108.4 . . ?
C8' C7' H7'B 108.4 . . ?
C9' C8' H8'A 109.3 . . ?
C9' C8' H8'B 109.3 . . ?
C7' C8' C9' 112(3) . . ?
C7' C8' H8'A 109.3 . . ?
C7' C8' H8'B 109.3 . . ?
H8'A C8' H8'B 108.0 . . ?

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
Cd1 O4 N5 O6 146(4) . . . . ?
Cd1 O4 N5 O5 -44(4) . . . . ?
Cd1 N2 C6 C5 75(3) . . . . ?
Cd1' N3' C7' C8' -178.1(19) . . . . ?
Cd1' N1' C1' C2' 165(2) . . . . ?
O2 N4 O3 Cd1 -171(3) . . . . ?
O2 N4 O1 Cd1 170(3) . . . . ?
O3' N4' O1' Cd1' 7(4) . . . . ?
N3' C7' C8' C9' 177(3) . . . . ?
C5' C4' C3' C2' 75(4) . . . . ?
C4' C5' C6' N2' 170(3) . . . 2_856 ?
C4' C3' C2' C1' -176(3) . . . . ?
O6' N5' O4' Cd1' -145(3) . . . . ?
O2' N4' O1' Cd1' -176(3) . . . . ?
C9' C9 C8 C7 -176(2) . . . . ?
N1 C1 C2 C3 54(5) . . . . ?
C2 C1 N1 Cd1 -169(3) . . . . ?
C2 C3 C4 C5 -75(4) . . . 2_545 ?
O3 N4 O1 Cd1 -13(4) . . . . ?
N2 C6 C5 C4 -172(3) . . . 2 ?
C6' C5' C4' C3' -177(2) . . . . ?
N1' C1' C2' C3' -52(4) . . . . ?
O1 N4 O3 Cd1 11(3) . . . . ?
N3 C7 C8 C9 -163(3) . . . . ?
C9 C9' C8' C7' 179(2) . . . . ?
O5' N5' O4' Cd1' 36(4) . . . . ?
C8 C7 N3 Cd1 173.0(19) . . . . ?
C4 C3 C2 C1 175(3) . . . . ?
C8' C9' C9 C8 -177(3) . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999925 0.00000000 0.00122348
omega rotation goniometer -1 . -0.88992000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -2.28590000 -0.76675894 0.00000000
0.64193514
phi rotation goniometer -1 kappa . 0.00018850 0.00000000 0.99999998
theta rotation goniometer -1 . -0.75634000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.841
_oxdiff_exptl_absorpt_empirical_full_min 0.851
####################################################################### 
# 
# 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_0_0001_GPa_Cu_HDA_2_MeCN_2x2BF4
_database_code_depnum_ccdc_archive 'CCDC 2262365'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_audit_creation_date             2021-08-18
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2 Cu F8.07 N6'
_chemical_formula_weight         553.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         C6H14N2Cu
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   12.9608(7)
_cell_length_b                   14.1880(8)
_cell_length_c                   27.6850(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5091.0(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1157
_cell_measurement_temperature    293(4)
_cell_measurement_theta_max      27.6020
_cell_measurement_theta_min      3.4560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2301
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.111
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            3238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.211
_diffrn_reflns_theta_min         3.067
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     36.00  62.00   1.00   12.50    --   15.36 179.00  30.00   26
  2  ω    -25.00  18.00   1.00   12.50    --  -16.84 -99.00-150.00   43
  3  ω    -81.00 -11.00   1.00   12.50    --  -16.84 -37.00 150.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0074662000
_diffrn_orient_matrix_UB_12      0.0162611000
_diffrn_orient_matrix_UB_13      -0.0239694000
_diffrn_orient_matrix_UB_21      0.0496814000
_diffrn_orient_matrix_UB_22      -0.0209687000
_diffrn_orient_matrix_UB_23      -0.0003230000
_diffrn_orient_matrix_UB_31      -0.0216673000
_diffrn_orient_matrix_UB_32      -0.0423945000
_diffrn_orient_matrix_UB_33      -0.0090302000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1186
_reflns_number_total             1347
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1347
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.059
_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)+(0.0986P)²+9.1566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1547
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_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
Cu1 Cu 0.375000 0.375000 0.375000 0.0276(3) Uani 1 4 d S T P . .
N1 N 0.48763(19) 0.38748(16) 0.42651(9) 0.0336(6) Uani 1 1 d . . . . .
H1A H 0.532575 0.430180 0.415921 0.040 Uiso 1 1 calc R U . . .
H1B H 0.458122 0.411506 0.452794 0.040 Uiso 1 1 calc R U . . .
C3 C 0.7002(3) 0.2404(3) 0.48708(15) 0.0524(9) Uani 1 1 d . . . . .
H3A H 0.655210 0.205397 0.508579 0.063 Uiso 1 1 calc R U . . .
H3B H 0.714534 0.200512 0.459422 0.063 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.5532(3) 0.375000 0.0634(14) Uani 1 2 d S T P . .
C1 C 0.5472(3) 0.3046(2) 0.44185(13) 0.0453(8) Uani 1 1 d . . . . .
H1C H 0.566165 0.268639 0.413388 0.054 Uiso 1 1 calc R U . . .
H1D H 0.503263 0.264885 0.461609 0.054 Uiso 1 1 calc R U . . .
C2 C 0.6434(3) 0.3268(3) 0.46979(15) 0.0478(9) Uani 1 1 d . . . . .
H2A H 0.625134 0.365123 0.497524 0.057 Uiso 1 1 calc R U . . .
H2B H 0.689164 0.363707 0.449532 0.057 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.7359(5) 0.375000 0.097(3) Uani 1 2 d S T P . .
H5A H 0.439526 0.758483 0.362499 0.146 Uiso 0.5 1 calc R U P A -1
H5B H 0.365862 0.758483 0.407412 0.146 Uiso 0.5 1 calc R U P A -1
H5C H 0.319612 0.758483 0.355089 0.146 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.6318(5) 0.375000 0.0637(17) Uani 1 2 d S T P . .
B1 B 0.625000 0.125000 0.3120(2) 0.0543(16) Uani 1 2 d S T P . .
F1 F 0.6536(4) 0.1956(3) 0.34188(17) 0.1377(17) Uani 1 1 d . . . . .
F2 F 0.5515(4) 0.1632(3) 0.28449(13) 0.1365(17) 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
Cu1 N1 2.048(2) . ?
Cu1 N1 2.048(2) 7 ?
Cu1 N1 2.048(2) 12 ?
Cu1 N1 2.048(2) 14 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.470(4) . ?
C3 C3 1.501(6) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.508(5) . ?
N2 C4 1.116(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.500(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C5 C4 1.477(10) . ?
B1 F1 1.351(5) . ?
B1 F1 1.351(5) 2_655 ?
B1 F2 1.335(5) 2_655 ?
B1 F2 1.335(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
N1 Cu1 N1 170.08(13) . 12 ?
N1 Cu1 N1 91.76(15) 12 7 ?
N1 Cu1 N1 89.09(15) . 7 ?
N1 Cu1 N1 91.76(15) . 14 ?
N1 Cu1 N1 89.10(15) 12 14 ?
N1 Cu1 N1 170.08(13) 14 7 ?
Cu1 N1 H1A 107.2 . . ?
Cu1 N1 H1B 107.2 . . ?
H1A N1 H1B 106.9 . . ?
C1 N1 Cu1 120.42(19) . . ?
C1 N1 H1A 107.2 . . ?
C1 N1 H1B 107.2 . . ?
C3 C3 H3A 108.5 29_656 . ?
C3 C3 H3B 108.5 29_656 . ?
C3 C3 C2 115.1(4) 29_656 . ?
H3A C3 H3B 107.5 . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
N1 C1 H1C 108.6 . . ?
N1 C1 H1D 108.6 . . ?
N1 C1 C2 114.6(3) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.6 . . ?
C2 C1 H1D 108.6 . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 C3 113.5(3) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
N2 C4 C5 180.0 . . ?
F1 B1 F1 104.6(6) . 2_655 ?
F2 B1 F1 117.0(3) 2_655 . ?
F2 B1 F1 104.1(2) 2_655 2_655 ?
F2 B1 F1 117.0(3) . 2_655 ?
F2 B1 F1 104.1(2) . . ?
F2 B1 F2 110.4(6) . 2_655 ?

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
Cu1 N1 C1 C2 165.2(3) . . . . ?
N1 C1 C2 C3 177.3(3) . . . . ?
C3 C3 C2 C1 176.9(4) 29_656 . . . ?

_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 1.306
_oxdiff_exptl_absorpt_empirical_full_min 0.866
####################################################################### 
# 
# 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_4_3_GPa_Cd2_HDA_3_NO3_4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262364'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We made several attempts to obtain better quality data for this 
structure however, due to absorption of the sample, disorder, poor crystal quality etc.
 crystal diffracted weakly. Furthermore the data come from high-pressure studies and 
 are limited by the DAC opening angle.
;
_vrf_PLAT020_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.340 Report
RESPONSE: We made several attempts to obtain better quality data for this structure
 however, due to absorption of the sample, disorder, poor crystal quality etc. 
 crystal diffracted weakly. Furthermore the data come from high-pressure studies 
 and are limited by the DAC opening angle.
;
_vrf_PLAT029_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.331 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT090_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.62 Note
RESPONSE: The data/parameter ratio is affected by the access limits of
 the DAC.
;
_vrf_PLAT342_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.17 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT026_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        39% Check
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT082_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: We made several attempts to obtain better quality data for
 this structure however, due to absorption of the sample, disorder, poor crystal quality etc. 
 crystal diffracted weakly. Furthermore the data come from high-pressure studies and 
 are limited by the DAC opening angle.
;
_vrf_PLAT084_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.45 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT149_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.11 Degree
RESPONSE: We made several attempts to obtain better quality data for 
this structure however, due to absorption of the sample, disorder, 
poor crystal quality etc. crystal diffracted weakly. Furthermore the 
data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT410_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Short Intra H...H Contact  H9'A     ..H6'A     .       1.83 Ang.
RESPONSE: Due to the high-pressure some atoms may have an ill-defined
 connectivity or are subjected to a unresolved spatial disorder. These 
 factors contribute for inaccurate automatic placement of the hydrogen atoms.
;
_vrf_PLAT411_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Short Inter H...H Contact  H7B      ..H4'A     .       1.93 Ang.
RESPONSE: Due to the high-pressure some atoms may have an ill-defined 
connectivity or are subjected to a unresolved spatial disorder. These 
factors contribute for inaccurate automatic placement of the hydrogen atoms.
;
_vrf_PLAT911_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.588        729 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT915_4_3_GPa_Cd2_HDA_3_NO3_4 
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         34 %
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2023-05-10
_chemical_name_common            Cd2_HDA_3_NO3_4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H24 Cd N5 O6'
_chemical_formula_sum            'C9 H24 Cd N5 O6'
_chemical_formula_weight         410.73
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd N4 O4 C10 H10'
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'
Cd Cd -0.8075 1.2024 '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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   14.10(4)
_cell_length_b                   6.4726(15)
_cell_length_c                   14.568(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.60(11)
_cell_angle_gamma                90
_cell_volume                     1325(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1401
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3480
_cell_measurement_theta_min      2.8650
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.566
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             836
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 8 11 0.0462
3 2 -20 0.1871
4 -5 -6 0.0644
-3 -3 19 0.1482
-19 -1 -2 0.0148
19 1 2 0.0246

_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.08
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.1528 7.6240 10.7839 0.0598 0.4493 -0.8914
3.1480 2.2028 -19.8284 0.0919 0.6946 0.7135
3.5449 -4.6448 -6.1384 -0.0922 -0.2802 0.5337
-2.7411 -3.2180 19.1378 -0.1020 -0.7728 -0.6264
-19.4154 -1.1261 -2.1135 0.9915 -0.1299 -0.0092
19.4154 1.1261 2.1135 -0.9915 0.1299 0.0092

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3401
_diffrn_reflns_av_unetI/netI     0.2258
_diffrn_reflns_Laue_measured_fraction_full 0.331
_diffrn_reflns_Laue_measured_fraction_max 0.331
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8713
_diffrn_reflns_point_group_measured_fraction_full 0.334
_diffrn_reflns_point_group_measured_fraction_max 0.334
_diffrn_reflns_theta_full        24.704
_diffrn_reflns_theta_max         24.704
_diffrn_reflns_theta_min         1.934
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.331
_diffrn_measured_fraction_theta_max 0.331
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 4.30(2) GPa
 (4300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
 17  ω    -23.00   9.00   1.00   25.00    --    0.12 -13.00   3.00   32
 18  ω    -22.00  11.00   1.00   25.00    --   30.76  53.00 -17.00   33
 19  ω     89.00 114.00   1.00   25.00    --   30.76 134.00 -57.00   25
 20  ω     -9.00  19.00   1.00   25.00    --  -30.53 -81.00-151.00   28
 21  ω      7.00  33.00   1.00   25.00    --  -30.53-114.00-135.00   26
 22  ω     58.00  90.00   1.00   25.00    --    0.12-178.00-120.00   32
 23  ω    -21.00   5.00   1.00   25.00    --    0.12  82.00 153.00   26
 24  ω    -25.00   0.00   1.00   25.00    --   30.76  53.00 162.00   25
 25  ω    -68.00 -15.00   1.00   25.00    --  -30.53  82.00 153.00   53
 26  ω    -24.00  18.00   1.00   25.00    --   30.76   0.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0496147000
_diffrn_orient_matrix_UB_12      -0.0012870000
_diffrn_orient_matrix_UB_13      -0.0126533000
_diffrn_orient_matrix_UB_21      0.0037944000
_diffrn_orient_matrix_UB_22      0.0948024000
_diffrn_orient_matrix_UB_23      -0.0238974000
_diffrn_orient_matrix_UB_31      0.0080917000
_diffrn_orient_matrix_UB_32      -0.0548158000
_diffrn_orient_matrix_UB_33      -0.0407881000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.337
_reflns_Friedel_fraction_max     0.337
_reflns_number_gt                584
_reflns_number_total             1508
_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       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 
;
 Flack x determined using 136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         1508
_refine_ls_number_restraints     800
_refine_ls_R_factor_all          0.2921
_refine_ls_R_factor_gt           0.1558
_refine_ls_restrained_S_all      0.991
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3622
_refine_ls_wR_factor_ref         0.4524
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 N2'-C6'_$1
 1.4 with sigma of 0.02
 C9'-C9
 1.5 with sigma of 0.02
 C9'-C8'
 1.5 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 C4_$2-C5
 1.5 with sigma of 0.02
 C7'-N3'
 1.45 with sigma of 0.02
 H1'A-H3'C
 2.05 with sigma of 0.02
 H8A_$3-H4'A_$4
 2.05 with sigma of 0.02
 H1'A-H3'D
 2.05 with sigma of 0.02
 C4-C3 \\sim C3-C2 \\sim C2-C1 \\sim C8-C7 \\sim C9-C8 \\sim C9'-C9 \\sim
C9'-C8' \\sim C8'-C7' \\sim C6-C5 ~
 C2'-C1' \\sim C3'-C2' \\sim C4'-C3' \\sim C5'-C4' \\sim C6'-C5'
 with sigma of 0.02
 Cd1'-N1' \\sim Cd1'-N3' \\sim Cd1-N3 \\sim Cd1-N2 \\sim Cd1'-N2' \\sim Cd1-N1
 with sigma of 0.02
 N1'-C1' \\sim N3'-C7' \\sim N3-C7 \\sim N2-C6 \\sim N1-C1
 with sigma of 0.02
 O4-N5 \\sim O5-N5 \\sim O6-N5 \\sim O3-N4 \\sim O2-N4 \\sim O1-N4 \\sim
O2'-N4' \\sim O1'-N4' \\sim O3'-N4' ~
 O4'-N5' \\sim O5'-N5' \\sim O6'-N5'
 with sigma of 0.02
 O6'-O5' \\sim O5'-O4' \\sim O6'-O4' \\sim O2'-O1' \\sim O3'-O1' \\sim O3'-O2'
\\sim O5-O4 \\sim O6-O4 ~
 O6-O5 \\sim O3-O1 \\sim O2-O1 \\sim O3-O2
 with sigma of 0.02
3. Restrained planarity
 O4, N5, O6, O5
 with sigma of 0.1
 O4', N5', O6', O5'
 with sigma of 0.1
 O1', N4', O3', O2'
 with sigma of 0.1
 O3, O1, N4, O2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C9') \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq, Uanis(N3')
\\sim Ueq, Uanis(Cd1') \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O4') \\sim Ueq,
Uanis(O1') \\sim Ueq, Uanis(N2') \\sim Ueq, Uanis(N1') \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(N5') \\sim Ueq, Uanis(N4') \\sim Ueq, Uanis(C1') \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(O6') \\sim Ueq, Uanis(O5') \\sim Ueq, Uanis(O3')
\\sim Ueq, Uanis(O2') \\sim Ueq, Uanis(C2') \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C3') \\sim Ueq, Uanis(Cd1) \\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(C5') \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(N4) \\sim Ueq, Uanis(C6') \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O1) \\sim Ueq,
Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.03 and sigma for terminal atoms of 0.06
Uanis(N1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.02
Uanis(O3') \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq, Uanis(N3')
\\sim Ueq, Uanis(C9') \\sim Ueq, Uanis(Cd1') \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(O1') \\sim Ueq, Uanis(N2') \\sim Ueq, Uanis(N1') \\sim Ueq, Uanis(O4')
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N4') \\sim Ueq, Uanis(C1') \\sim Ueq,
Uanis(N5') \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O2') \\sim Ueq, Uanis(C2')
\\sim Ueq, Uanis(O6') \\sim Ueq, Uanis(O5') \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C3') \\sim Ueq, Uanis(Cd1) \\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(N4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C6') \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N4') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2') = Uanis(N4') = Uanis(O1') = Uanis(O3')
Uanis(O4') = Uanis(N5') = Uanis(O6') = Uanis(O5')
Uanis(O4) = Uanis(N5) = Uanis(O6) = Uanis(O5)
Uanis(N1) = Uanis(C1) = Uanis(C2)
5. Rigid body (RIGU) restrains
 Cd1, C7', C8', N3', C9', Cd1', C9, O1', N2', N1', O4', C8, N4', C1', N5', C7,
 O3', O2', C2', O6', O5', N3, C3', C4', N1, O4, O3, N2, O1, C5', C1, N5, N4, C6,
  C6', C2, O6, O5, O2, C5, C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Secondary CH2 refined with riding coordinates:
 C7'(H7'A,H7'B), N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), C1(H1C,H1D), C6(H6A,
 H6B), C7(H7A,H7B), C2(H2C,H2D), C5(H5A,H5B), C8(H8A,H8B), C3(H3C,H3D), C9(H9A,
 H9B), C4(H4A,H4B), C9'(H9'A,H9'B), C8'(H8'A,H8'B), N3'(H3'A,H3'B), N2'(H2'A,
 H2'B), N1'(H1'A,H1'B), C1'(H1'C,H1'D), C2'(H2'C,H2'D), C3'(H3'C,H3'D),
 C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B)
;
_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
C7' C 0.961(9) 0.31(2) 0.323(9) 0.10(3) Uani 1 1 d D U . . .
H7'A H 0.963480 0.457084 0.313006 0.115 Uiso 1 1 calc R U . . .
H7'B H 0.946188 0.289129 0.386742 0.115 Uiso 1 1 calc R U . . .
Cd1 Cd 0.3404(17) 0.085(2) 0.0836(7) 0.115(14) Uani 1 1 d D U . . .
N1 N 0.211(6) -0.113(13) 0.109(6) 0.077(19) Uani 1 1 d D U . . .
H1A H 0.231792 -0.236444 0.128954 0.093 Uiso 1 1 calc R U . . .
H1B H 0.181741 -0.055375 0.154777 0.093 Uiso 1 1 calc R U . . .
O4 O 0.264(8) 0.380(10) 0.129(5) 0.093(18) Uani 1 1 d D U . . .
O3 O 0.370(8) -0.239(10) -0.015(5) 0.09(2) Uani 1 1 d D U . . .
N2 N 0.345(12) 0.234(15) -0.059(5) 0.07(2) Uani 1 1 d D U . . .
H2A H 0.349713 0.370654 -0.052070 0.087 Uiso 1 1 calc R U . . .
H2B H 0.396203 0.189905 -0.084424 0.087 Uiso 1 1 calc R U . . .
O1 O 0.442(10) -0.226(10) 0.115(5) 0.10(2) Uani 1 1 d D U . . .
N3 N 0.463(6) 0.232(13) 0.172(4) 0.07(2) Uani 1 1 d D U . . .
H3A H 0.490220 0.325535 0.138313 0.081 Uiso 1 1 calc R U . . .
H3B H 0.438637 0.298958 0.218264 0.081 Uiso 1 1 calc R U . . .
C1 C 0.141(8) -0.144(16) 0.031(6) 0.077(19) Uani 1 1 d D U . . .
H1C H 0.169385 -0.227107 -0.014628 0.093 Uiso 1 1 calc R U . . .
H1D H 0.124770 -0.010933 0.003759 0.093 Uiso 1 1 calc R U . . .
N5 N 0.189(8) 0.394(7) 0.162(4) 0.093(18) Uani 1 1 d D U . . .
N4 N 0.431(8) -0.304(8) 0.040(4) 0.10(3) Uani 1 1 d D U . . .
C6 C 0.260(10) 0.187(14) -0.120(7) 0.06(3) Uani 1 1 d D U . . .
H6A H 0.244918 0.041266 -0.114366 0.068 Uiso 1 1 calc R U . . .
H6B H 0.273185 0.213769 -0.182881 0.068 Uiso 1 1 calc R U . . .
C7 C 0.538(8) 0.097(17) 0.213(6) 0.09(3) Uani 1 1 d D U . . .
H7A H 0.566608 0.019255 0.164925 0.102 Uiso 1 1 calc R U . . .
H7B H 0.512604 -0.000155 0.255143 0.102 Uiso 1 1 calc R U . . .
C2 C 0.051(9) -0.248(16) 0.056(6) 0.077(19) Uani 1 1 d D U . . .
H2C H 0.005757 -0.242358 0.002109 0.093 Uiso 1 1 calc R U . . .
H2D H 0.065445 -0.392530 0.067476 0.093 Uiso 1 1 calc R U . . .
O6 O 0.175(10) 0.529(9) 0.216(5) 0.093(18) Uani 1 1 d D U . . .
O5 O 0.129(8) 0.265(11) 0.144(5) 0.093(18) Uani 1 1 d D U . . .
O2 O 0.480(10) -0.448(11) 0.022(5) 0.10(4) Uani 1 1 d D U . . .
C5 C 0.177(10) 0.315(17) -0.095(7) 0.07(3) Uani 1 1 d D U . . .
H5A H 0.164200 0.293645 -0.031347 0.086 Uiso 1 1 calc R U . . .
H5B H 0.189146 0.461068 -0.104286 0.086 Uiso 1 1 calc R U . . .
C8 C 0.611(11) 0.235(14) 0.263(9) 0.11(4) Uani 1 1 d D U . . .
H8A H 0.613385 0.207473 0.328260 0.132 Uiso 1 1 calc R U . . .
H8B H 0.593307 0.378175 0.252414 0.132 Uiso 1 1 calc R U . . .
C3 C 0.001(11) -0.169(14) 0.136(7) 0.07(3) Uani 1 1 d D U . . .
H3C H -0.007883 -0.021356 0.127626 0.083 Uiso 1 1 calc R U . . .
H3D H 0.044214 -0.186453 0.190972 0.083 Uiso 1 1 calc R U . . .
C9 C 0.707(12) 0.194(16) 0.228(7) 0.07(2) Uani 1 1 d D U . . .
H9A H 0.707264 0.244400 0.164937 0.085 Uiso 1 1 calc R U . . .
H9B H 0.718878 0.046774 0.227362 0.085 Uiso 1 1 calc R U . . .
C4 C -0.094(11) -0.256(14) 0.159(6) 0.05(3) Uani 1 1 d D U . . .
H4A H -0.090674 -0.405420 0.156350 0.065 Uiso 1 1 calc R U . . .
H4B H -0.105222 -0.217114 0.221203 0.065 Uiso 1 1 calc R U . . .
C9' C 0.784(11) 0.301(19) 0.288(8) 0.09(3) Uani 1 1 d D U . . .
H9'A H 0.779715 0.449064 0.278698 0.105 Uiso 1 1 calc R U . . .
H9'B H 0.776650 0.271026 0.351889 0.105 Uiso 1 1 calc R U . . .
C8' C 0.879(10) 0.224(16) 0.262(7) 0.07(3) Uani 1 1 d D U . . .
H8'A H 0.887239 0.262342 0.198541 0.089 Uiso 1 1 calc R U . . .
H8'B H 0.880112 0.073993 0.265321 0.089 Uiso 1 1 calc R U . . .
N3' N 1.055(7) 0.225(13) 0.314(5) 0.07(2) Uani 1 1 d D U . . .
H3'A H 1.067322 0.228036 0.254876 0.085 Uiso 1 1 calc R U . . .
H3'B H 1.057061 0.094131 0.332354 0.085 Uiso 1 1 calc R U . . .
Cd1' Cd 1.1702(17) 0.408(2) 0.3985(7) 0.116(15) Uani 1 1 d D U . . .
O4' O 1.240(9) 0.031(10) 0.357(5) 0.102(17) Uani 1 1 d D U . . .
O1' O 1.075(11) 0.736(11) 0.369(5) 0.115(19) Uani 1 1 d D U . . .
N2' N 1.183(11) 0.283(18) 0.546(4) 0.12(3) Uani 1 1 d D U . . .
H2'A H 1.137176 0.347758 0.572642 0.146 Uiso 1 1 calc R U . . .
H2'B H 1.164033 0.152421 0.539536 0.146 Uiso 1 1 calc R U . . .
N1' N 1.305(5) 0.602(13) 0.401(5) 0.08(2) Uani 1 1 d D U . . .
H1'A H 1.340351 0.547191 0.358795 0.100 Uiso 1 1 calc DR U . . .
H1'B H 1.287217 0.726429 0.379250 0.100 Uiso 1 1 calc R U . . .
N5' N 1.314(9) 0.061(8) 0.322(4) 0.102(17) Uani 1 1 d D U . . .
N4' N 1.082(9) 0.821(9) 0.442(4) 0.115(19) Uani 1 1 d D U . . .
C1' C 1.369(8) 0.639(16) 0.482(6) 0.08(3) Uani 1 1 d D U . . .
H1'C H 1.392876 0.509868 0.509364 0.101 Uiso 1 1 calc R U . . .
H1'D H 1.338512 0.717719 0.528013 0.101 Uiso 1 1 calc R U . . .
O6' O 1.338(11) -0.053(10) 0.263(5) 0.102(17) Uani 1 1 d D U . . .
O5' O 1.362(10) 0.209(12) 0.345(6) 0.102(17) Uani 1 1 d D U . . .
O3' O 1.141(9) 0.765(12) 0.500(5) 0.115(19) Uani 1 1 d D U . . .
O2' O 1.032(10) 0.966(12) 0.456(5) 0.115(19) Uani 1 1 d D U . . .
C2' C 1.447(11) 0.760(14) 0.443(7) 0.08(3) Uani 1 1 d D U . . .
H2'C H 1.501300 0.764428 0.488347 0.095 Uiso 1 1 calc R U . . .
H2'D H 1.425213 0.900961 0.432958 0.095 Uiso 1 1 calc R U . . .
C3' C 1.481(6) 0.681(14) 0.354(6) 0.09(3) Uani 1 1 d D U . . .
H3'C H 1.486596 0.531334 0.354592 0.103 Uiso 1 1 calc DR U . . .
H3'D H 1.438363 0.722243 0.301591 0.103 Uiso 1 1 calc DR U . . .
C4' C 1.577(6) 0.783(13) 0.352(6) 0.07(2) Uani 1 1 d D U . . .
H4'A H 1.572436 0.923536 0.374144 0.084 Uiso 1 1 calc R U . . .
H4'B H 1.594168 0.787701 0.289183 0.084 Uiso 1 1 calc R U . . .
C5' C 1.653(8) 0.670(17) 0.411(8) 0.08(3) Uani 1 1 d D U . . .
H5'A H 1.652777 0.523842 0.396050 0.099 Uiso 1 1 calc R U . . .
H5'B H 1.644403 0.687152 0.475687 0.099 Uiso 1 1 calc R U . . .
C6' C 1.742(9) 0.77(2) 0.385(7) 0.09(3) Uani 1 1 d D U . . .
H6'A H 1.764825 0.700234 0.332693 0.106 Uiso 1 1 calc R U . . .
H6'B H 1.726682 0.912926 0.364884 0.106 Uiso 1 1 calc R U . . .


_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
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C7' C8' 1.51(3) . ?
C7' N3' 1.46(3) . ?
Cd1 N1 2.29(5) . ?
Cd1 O4 2.32(7) . ?
Cd1 O3 2.59(7) . ?
Cd1 N2 2.29(4) . ?
Cd1 O1 2.49(10) . ?
Cd1 N3 2.28(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.46(4) . ?
O4 N5 1.20(3) . ?
O3 N4 1.20(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C6 1.46(5) . ?
O1 N4 1.20(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C7 1.46(4) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.51(3) . ?
N5 O6 1.20(3) . ?
N5 O5 1.20(3) . ?
N4 O2 1.20(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.51(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.50(2) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.51(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.50(3) 2 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.51(3) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C4 1.51(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C9' 1.51(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C9' C8' 1.51(2) . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?
N3' H3'A 0.8900 . ?
N3' H3'B 0.8900 . ?
N3' Cd1' 2.28(5) . ?
Cd1' O4' 2.72(7) . ?
Cd1' O1' 2.53(10) . ?
Cd1' N2' 2.29(5) . ?
Cd1' N1' 2.28(5) . ?
O4' N5' 1.20(3) . ?
O1' N4' 1.20(3) . ?
N2' H2'A 0.8900 . ?
N2' H2'B 0.8900 . ?
N2' C6' 1.40(3) 2_846 ?
N1' H1'A 0.8900 . ?
N1' H1'B 0.8900 . ?
N1' C1' 1.45(4) . ?
N5' O6' 1.20(3) . ?
N5' O5' 1.20(3) . ?
N4' O3' 1.20(3) . ?
N4' O2' 1.20(3) . ?
C1' H1'C 0.9700 . ?
C1' H1'D 0.9700 . ?
C1' C2' 1.50(3) . ?
C2' H2'C 0.9700 . ?
C2' H2'D 0.9700 . ?
C2' C3' 1.50(3) . ?
C3' H3'C 0.9700 . ?
C3' H3'D 0.9700 . ?
C3' C4' 1.50(3) . ?
C4' H4'A 0.9700 . ?
C4' H4'B 0.9700 . ?
C4' C5' 1.50(3) . ?
C5' H5'A 0.9700 . ?
C5' H5'B 0.9700 . ?
C5' C6' 1.50(3) . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?

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
H7'A C7' H7'B 107.2 . . ?
C8' C7' H7'A 107.8 . . ?
C8' C7' H7'B 107.8 . . ?
N3' C7' H7'A 107.8 . . ?
N3' C7' H7'B 107.8 . . ?
N3' C7' C8' 118(9) . . ?
N1 Cd1 O3 79(3) . . ?
N1 Cd1 N2 118(5) . . ?
N1 Cd1 O1 88(4) . . ?
O4 Cd1 N1 91(4) . . ?
O4 Cd1 O3 158(4) . . ?
O4 Cd1 N2 88(3) . . ?
O4 Cd1 O1 153(3) . . ?
O4 Cd1 N3 81(4) . . ?
N2 Cd1 O3 80(3) . . ?
N2 Cd1 O1 117(4) . . ?
O1 Cd1 O3 48.1(16) . . ?
N3 Cd1 N1 136(3) . . ?
N3 Cd1 O3 120(4) . . ?
N3 Cd1 N2 105(4) . . ?
N3 Cd1 O1 80(4) . . ?
Cd1 N1 H1A 108.1 . . ?
Cd1 N1 H1B 108.1 . . ?
H1A N1 H1B 107.3 . . ?
C1 N1 Cd1 117(5) . . ?
C1 N1 H1A 108.1 . . ?
C1 N1 H1B 108.1 . . ?
N5 O4 Cd1 128(4) . . ?
N4 O3 Cd1 93(4) . . ?
Cd1 N2 H2A 109.1 . . ?
Cd1 N2 H2B 109.1 . . ?
H2A N2 H2B 107.9 . . ?
C6 N2 Cd1 112(7) . . ?
C6 N2 H2A 109.1 . . ?
C6 N2 H2B 109.1 . . ?
N4 O1 Cd1 98(3) . . ?
Cd1 N3 H3A 107.8 . . ?
Cd1 N3 H3B 107.8 . . ?
H3A N3 H3B 107.1 . . ?
C7 N3 Cd1 118(6) . . ?
C7 N3 H3A 107.8 . . ?
C7 N3 H3B 107.8 . . ?
N1 C1 H1C 108.7 . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 C2 114(8) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.7 . . ?
C2 C1 H1D 108.7 . . ?
O4 N5 O5 119(2) . . ?
O6 N5 O4 121(3) . . ?
O6 N5 O5 120(2) . . ?
O3 N4 O1 119(2) . . ?
O3 N4 O2 121(2) . . ?
O1 N4 O2 120(2) . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 C5 111(10) . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
N3 C7 H7A 110.4 . . ?
N3 C7 H7B 110.4 . . ?
N3 C7 C8 106(10) . . ?
H7A C7 H7B 108.6 . . ?
C8 C7 H7A 110.4 . . ?
C8 C7 H7B 110.4 . . ?
C1 C2 H2C 107.5 . . ?
C1 C2 H2D 107.5 . . ?
H2C C2 H2D 107.0 . . ?
C3 C2 C1 119(10) . . ?
C3 C2 H2C 107.5 . . ?
C3 C2 H2D 107.5 . . ?
C6 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
C4 C5 C6 106(10) 2 . ?
C4 C5 H5A 110.6 2 . ?
C4 C5 H5B 110.6 2 . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C7 C8 C9 109(10) . . ?
H8A C8 H8B 108.3 . . ?
C9 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
C2 C3 H3C 107.0 . . ?
C2 C3 H3D 107.0 . . ?
C2 C3 C4 121(9) . . ?
H3C C3 H3D 106.8 . . ?
C4 C3 H3C 107.0 . . ?
C4 C3 H3D 107.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 C9' 111(8) . . ?
H9A C9 H9B 108.1 . . ?
C9' C9 H9A 109.5 . . ?
C9' C9 H9B 109.5 . . ?
C5 C4 C3 114(8) 2_545 . ?
C5 C4 H4A 108.7 2_545 . ?
C5 C4 H4B 108.7 2_545 . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C9 C9' H9'A 110.0 . . ?
C9 C9' H9'B 110.0 . . ?
H9'A C9' H9'B 108.3 . . ?
C8' C9' C9 109(10) . . ?
C8' C9' H9'A 110.0 . . ?
C8' C9' H9'B 110.0 . . ?
C7' C8' H8'A 109.1 . . ?
C7' C8' H8'B 109.1 . . ?
C9' C8' C7' 112(9) . . ?
C9' C8' H8'A 109.1 . . ?
C9' C8' H8'B 109.1 . . ?
H8'A C8' H8'B 107.8 . . ?
C7' N3' H3'A 109.3 . . ?
C7' N3' H3'B 109.3 . . ?
C7' N3' Cd1' 112(7) . . ?
H3'A N3' H3'B 107.9 . . ?
Cd1' N3' H3'A 109.3 . . ?
Cd1' N3' H3'B 109.3 . . ?
N3' Cd1' O4' 71(4) . . ?
N3' Cd1' O1' 90(4) . . ?
N3' Cd1' N2' 109(5) . . ?
O1' Cd1' O4' 156(3) . . ?
N2' Cd1' O4' 84(4) . . ?
N2' Cd1' O1' 117(4) . . ?
N1' Cd1' N3' 148(3) . . ?
N1' Cd1' O4' 100(3) . . ?
N1' Cd1' O1' 88(4) . . ?
N1' Cd1' N2' 100(5) . . ?
N5' O4' Cd1' 107(4) . . ?
N4' O1' Cd1' 103(4) . . ?
Cd1' N2' H2'A 103.7 . . ?
Cd1' N2' H2'B 103.7 . . ?
H2'A N2' H2'B 105.4 . . ?
C6' N2' Cd1' 134(9) 2_846 . ?
C6' N2' H2'A 103.7 2_846 . ?
C6' N2' H2'B 103.7 2_846 . ?
Cd1' N1' H1'A 106.3 . . ?
Cd1' N1' H1'B 106.3 . . ?
H1'A N1' H1'B 106.4 . . ?
C1' N1' Cd1' 124(5) . . ?
C1' N1' H1'A 106.3 . . ?
C1' N1' H1'B 106.3 . . ?
O4' N5' O6' 120(2) . . ?
O4' N5' O5' 120(2) . . ?
O5' N5' O6' 120(2) . . ?
O1' N4' O3' 120(2) . . ?
O1' N4' O2' 120(2) . . ?
O3' N4' O2' 120(2) . . ?
N1' C1' H1'C 111.5 . . ?
N1' C1' H1'D 111.5 . . ?
N1' C1' C2' 101(9) . . ?
H1'C C1' H1'D 109.3 . . ?
C2' C1' H1'C 111.5 . . ?
C2' C1' H1'D 111.5 . . ?
C1' C2' H2'C 108.2 . . ?
C1' C2' H2'D 108.2 . . ?
C1' C2' C3' 116(8) . . ?
H2'C C2' H2'D 107.4 . . ?
C3' C2' H2'C 108.2 . . ?
C3' C2' H2'D 108.3 . . ?
C2' C3' H3'C 111.3 . . ?
C2' C3' H3'D 111.3 . . ?
H3'C C3' H3'D 109.2 . . ?
C4' C3' C2' 102(9) . . ?
C4' C3' H3'C 111.3 . . ?
C4' C3' H3'D 111.3 . . ?
C3' C4' H4'A 109.2 . . ?
C3' C4' H4'B 109.2 . . ?
C3' C4' C5' 112(7) . . ?
H4'A C4' H4'B 107.9 . . ?
C5' C4' H4'A 109.2 . . ?
C5' C4' H4'B 109.2 . . ?
C4' C5' H5'A 111.2 . . ?
C4' C5' H5'B 111.2 . . ?
C4' C5' C6' 103(8) . . ?
H5'A C5' H5'B 109.2 . . ?
C6' C5' H5'A 111.2 . . ?
C6' C5' H5'B 111.2 . . ?
N2' C6' C5' 116(10) 2_856 . ?
N2' C6' H6'A 108.3 2_856 . ?
N2' C6' H6'B 108.3 2_856 . ?
C5' C6' H6'A 108.3 . . ?
C5' C6' H6'B 108.3 . . ?
H6'A C6' H6'B 107.4 . . ?

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
Cd1 N1 C1 C2 -171(7) . . . . ?
Cd1 O4 N5 O6 149(6) . . . . ?
Cd1 O4 N5 O5 -28(8) . . . . ?
Cd1 O3 N4 O1 11(6) . . . . ?
Cd1 O3 N4 O2 -170(6) . . . . ?
Cd1 N2 C6 C5 77(9) . . . . ?
Cd1 O1 N4 O3 -11(6) . . . . ?
Cd1 O1 N4 O2 169(6) . . . . ?
Cd1 N3 C7 C8 177(7) . . . . ?
N1 C1 C2 C3 49(14) . . . . ?
N2 C6 C5 C4 -177(7) . . . 2 ?
N3 C7 C8 C9 -125(7) . . . . ?
C1 C2 C3 C4 175(9) . . . . ?
C7 C8 C9 C9' -170(9) . . . . ?
C2 C3 C4 C5 -75(12) . . . 2_545 ?
C8 C9 C9' C8' 169(8) . . . . ?
C9 C9' C8' C7' -175(9) . . . . ?
C8' C7' N3' Cd1' 172(8) . . . . ?
N3' C7' C8' C9' 172(10) . . . . ?
Cd1' O4' N5' O6' -147(6) . . . . ?
Cd1' O4' N5' O5' 30(6) . . . . ?
Cd1' O1' N4' O3' 15(8) . . . . ?
Cd1' O1' N4' O2' -168(6) . . . . ?
Cd1' N1' C1' C2' 176(6) . . . . ?
N1' C1' C2' C3' -44(12) . . . . ?
C1' C2' C3' C4' -161(9) . . . . ?
C2' C3' C4' C5' 81(10) . . . . ?
C3' C4' C5' C6' 170(8) . . . . ?
C4' C5' C6' N2' 149(11) . . . 2_856 ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999965 0.00000000 0.00083095
omega rotation goniometer -1 . -0.86822000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.33501000 -0.76655342 0.00000000
0.64218054
phi rotation goniometer -1 kappa . 0.00009338 0.00000000 1.00000000
theta rotation goniometer -1 . -0.81978000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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 4.013
_oxdiff_exptl_absorpt_empirical_full_min 0.408
####################################################################### 
# 
# 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_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262367'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.334 Report
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT026_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        24% Check
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT029_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.381 Why?
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.53 Note
RESPONSE: The data/parameter ratio is affected by the access 
limits of the DAC.
;
_vrf_PLAT341_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.065 Ang.
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT911_0_4_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        199 Report
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_audit_creation_date             2023-03-07
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2 Cu F8 N6'
_chemical_formula_weight         551.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4H9.5B0.5Cu0.3F2N1.5
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.19(3)
_cell_length_b                   13.731(6)
_cell_length_c                   26.844(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4862(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    267
_cell_measurement_temperature    293.01(10)
_cell_measurement_theta_max      28.9480
_cell_measurement_theta_min      3.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
21 0 27 0.1000
0 14 -43 0.1000
0 -14 43 0.1000
-21 0 27 0.1000
13 22 0 0.1000
-13 -22 0 0.1000

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.07
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.375     0.454
         range of gasket transmission (min-max)           0.886     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 300.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Absorption coeff of pressure medium =   0.00 mm-1
;
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
21.1589 -0.2619 27.1777 1.1282 0.5116 -0.5242
-0.1531 14.1107 -43.0600 -0.2933 -1.2895 -0.2887
0.1531 -14.1107 43.0600 0.2933 1.2895 0.2887
-21.1282 0.1413 26.8040 -1.0413 0.8373 0.0653
12.8868 21.8982 -0.0015 0.3194 -0.4392 -1.2103
-12.8868 -21.8982 0.0015 -0.3194 0.4392 1.2103

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3341
_diffrn_reflns_av_unetI/netI     0.8568
_diffrn_reflns_Laue_measured_fraction_full 0.381
_diffrn_reflns_Laue_measured_fraction_max 0.252
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            1551
_diffrn_reflns_point_group_measured_fraction_full 0.381
_diffrn_reflns_point_group_measured_fraction_max 0.252
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.573
_diffrn_reflns_theta_min         3.126
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.381
_diffrn_measured_fraction_theta_max 0.252
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.40(2) GPa
 (400000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.40   0.85   35.00   0.00 -30.00   0.00    --    64
  2  φ    140.00 199.50   0.85   35.00   0.00 -30.00   0.00    --    70
  3  φ    160.00 216.95   0.85   35.00   0.00  30.00   0.00    --    67
  4  φ    -20.00  34.40   0.85   35.00   0.00  30.00   0.00    --    64
  5  ω      4.40  23.95   0.85   35.00    --   30.00  39.46 -16.00   23
  6  ω      4.40  23.95   0.85   35.00    --   30.00  39.46 164.00   23
  7  ω    -50.00   9.50   0.85   35.00    --  -30.00  39.46 167.10   70
  8  ω    -50.00   9.50   0.85   35.00    --  -30.00  39.46 -12.90   70
  9  ω    -63.00  -8.60   0.85   35.00    --  -30.00  81.40 -33.00   64
 10  ω    -63.00  -8.60   0.85   35.00    --  -30.00  81.40 147.00   64
 11  ω     -3.10  11.35   0.85   35.00    --   30.00  81.40 147.00   17
 12  ω     -3.10  11.35   0.85   35.00    --   30.00  81.40 -33.00   17
 13  ω    -34.00 -18.70   0.85   35.00    --   30.00 134.60 -60.00   18
 14  ω    -34.00 -18.70   0.85   35.00    --   30.00 134.60 120.00   18
 15  ω    -90.00 -36.45   0.85   35.00    --  -30.00 134.60 120.00   63
 16  ω    -90.00 -36.45   0.85   35.00    --  -30.00 134.60 -60.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0511417000
_diffrn_orient_matrix_UB_12      -0.0155127000
_diffrn_orient_matrix_UB_13      0.0015455000
_diffrn_orient_matrix_UB_21      -0.0080688000
_diffrn_orient_matrix_UB_22      -0.0153077000
_diffrn_orient_matrix_UB_23      0.0249598000
_diffrn_orient_matrix_UB_31      -0.0143113000
_diffrn_orient_matrix_UB_32      -0.0468488000
_diffrn_orient_matrix_UB_33      -0.0085965000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                123
_reflns_number_total             516
_reflns_odcompleteness_completeness 38.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         516
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.3838
_refine_ls_R_factor_gt           0.0887
_refine_ls_restrained_S_all      0.826
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0620P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.2732
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N2, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, B1, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_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
Cu1 Cu 0.375000 0.375000 0.375000 0.071(5) Uani 1 4 d S T P . .
N1 N 0.4824(18) 0.3859(10) 0.4277(5) 0.080(6) Uani 1 1 d . U . . .
H1A H 0.523876 0.433607 0.418362 0.096 Uiso 1 1 calc R U . . .
H1B H 0.451667 0.405976 0.455377 0.096 Uiso 1 1 calc R U . . .
C3 C 0.696(5) 0.242(3) 0.4894(16) 0.158(18) Uani 1 1 d . . . . .
H3A H 0.702403 0.195748 0.462280 0.190 Uiso 1 1 calc R U . . .
H3B H 0.656717 0.210606 0.515259 0.190 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.556(2) 0.375000 0.129(11) Uani 1 2 d S TU P . .
C1 C 0.548(3) 0.3009(17) 0.4421(8) 0.100(12) Uani 1 1 d . . . . .
H1C H 0.507669 0.255218 0.461173 0.120 Uiso 1 1 calc R U . . .
H1D H 0.570011 0.267941 0.411974 0.120 Uiso 1 1 calc R U . . .
C2 C 0.636(4) 0.3265(17) 0.4706(9) 0.137(14) Uani 1 1 d . . . . .
H2A H 0.613993 0.365290 0.498837 0.164 Uiso 1 1 calc R U . . .
H2B H 0.679146 0.367031 0.450138 0.164 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.746(2) 0.375000 0.182(16) Uani 1 2 d S TU P . .
H5A H 0.313358 0.769034 0.360191 0.273 Uiso 0.5 1 calc R U P A -1
H5B H 0.431921 0.769034 0.356172 0.273 Uiso 0.5 1 calc R U P A -1
H5C H 0.379722 0.769034 0.408637 0.273 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.633(3) 0.375000 0.133(12) Uani 1 2 d S TU P . .
B1 B 0.625000 0.125000 0.304(2) 0.157(16) Uani 1 2 d S T P . .
F1 F 0.669(3) 0.1905(11) 0.3441(5) 0.27(2) Uani 1 1 d . . . . .
F2 F 0.560(3) 0.1704(12) 0.2879(6) 0.210(13) 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
Cu1 N1 2.008(18) 12 ?
Cu1 N1 2.008(18) 14 ?
Cu1 N1 2.008(18) 7 ?
Cu1 N1 2.008(18) . ?
Cu1 N2 2.48(3) 14 ?
Cu1 N2 2.48(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.50(3) . ?
C3 C3 1.54(11) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.50(5) . ?
N2 C4 1.07(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.43(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 0.9964 . ?
C5 H5B 0.9964 . ?
C5 H5C 0.9964 . ?
C5 C4 1.54(4) . ?
B1 F1 1.51(5) 2_655 ?
B1 F1 1.51(5) . ?
B1 F2 1.15(3) . ?
B1 F2 1.15(3) 2_655 ?

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 Cu1 N1 90.4(11) 12 7 ?
N1 Cu1 N1 90.2(11) 7 . ?
N1 Cu1 N1 171.5(8) 12 . ?
N1 Cu1 N1 90.3(11) 12 14 ?
N1 Cu1 N1 171.5(8) 7 14 ?
N1 Cu1 N1 90.4(11) 14 . ?
N1 Cu1 N2 85.7(4) . . ?
N1 Cu1 N2 85.7(4) 12 . ?
N1 Cu1 N2 94.3(4) . 14 ?
N1 Cu1 N2 85.7(4) 7 14 ?
N1 Cu1 N2 94.3(4) 14 . ?
N1 Cu1 N2 85.7(4) 14 14 ?
N1 Cu1 N2 94.3(4) 12 14 ?
N1 Cu1 N2 94.3(4) 7 . ?
N2 Cu1 N2 180.0 14 . ?
Cu1 N1 H1A 106.8 . . ?
Cu1 N1 H1B 106.9 . . ?
H1A N1 H1B 106.7 . . ?
C1 N1 Cu1 122.0(14) . . ?
C1 N1 H1A 106.8 . . ?
C1 N1 H1B 106.9 . . ?
C3 C3 H3A 107.0 29_656 . ?
C3 C3 H3B 107.5 29_656 . ?
H3A C3 H3B 106.8 . . ?
C2 C3 C3 120(4) . 29_656 ?
C2 C3 H3A 107.2 . . ?
C2 C3 H3B 107.2 . . ?
C4 N2 Cu1 180.000(11) . . ?
N1 C1 H1C 108.6 . . ?
N1 C1 H1D 108.7 . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 N1 114(2) . . ?
C2 C1 H1C 108.5 . . ?
C2 C1 H1D 108.9 . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C1 C2 C3 115(3) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
H5A C5 H5B 105.7 . . ?
H5A C5 H5C 105.7 . . ?
H5B C5 H5C 105.7 . . ?
C4 C5 H5A 113.0 . . ?
C4 C5 H5B 113.0 . . ?
C4 C5 H5C 113.0 . . ?
N2 C4 C5 180.000(16) . . ?
F1 B1 F1 90(3) . 2_655 ?
F2 B1 F1 108(3) . 2_655 ?
F2 B1 F1 103(2) 2_655 2_655 ?
F2 B1 F1 108(3) 2_655 . ?
F2 B1 F1 103(2) . . ?
F2 B1 F2 135(7) 2_655 . ?

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
Cu1 N1 C1 C2 165(3) . . . . ?
N1 C1 C2 C3 174(3) . . . . ?
C3 C3 C2 C1 167(6) 29_656 . . . ?

_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 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.755
####################################################################### 
# 
# 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_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262366'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.335 Report
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT029_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.395 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT088_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.85 Note
RESPONSE: The data/parameter ratio is affected by the access
 limits of the DAC.
;
_vrf_PLAT026_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        34% Check
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT341_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.035 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_0_15_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        295 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2021-08-18
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2 Cu F8 N6'
_chemical_formula_weight         551.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         C5.8H13.8B0.7Cu0.4F2.9N2.2
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   12.99(4)
_cell_length_b                   13.946(12)
_cell_length_c                   27.191(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4924(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    339
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8680
_cell_measurement_theta_min      4.9530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.07
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3349
_diffrn_reflns_av_unetI/netI     0.2696
_diffrn_reflns_Laue_measured_fraction_full 0.395
_diffrn_reflns_Laue_measured_fraction_max 0.353
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            2590
_diffrn_reflns_point_group_measured_fraction_full 0.395
_diffrn_reflns_point_group_measured_fraction_max 0.353
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.721
_diffrn_reflns_theta_min         5.173
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.395
_diffrn_measured_fraction_theta_max 0.353
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.15(2) GPa
 (150000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     68

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     75

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  216.80   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     71

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     68

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 60

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 60

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 75

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 75

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 70

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 70

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    7.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 33

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    7.40   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 33

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -23.80   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 24
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0523384000
_diffrn_orient_matrix_UB_12      0.0167146000
_diffrn_orient_matrix_UB_13      0.0013544000
_diffrn_orient_matrix_UB_21      -0.0080958000
_diffrn_orient_matrix_UB_22      0.0147896000
_diffrn_orient_matrix_UB_23      0.0243557000
_diffrn_orient_matrix_UB_31      0.0167798000
_diffrn_orient_matrix_UB_32      -0.0449147000
_diffrn_orient_matrix_UB_33      0.0084142000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                156
_reflns_number_total             462
_reflns_odcompleteness_completeness 40.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         462
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.2220
_refine_ls_R_factor_gt           0.0921
_refine_ls_restrained_S_all      0.827
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1169P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2579
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3_$1-C3
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C4 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1, Cu1, N2, C1, C4, C2, C5, C3, F1, B1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_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
Cu1 Cu 0.375000 0.375000 0.375000 0.063(4) Uani 1 4 d S T P . .
N1 N 0.4849(14) 0.3859(7) 0.4282(3) 0.070(8) Uani 1 1 d . U . . .
H1A H 0.528039 0.431847 0.418662 0.083 Uiso 1 1 calc R U . . .
H1B H 0.453469 0.407359 0.455114 0.083 Uiso 1 1 calc R U . . .
C3 C 0.7037(14) 0.2433(13) 0.4864(7) 0.089(10) Uani 1 1 d D U . . .
H3A H 0.658584 0.203864 0.506396 0.107 Uiso 1 1 calc R U . . .
H3B H 0.721161 0.205712 0.457561 0.107 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.5534(14) 0.375000 0.095(14) Uani 1 2 d S TU P . .
C1 C 0.549(3) 0.3038(10) 0.4436(5) 0.073(9) Uani 1 1 d . U . . .
H1C H 0.508059 0.262665 0.464692 0.087 Uiso 1 1 calc R U . . .
H1D H 0.567179 0.266984 0.414590 0.087 Uiso 1 1 calc R U . . .
C2 C 0.640(3) 0.3286(13) 0.4687(6) 0.086(9) Uani 1 1 d . U . . .
H2A H 0.622156 0.367759 0.496868 0.104 Uiso 1 1 calc R U . . .
H2B H 0.682452 0.367335 0.447024 0.104 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.7349(16) 0.375000 0.115(10) Uani 1 2 d S TU P . .
H5A H 0.352888 0.757824 0.406567 0.173 Uiso 0.5 1 calc R U P A -1
H5B H 0.328811 0.757824 0.350072 0.173 Uiso 0.5 1 calc R U P A -1
H5C H 0.443301 0.757824 0.368361 0.173 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.6348(17) 0.375000 0.083(7) Uani 1 2 d S TU P . .
B1 B 0.625000 0.125000 0.3128(12) 0.153(14) Uani 1 2 d S T P . .
F1 F 0.657(2) 0.1898(9) 0.3419(4) 0.249(15) Uani 1 1 d . . . . .
F2 F 0.562(2) 0.1677(10) 0.2850(3) 0.224(12) 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
Cu1 N1 2.038(14) 12 ?
Cu1 N1 2.038(14) . ?
Cu1 N1 2.038(14) 7 ?
Cu1 N1 2.038(14) 14 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.47(2) . ?
C3 C3 1.43(2) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.53(3) . ?
N2 C4 1.14(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.41(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 1.0783 . ?
C5 H5B 1.0783 . ?
C5 H5C 1.0783 . ?
C5 C4 1.40(3) . ?
B1 F1 1.27(2) 2_655 ?
B1 F1 1.27(2) . ?
B1 F2 1.26(2) 2_655 ?
B1 F2 1.26(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
N1 Cu1 N1 89.6(9) 12 7 ?
N1 Cu1 N1 89.6(9) 14 . ?
N1 Cu1 N1 91.1(9) 7 . ?
N1 Cu1 N1 91.1(9) 12 14 ?
N1 Cu1 N1 171.5(6) 7 14 ?
N1 Cu1 N1 171.5(6) 12 . ?
Cu1 N1 H1A 106.7 . . ?
Cu1 N1 H1B 106.7 . . ?
H1A N1 H1B 106.6 . . ?
C1 N1 Cu1 122.6(10) . . ?
C1 N1 H1A 106.5 . . ?
C1 N1 H1B 106.8 . . ?
C3 C3 H3A 107.0 29_656 . ?
C3 C3 H3B 107.0 29_656 . ?
C3 C3 C2 121(2) 29_656 . ?
H3A C3 H3B 106.8 . . ?
C2 C3 H3A 107.0 . . ?
C2 C3 H3B 107.0 . . ?
N1 C1 H1C 108.4 . . ?
N1 C1 H1D 108.6 . . ?
H1C C1 H1D 107.5 . . ?
C2 C1 N1 114.9(14) . . ?
C2 C1 H1C 108.6 . . ?
C2 C1 H1D 108.7 . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C1 C2 C3 114.6(16) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
H5A C5 H5B 93.9 . . ?
H5A C5 H5C 93.9 . . ?
H5B C5 H5C 93.9 . . ?
C4 C5 H5A 122.5 . . ?
C4 C5 H5B 122.5 . . ?
C4 C5 H5C 122.5 . . ?
N2 C4 C5 180.000(11) . . ?
F1 B1 F1 103(3) 2_655 . ?
F2 B1 F1 119.4(17) 2_655 . ?
F2 B1 F1 119.4(17) . 2_655 ?
F2 B1 F1 104.6(10) . . ?
F2 B1 F1 104.6(10) 2_655 2_655 ?
F2 B1 F2 107(3) . 2_655 ?

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
Cu1 N1 C1 C2 161.2(17) . . . . ?
N1 C1 C2 C3 177.5(14) . . . . ?
C3 C3 C2 C1 -178(3) 29_656 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
