# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046202'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2020-11-24 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT029_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.557 Why?
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT084_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.56 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT342_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.10063 Ang.
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT082_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: High R1 Value ..................................       0.18 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT088_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.04 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT149_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.07 Degree
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle. Additionally, in this case, the crystal loses its crystallinity which further reduces the amount of information.
;
_vrf_PLAT250_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.1 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle. Additionally, in this case, the crystal loses its crystallinity which further reduces the amount of information.
;
_vrf_PLAT910_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT911_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.333        127 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT930_Cd(BDC)(AZPY)DMF_3_66_GPa_MEW 
;
PROBLEM: FCF-based   Twin Law ( 1 0 1)[ 5 0 4] Est.d BASF       0.24 Check
RESPONSE: For this compound, we observed the phase transition from phase \a of orthorhombic space-group Cmce to phase \b of monoclinic P21/n. This phase transition may entail this alert.
;
# Added during the CSD deposition process: Tuesday 24 November 2020 05:18 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        Cd(BDC)(AZPY)*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_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                   11.362(6)
_cell_length_b                   13.31(3)
_cell_length_c                   13.269(8)
_cell_angle_alpha                90
_cell_angle_beta                 115.07(7)
_cell_angle_gamma                90
_cell_volume                     1818(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    467
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.5920
_cell_measurement_theta_min      4.2290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.076
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1420
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.557
_diffrn_reflns_Laue_measured_fraction_max 0.557
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2771
_diffrn_reflns_point_group_measured_fraction_full 0.557
_diffrn_reflns_point_group_measured_fraction_max 0.557
_diffrn_reflns_theta_full        13.700
_diffrn_reflns_theta_max         13.700
_diffrn_reflns_theta_min         4.246
_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 0.557
_diffrn_measured_fraction_theta_max 0.557
_diffrn_measurement_details      
;
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      -0.0029161000
_diffrn_orient_matrix_UB_12      -0.0510012000
_diffrn_orient_matrix_UB_13      -0.0161370000
_diffrn_orient_matrix_UB_21      0.0688784000
_diffrn_orient_matrix_UB_22      -0.0018882000
_diffrn_orient_matrix_UB_23      0.0229826000
_diffrn_orient_matrix_UB_31      0.0018543000
_diffrn_orient_matrix_UB_32      -0.0149455000
_diffrn_orient_matrix_UB_33      0.0520072000
_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                208
_reflns_number_total             314
_reflns_special_details          
;
Data were collected at room temperature and pressure of 3.66(2) GPa (3660000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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 1.3 (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         0.651
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         314
_refine_ls_number_restraints     385
_refine_ls_R_factor_all          0.2192
_refine_ls_R_factor_gt           0.1784
_refine_ls_restrained_S_all      0.712
_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)+(0.5000P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4696
_refine_ls_wR_factor_ref         0.5564
_refine_special_details          ?
_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 -0.0574(7) 0.0936(13) 0.0693(6) 0.196(4) Uani 1 1 d D . . . .
O4 O 0.076(5) 0.110(6) -0.011(6) 0.196(4) Uani 1 1 d D U . . .
C2' C 0.110(6) 0.037(9) 0.326(6) 0.196(4) Uani 1 1 d G U . . .
H2' H 0.035967 0.005464 0.323023 0.235 Uiso 1 1 calc R U . . .
C3' C 0.211(7) 0.061(10) 0.428(5) 0.196(4) Uani 1 1 d G U . . .
H3' H 0.203909 0.046119 0.493245 0.235 Uiso 1 1 calc R U . . .
C4' C 0.322(6) 0.108(10) 0.431(5) 0.196(4) Uani 1 1 d G U . . .
C5' C 0.333(6) 0.130(9) 0.333(7) 0.196(4) Uani 1 1 d G U . . .
H5' H 0.407473 0.161103 0.335860 0.235 Uiso 1 1 calc R U . . .
C6' C 0.232(8) 0.106(9) 0.231(5) 0.196(4) Uani 1 1 d G U . . .
H6' H 0.239532 0.120448 0.165637 0.235 Uiso 1 1 calc R U . . .
N1' N 0.121(6) 0.059(9) 0.227(5) 0.196(4) Uani 1 1 d G U . . .
C4 C 0.158(4) 0.222(4) -0.096(4) 0.196(4) Uani 1 1 d DG U . . .
C5 C 0.207(5) 0.160(5) -0.154(5) 0.196(4) Uani 1 1 d DG U . . .
H5 H 0.202449 0.091009 -0.149347 0.235 Uiso 1 1 calc R U . . .
C6 C 0.264(5) 0.203(5) -0.218(4) 0.196(4) Uani 1 1 d DG U . . .
H6 H 0.297223 0.161598 -0.256915 0.235 Uiso 1 1 calc R U . . .
C1 C 0.272(5) 0.307(5) -0.225(4) 0.196(4) Uani 1 1 d DG U . . .
C2 C 0.222(6) 0.368(5) -0.168(5) 0.196(4) Uani 1 1 d DG U . . .
H2 H 0.227277 0.437545 -0.172247 0.235 Uiso 1 1 calc R U . . .
C3 C 0.166(5) 0.326(4) -0.103(4) 0.196(4) Uani 1 1 d DG U . . .
H3 H 0.132503 0.366958 -0.064678 0.235 Uiso 1 1 calc R U . . .
O3 O 0.021(5) 0.203(5) -0.010(5) 0.196(4) Uani 1 1 d D U . . .
N2' N 0.441(6) 0.088(7) 0.541(6) 0.196(4) Uani 1 1 d . U . . .
N2" N 0.400(6) 0.064(11) 0.623(6) 0.196(4) Uani 1 1 d . U . . .
C4" C 0.527(5) 0.079(9) 0.725(4) 0.196(4) Uani 1 1 d G U . . .
C3" C 0.550(5) 0.011(8) 0.811(5) 0.196(4) Uani 1 1 d G U . . .
H3" H 0.490012 -0.039668 0.802334 0.235 Uiso 1 1 calc R U . . .
C2" C 0.664(5) 0.017(6) 0.908(5) 0.196(4) Uani 1 1 d DG U . . .
H2" H 0.679220 -0.028591 0.965404 0.235 Uiso 1 1 calc R U . . .
N1" N 0.754(4) 0.092(5) 0.921(4) 0.196(4) Uani 1 1 d G U . . .
C6" C 0.730(5) 0.161(6) 0.835(4) 0.196(4) Uani 1 1 d DG U . . .
H6" H 0.790540 0.211121 0.843286 0.235 Uiso 1 1 calc R U . . .
C5" C 0.617(6) 0.154(8) 0.737(4) 0.196(4) Uani 1 1 d G U . . .
H5" H 0.601333 0.200045 0.680213 0.235 Uiso 1 1 calc R U . . .
C7 C 0.359(7) 0.351(6) -0.271(7) 0.196(4) Uani 1 1 d D U . . .
O2 O 0.394(5) 0.305(9) -0.331(5) 0.196(4) Uani 1 1 d D U . . .
C8 C 0.086(9) 0.181(5) -0.046(7) 0.196(4) Uani 1 1 d D U . . .
O1 O 0.324(5) 0.417(6) -0.339(5) 0.196(4) 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 O4 2.20(5) . ?
Cd1 N1' 2.26(6) . ?
Cd1 O3 2.20(5) . ?
Cd1 N1" 2.22(8) 1_454 ?
Cd1 C7 2.76(6) 4_566 ?
Cd1 O2 2.12(8) 4_566 ?
Cd1 O1 2.17(5) 4_566 ?
O4 C8 1.07(7) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.53(8) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.37(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.50(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.07(7) . ?
N2' N2" 1.39(8) . ?
N2" C4" 1.52(8) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.20(7) . ?
C7 O1 1.20(7) . ?

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 N1' 87(3) . . ?
O4 Cd1 N1" 100(8) . 1_454 ?
O4 Cd1 C7 151(3) . 4_566 ?
N1' Cd1 C7 79(3) . 4_566 ?
O3 Cd1 O4 37(3) . . ?
O3 Cd1 N1' 101(3) . . ?
O3 Cd1 N1" 91(9) . 1_454 ?
O3 Cd1 C7 122(2) . 4_566 ?
N1" Cd1 N1' 167(10) 1_454 . ?
N1" Cd1 C7 100(9) 1_454 4_566 ?
O2 Cd1 O4 131(3) 4_566 . ?
O2 Cd1 N1' 85(3) 4_566 . ?
O2 Cd1 O3 98(4) 4_566 . ?
O2 Cd1 N1" 99(10) 4_566 1_454 ?
O2 Cd1 C7 24(2) 4_566 4_566 ?
O2 Cd1 O1 46(3) 4_566 4_566 ?
O1 Cd1 O4 175(2) 4_566 . ?
O1 Cd1 N1' 90(3) 4_566 . ?
O1 Cd1 O3 142(2) 4_566 . ?
O1 Cd1 N1" 84(8) 4_566 1_454 ?
O1 Cd1 C7 24.6(16) 4_566 4_566 ?
C8 O4 Cd1 121(7) . . ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 112(6) . . ?
C5' C4' N2' 122(6) . . ?
C4' C5' H5' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
N1' C6' C5' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 121(4) . . ?
C6' N1' Cd1 113(4) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C8 C4 C5 119.6(10) . . ?
C8 C4 C3 119.7(9) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C1 C6 H6 120.0 . . ?
C6 C1 C7 119.3(10) . . ?
C2 C1 C6 120.0 . . ?
C2 C1 C7 119.1(10) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 121(7) . . ?
N2" N2' C4' 109(6) . . ?
N2' N2" C4" 99(6) . . ?
C3" C4" N2" 115(7) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 125(7) . . ?
C4" C3" H3" 120.0 . . ?
C2" C3" C4" 120.00(9) . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
C3" C2" N1" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 119.8(8) . 1_656 ?
C6" N1" Cd1 120.0(8) . 1_656 ?
C6" N1" C2" 120.0 . . ?
N1" C6" H6" 120.0 . . ?
C5" C6" N1" 120.00(8) . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 158(5) . 4_665 ?
O2 C7 Cd1 47(4) . 4_665 ?
O2 C7 C1 122(5) . . ?
O1 C7 Cd1 49(3) . 4_665 ?
O1 C7 C1 122(5) . . ?
O1 C7 O2 89(7) . . ?
C7 O2 Cd1 109(6) . 4_665 ?
O4 C8 C4 139(6) . . ?
O3 C8 O4 81(10) . . ?
O3 C8 C4 140(6) . . ?
C7 O1 Cd1 106(4) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 C4 177(8) . . . . ?
Cd1 O4 C8 O3 4(9) . . . . ?
Cd1 O3 C8 O4 -4(10) . . . . ?
Cd1 O3 C8 C4 -177(8) . . . . ?
Cd1 N1" C6" C5" 174(3) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' -155(8) . . . . ?
C3' C2' N1' Cd1 -150(6) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -23(9) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" -164(8) . . . . ?
C5' C4' N2' N2" -178(8) . . . . ?
C5' C6' N1' Cd1 152(6) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 26(17) . . . . ?
C5 C4 C8 O3 -165(11) . . . . ?
C5 C6 C1 C2 0.0 . . . . ?
C5 C6 C1 C7 166(5) . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C1 C7 Cd1 75(8) . . . 4_665 ?
C6 C1 C7 O2 22(9) . . . . ?
C6 C1 C7 O1 133(8) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 155(4) . . . 4_665 ?
C1 C7 O1 Cd1 -155(4) . . . 4_665 ?
C2 C1 C7 Cd1 -119(7) . . . 4_665 ?
C2 C1 C7 O2 -172(6) . . . . ?
C2 C1 C7 O1 -61(10) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C8 O4 -163(13) . . . . ?
C3 C4 C8 O3 6(15) . . . . ?
N2' C4' C5' C6' 152(9) . . . . ?
N2' N2" C4" C3" -143(7) . . . . ?
N2' N2" C4" C5" 38(10) . . . . ?
N2" C4" C3" C2" -180(6) . . . . ?
N2" C4" C5" C6" 180(7) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 -174(3) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 -166(5) . . . . ?
O2 C7 O1 Cd1 -27(7) . . . 4_665 ?
C8 C4 C5 C6 171(5) . . . . ?
C8 C4 C3 C2 -171(5) . . . . ?
O1 C7 O2 Cd1 28(7) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 162.4 54.1 ?
2 0.500 0.500 0.000 162.4 54.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
####################################################################### 
# 
# 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_CdBDCAZPYDMF_0_3_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046198'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.455 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT088_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.22 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT342_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03142 Ang.
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT911_CdBDCAZPYDMF_0_3_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526         82 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_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      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, z-1/2'

_cell_length_a                   13.643(3)
_cell_length_b                   20.739(3)
_cell_length_c                   14.20(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4019(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1930
_cell_measurement_theta_min      3.5500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.820
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
19 -4 -4 0.0499
-3 -28 -3 0.0338
2 29 3 0.0682
-4 5 -19 0.0213
3 -6 19 0.0493
-19 5 2 0.2213

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1485
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.455
_diffrn_reflns_Laue_measured_fraction_max 0.455
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9246
_diffrn_reflns_point_group_measured_fraction_full 0.455
_diffrn_reflns_point_group_measured_fraction_max 0.455
_diffrn_reflns_theta_full        21.962
_diffrn_reflns_theta_max         21.962
_diffrn_reflns_theta_min         3.575
_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 0.455
_diffrn_measured_fraction_theta_max 0.455
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.30(2) GPa (300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      -0.0018967000
_diffrn_orient_matrix_UB_12      0.0027253000
_diffrn_orient_matrix_UB_13      -0.0496051000
_diffrn_orient_matrix_UB_21      -0.0443057000
_diffrn_orient_matrix_UB_22      0.0175847000
_diffrn_orient_matrix_UB_23      0.0036173000
_diffrn_orient_matrix_UB_31      0.0272868000
_diffrn_orient_matrix_UB_32      0.0292639000
_diffrn_orient_matrix_UB_33      0.0023938000
_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                363
_reflns_number_total             586
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         0.366
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.081
_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     139
_refine_ls_number_reflns         586
_refine_ls_number_restraints     221
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      0.882
_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)+(0.1240P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1907
_refine_special_details          ?
_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 0.000000 0.06477(7) 0.0958(3) 0.082(4) Uani 1 2 d S T P . .
O4 O 0.000000 0.4414(9) 0.433(2) 0.149(15) Uani 1 2 d DS T P . .
O3 O 0.000000 0.4850(7) 0.298(3) 0.140(16) Uani 1 2 d DS T P . .
O1 O 0.000000 0.1798(10) 0.091(3) 0.107(12) Uani 1 2 d DS T P . .
C1 C 0.000000 0.2482(9) 0.218(2) 0.089(13) Uani 1 2 d DS T P . .
C8 C 0.000000 0.4371(16) 0.348(2) 0.116(15) Uani 1 2 d DS T P . .
C2 C 0.000000 0.3044(8) 0.165(2) 0.105(14) Uani 1 2 d DS T P . .
H2 H 0.000000 0.300824 0.099861 0.126 Uiso 1 2 calc R U P . .
O2 O 0.000000 0.1360(7) 0.220(3) 0.105(12) Uani 1 2 d DS T P . .
C5 C 0.000000 0.3144(7) 0.361(2) 0.092(14) Uani 1 2 d DS T P . .
H5 H 0.000000 0.317540 0.426203 0.110 Uiso 1 2 calc R U P . .
C6 C 0.000000 0.2555(9) 0.315(2) 0.097(13) Uani 1 2 d DS T P . .
H6 H 0.000000 0.218423 0.352025 0.117 Uiso 1 2 calc R U P . .
C7 C 0.000000 0.1830(19) 0.174(3) 0.104(14) Uani 1 2 d DS T P . .
C4 C 0.000000 0.3692(11) 0.303(2) 0.112(14) Uani 1 2 d DS T P . .
C3 C 0.000000 0.3662(10) 0.205(2) 0.116(15) Uani 1 2 d DS T P . .
H3 H 0.000000 0.403142 0.167486 0.139 Uiso 1 2 calc R U P . .
C2' C 0.2159(10) 0.1075(7) 0.0192(18) 0.163(16) Uani 1 1 d G U . . .
H2' H 0.179209 0.135014 -0.018621 0.195 Uiso 1 1 calc R U . . .
N1' N 0.1691(7) 0.0642(5) 0.0787(17) 0.126(14) Uani 1 1 d G U . . .
C6' C 0.2240(10) 0.0231(6) 0.1353(18) 0.170(16) Uani 1 1 d G U . . .
H6' H 0.192641 -0.005899 0.175129 0.203 Uiso 1 1 calc R U . . .
C5' C 0.3258(9) 0.0254(7) 0.1323(19) 0.185(18) Uani 1 1 d G U . . .
H5' H 0.362515 -0.002075 0.170194 0.222 Uiso 1 1 calc R U . . .
C4' C 0.3726(7) 0.0688(7) 0.073(2) 0.177(18) Uani 1 1 d G U . . .
C3' C 0.3177(10) 0.1098(8) 0.016(2) 0.188(17) Uani 1 1 d G U . . .
H3' H 0.349087 0.138837 -0.023556 0.225 Uiso 1 1 calc R U . . .
N2' N 0.480(3) 0.0444(13) 0.085(6) 0.20(4) Uani 0.5 1 d . . P A -1
N2" N 0.480(3) 0.0965(14) 0.066(6) 0.24(5) Uani 0.5 1 d . . 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 O4 2.59(2) 10_556 ?
Cd1 O4 2.31(3) 2_554 ?
Cd1 O3 2.23(3) 10_556 ?
Cd1 O1 2.39(2) . ?
Cd1 O2 2.30(3) . ?
Cd1 C7 2.69(4) . ?
Cd1 N1' 2.320(9) . ?
Cd1 N1' 2.320(11) 11 ?
O4 C8 1.22(3) . ?
O3 C8 1.21(3) . ?
O1 C7 1.18(4) . ?
C1 C2 1.389(16) . ?
C1 C6 1.387(18) . ?
C1 C7 1.49(5) . ?
C8 C4 1.55(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.398(16) . ?
O2 C7 1.17(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(16) . ?
C5 C4 1.406(16) . ?
C6 H6 0.9300 . ?
C4 C3 1.395(19) . ?
C3 H3 0.9300 . ?
C2' H2' 0.9300 . ?
C2' N1' 1.3900 . ?
C2' C3' 1.3900 . ?
N1' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' C5' 1.3900 . ?
C5' H5' 0.9300 . ?
C5' C4' 1.3900 . ?
C4' C3' 1.3900 . ?
C4' N2' 1.56(4) . ?
C4' N2" 1.58(4) . ?
C3' H3' 0.9300 . ?
N2' N2" 1.11(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
O4 Cd1 O4 77.6(9) 2_554 10_556 ?
O4 Cd1 O1 91.5(13) 2_554 . ?
O4 Cd1 C7 117.5(8) 2_554 . ?
O4 Cd1 C7 164.9(10) 10_556 . ?
O4 Cd1 N1' 84.0(6) 2_554 . ?
O4 Cd1 N1' 84.0(13) 2_554 11 ?
O3 Cd1 O4 129.0(10) 10_556 2_554 ?
O3 Cd1 O4 51.4(12) 10_556 10_556 ?
O3 Cd1 O1 139.4(14) 10_556 . ?
O3 Cd1 O2 87.8(13) 10_556 . ?
O3 Cd1 C7 113.5(11) 10_556 . ?
O3 Cd1 N1' 93.8(11) 10_556 11 ?
O3 Cd1 N1' 93.8(4) 10_556 . ?
O1 Cd1 O4 169.2(14) . 10_556 ?
O1 Cd1 C7 26.0(8) . . ?
O2 Cd1 O4 143.2(9) . 2_554 ?
O2 Cd1 O4 139.2(11) . 10_556 ?
O2 Cd1 O1 51.7(15) . . ?
O2 Cd1 C7 25.7(8) . . ?
O2 Cd1 N1' 94.8(5) . . ?
O2 Cd1 N1' 94.8(12) . 11 ?
N1' Cd1 O4 88.7(10) 11 10_556 ?
N1' Cd1 O4 88.7(3) . 10_556 ?
N1' Cd1 O1 90.1(10) 11 . ?
N1' Cd1 O1 90.1(3) . . ?
N1' Cd1 C7 92.7(11) 11 . ?
N1' Cd1 C7 92.7(3) . . ?
N1' Cd1 N1' 168.0(18) . 11 ?
Cd1 O4 Cd1 102.4(9) 2 10_566 ?
C8 O4 Cd1 85(3) . 10_566 ?
C8 O4 Cd1 173(3) . 2 ?
C8 O3 Cd1 103(3) . 10_566 ?
C7 O1 Cd1 92(3) . . ?
C2 C1 C7 122(3) . . ?
C6 C1 C2 117(3) . . ?
C6 C1 C7 121(2) . . ?
O4 C8 C4 119(2) . . ?
O3 C8 O4 121(4) . . ?
O3 C8 C4 120(3) . . ?
C1 C2 H2 118.2 . . ?
C1 C2 C3 124(3) . . ?
C3 C2 H2 118.2 . . ?
C7 O2 Cd1 96(3) . . ?
C6 C5 H5 122.0 . . ?
C6 C5 C4 116(3) . . ?
C4 C5 H5 122.0 . . ?
C1 C6 H6 117.9 . . ?
C5 C6 C1 124(3) . . ?
C5 C6 H6 117.9 . . ?
O1 C7 Cd1 63(3) . . ?
O1 C7 C1 118(3) . . ?
C1 C7 Cd1 179(2) . . ?
O2 C7 Cd1 58(2) . . ?
O2 C7 O1 121(5) . . ?
O2 C7 C1 121(3) . . ?
C5 C4 C8 119.5(18) . . ?
C3 C4 C8 117.1(19) . . ?
C3 C4 C5 123(3) . . ?
C2 C3 H3 121.9 . . ?
C4 C3 C2 116(3) . . ?
C4 C3 H3 121.9 . . ?
N1' C2' H2' 120.0 . . ?
N1' C2' C3' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C2' N1' Cd1 121.2(7) . . ?
C2' N1' C6' 120.0 . . ?
C6' N1' Cd1 118.6(8) . . ?
N1' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C5' C4' N2' 99(2) . . ?
C5' C4' N2" 134(3) . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 140(2) . . ?
C3' C4' N2" 104(2) . . ?
N2' C4' N2" 41.5(16) . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
N2" N2' C4' 70(3) . . ?
N2' N2" C4' 68(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 O4 C8 O3 0.000(8) 10_566 . . . ?
Cd1 O4 C8 C4 180.000(8) 10_566 . . . ?
Cd1 O3 C8 O4 0.000(11) 10_566 . . . ?
Cd1 O3 C8 C4 180.000(7) 10_566 . . . ?
Cd1 O1 C7 C1 180.000(4) . . . . ?
Cd1 O1 C7 O2 0.000(4) . . . . ?
Cd1 O2 C7 O1 0.000(4) . . . . ?
Cd1 O2 C7 C1 180.000(4) . . . . ?
Cd1 N1' C6' C5' -174.7(9) . . . . ?
O4 C8 C4 C5 0.000(11) . . . . ?
O4 C8 C4 C3 180.000(9) . . . . ?
O3 C8 C4 C5 180.000(10) . . . . ?
O3 C8 C4 C3 0.000(11) . . . . ?
C1 C2 C3 C4 0.000(6) . . . . ?
C8 C4 C3 C2 180.000(6) . . . . ?
C2 C1 C6 C5 0.000(4) . . . . ?
C2 C1 C7 O1 0.000(6) . . . . ?
C2 C1 C7 O2 180.000(5) . . . . ?
C5 C4 C3 C2 0.000(4) . . . . ?
C6 C1 C2 C3 0.000(6) . . . . ?
C6 C1 C7 O1 180.000(6) . . . . ?
C6 C1 C7 O2 0.000(6) . . . . ?
C6 C5 C4 C8 180.000(7) . . . . ?
C6 C5 C4 C3 0.000(6) . . . . ?
C7 C1 C2 C3 180.000(4) . . . . ?
C7 C1 C6 C5 180.000(5) . . . . ?
C4 C5 C6 C1 0.000(3) . . . . ?
C2' N1' C6' C5' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
N1' C6' C5' C4' 0.0 . . . . ?
C6' C5' C4' C3' 0.0 . . . . ?
C6' C5' C4' N2' -171(3) . . . . ?
C6' C5' C4' N2" 163(4) . . . . ?
C5' C4' C3' C2' 0.0 . . . . ?
C5' C4' N2' N2" -153(5) . . . . ?
C5' C4' N2" N2' 39(7) . . . . ?
C3' C2' N1' Cd1 174.5(9) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' N2' N2" 39(7) . . . . ?
C3' C4' N2" N2' -156(5) . . . . ?
N2' C4' C3' C2' 167(4) . . . . ?
N2" C4' C3' C2' -168(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.250 -0.747 281.7 57.8 ?
2 0.250 0.750 -0.603 281.7 57.8 ?
3 0.750 0.250 -0.603 281.7 57.8 ?
4 0.750 0.750 -0.747 281.7 57.8 ?

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_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 2.175
_oxdiff_exptl_absorpt_empirical_full_min 0.606
####################################################################### 
# 
# 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_CdBDCAZPYDMF_0_9_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046200'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_0_9_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_0_9_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_0_9_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.453 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT088_CdBDCAZPYDMF_0_9_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.18 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT342_CdBDCAZPYDMF_0_9_GPa_MEW 
;
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_CdBDCAZPYDMF_0_9_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526        398 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C18H12CdN4O4
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                   12.132(3)
_cell_length_b                   13.893(18)
_cell_length_c                   12.591(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.69(2)
_cell_angle_gamma                90
_cell_volume                     1943(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    923
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9270
_cell_measurement_theta_min      3.5230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.831
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 2 -6 0.1685
10 -4 9 0.0946
-15 -2 14 0.0299
15 4 -14 0.0552
-1 16 10 0.0443
1 -16 -10 0.0541

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1738
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.453
_diffrn_reflns_Laue_measured_fraction_max 0.453
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8888
_diffrn_reflns_point_group_measured_fraction_full 0.453
_diffrn_reflns_point_group_measured_fraction_max 0.453
_diffrn_reflns_theta_full        21.965
_diffrn_reflns_theta_max         21.965
_diffrn_reflns_theta_min         3.014
_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 0.453
_diffrn_measured_fraction_theta_max 0.453
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.90(2) GPa (900000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      0.0005346000
_diffrn_orient_matrix_UB_12      -0.0507671000
_diffrn_orient_matrix_UB_13      -0.0059395000
_diffrn_orient_matrix_UB_21      -0.0274655000
_diffrn_orient_matrix_UB_22      0.0047945000
_diffrn_orient_matrix_UB_23      -0.0612301000
_diffrn_orient_matrix_UB_31      0.0576199000
_diffrn_orient_matrix_UB_32      0.0027425000
_diffrn_orient_matrix_UB_33      -0.0016821000
_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                574
_reflns_number_total             1077
_reflns_odcompleteness_completeness 47.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     21.92
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         1.031
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1077
_refine_ls_number_restraints     310
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.1111
_refine_ls_restrained_S_all      0.961
_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          0.2794
_refine_ls_wR_factor_ref         0.3280
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2'_$1-N2'_$2
 3 with sigma of 0.02
 O3-C8 \\sim C8-O4
 with sigma of 0.02
 C9-C7 \\sim C7-C2
 with sigma of 0.02
 C3-C2 \\sim C2-C1 \\sim C9-C1 \\sim C9-C5 \\sim C5-C4 \\sim C4-C3
 with sigma of 0.02
 O1-C7 \\sim C7-O2
 with sigma of 0.02
 C3-C8 \\sim C8-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4' \\sim C3' \\sim C2' \\sim N1' \\sim C6' \\sim C5': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C6" \\sim C5" \\sim C4" \\sim C3" \\sim C2" \\sim N1": within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N2") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O3, Cd1, N1', O4, C8, C2', C6', C4, C3', C5', C5, C3, C4', C9, C2, N2', C1,
 N2", C7, C4", O2, O1, C3", C5", C2", C6", N1"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6'), C5(H5), C9(H9), C2(H2), C3(H3),
 C3"(H3"), C2"(H2"), C6"(H6"), C5"(H5")
5.b Fitted hexagon refined as free rotating group:
 C2'(C3',C4',C5',C6',N1'), C4(C5,C9,C1,C2,C3), C4"(C3",C2",N1",C6",C5")
;
_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 -0.06183(17) 0.0974(4) 0.06501(16) 0.081(4) Uani 1 1 d . . . . .
O4 O 0.050(2) 0.070(4) -0.058(2) 0.070(14) Uani 1 1 d D . . . .
C2' C 0.1195(15) 0.025(2) 0.3181(17) 0.096(18) Uani 1 1 d G U . . .
H2' H 0.053722 -0.012949 0.311414 0.115 Uiso 1 1 calc R U . . .
C3' C 0.2232(18) 0.023(3) 0.4200(15) 0.085(18) Uani 1 1 d G U . . .
H3' H 0.226785 -0.015492 0.481505 0.103 Uiso 1 1 calc R U . . .
C4' C 0.3215(15) 0.080(3) 0.4299(14) 0.094(19) Uani 1 1 d G U . . .
C5' C 0.3161(15) 0.138(3) 0.338(2) 0.12(2) Uani 1 1 d G U . . .
H5' H 0.381868 0.175325 0.344576 0.142 Uiso 1 1 calc R U . . .
C6' C 0.2124(17) 0.139(3) 0.2360(17) 0.10(2) Uani 1 1 d G U . . .
H6' H 0.208807 0.177870 0.174485 0.124 Uiso 1 1 calc R U . . .
N1' N 0.1141(12) 0.083(2) 0.2261(12) 0.057(16) Uani 1 1 d G U . . .
C4 C 0.1330(11) 0.1983(18) -0.1243(11) 0.059(14) Uani 1 1 d DG . . . .
C5 C 0.1879(14) 0.1401(16) -0.1786(14) 0.052(14) Uani 1 1 d DG . . . .
H5 H 0.182834 0.073454 -0.174947 0.063 Uiso 1 1 calc R U . . .
C9 C 0.2505(12) 0.1815(18) -0.2383(12) 0.062(15) Uani 1 1 d DG . . . .
H9 H 0.287265 0.142535 -0.274697 0.075 Uiso 1 1 calc R U . . .
C1 C 0.2581(11) 0.2810(18) -0.2438(11) 0.055(15) Uani 1 1 d DG . . . .
C2 C 0.2032(14) 0.3392(17) -0.1895(15) 0.064(14) Uani 1 1 d DG . . . .
H2 H 0.208293 0.405839 -0.193087 0.076 Uiso 1 1 calc R U . . .
C3 C 0.1406(12) 0.2978(17) -0.1297(12) 0.062(15) Uani 1 1 d DG . . . .
H3 H 0.103860 0.336760 -0.093336 0.074 Uiso 1 1 calc R U . . .
O3 O 0.0197(18) 0.206(4) -0.0099(17) 0.093(14) Uani 1 1 d D . . . .
N2' N 0.440(2) 0.0830(17) 0.531(2) 0.10(2) Uani 1 1 d . . . . .
N2" N 0.424(2) 0.051(5) 0.617(2) 0.098(8) Uani 1 1 d . U . . .
C4" C 0.5433(13) 0.079(3) 0.7165(16) 0.096(14) Uani 1 1 d G U . . .
C3" C 0.5589(16) 0.027(3) 0.8159(19) 0.114(15) Uani 1 1 d G U . . .
H3" H 0.494924 -0.007909 0.819706 0.137 Uiso 1 1 calc R U . . .
C2" C 0.6701(18) 0.026(3) 0.9095(15) 0.102(12) Uani 1 1 d G U . . .
H2" H 0.680529 -0.008421 0.976015 0.122 Uiso 1 1 calc R U . . .
N1" N 0.7657(12) 0.078(3) 0.9038(12) 0.071(7) Uani 1 1 d G U . . .
C6" C 0.7501(15) 0.130(3) 0.8044(16) 0.096(12) Uani 1 1 d G U . . .
H6" H 0.814041 0.164401 0.800522 0.115 Uiso 1 1 calc R U . . .
C5" C 0.6389(18) 0.130(3) 0.7107(15) 0.111(15) Uani 1 1 d G U . . .
H5" H 0.628436 0.164914 0.644211 0.133 Uiso 1 1 calc R U . . .
C7 C 0.321(4) 0.327(3) -0.309(3) 0.076(17) Uani 1 1 d D . . . .
O2 O 0.3671(17) 0.268(3) -0.3590(16) 0.086(15) Uani 1 1 d D . . . .
C8 C 0.065(3) 0.156(3) -0.062(3) 0.053(14) Uani 1 1 d D . . . .
O1 O 0.324(3) 0.419(4) -0.321(2) 0.084(14) Uani 1 1 d 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
Cd1 O4 2.33(5) 3 ?
Cd1 O4 2.46(2) . ?
Cd1 N1' 2.287(13) . ?
Cd1 O3 2.22(4) . ?
Cd1 N1" 2.27(3) 1_454 ?
Cd1 C7 2.73(4) 4_566 ?
Cd1 O2 2.41(4) 4_566 ?
Cd1 C8 2.75(4) . ?
Cd1 O1 2.37(2) 4_566 ?
O4 C8 1.22(4) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.48(3) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.47(4) . ?
C5 H5 0.9300 . ?
C5 C9 1.3900 . ?
C9 H9 0.9300 . ?
C9 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.47(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.23(3) . ?
N2' N2" 1.25(4) . ?
N2" C4" 1.53(3) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.29(3) . ?
C7 O1 1.30(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
O4 Cd1 O4 76.1(14) 3 . ?
O4 Cd1 C7 117.5(8) 3 4_566 ?
O4 Cd1 C7 166.3(14) . 4_566 ?
O4 Cd1 O2 145.6(10) 3 4_566 ?
O4 Cd1 C8 102.4(9) 3 . ?
O4 Cd1 C8 26.3(8) . . ?
O4 Cd1 O1 89.2(14) 3 4_566 ?
N1' Cd1 O4 89.4(8) . . ?
N1' Cd1 O4 84.0(11) . 3 ?
N1' Cd1 C7 92.1(11) . 4_566 ?
N1' Cd1 O2 94.1(8) . 4_566 ?
N1' Cd1 C8 90.0(9) . . ?
N1' Cd1 O1 91.1(9) . 4_566 ?
O3 Cd1 O4 128.2(10) . 3 ?
O3 Cd1 O4 52.2(17) . . ?
O3 Cd1 N1' 91.2(8) . . ?
O3 Cd1 N1" 96(4) . 1_454 ?
O3 Cd1 C7 114.2(11) . 4_566 ?
O3 Cd1 O2 86.1(13) . 4_566 ?
O3 Cd1 C8 25.9(10) . . ?
O3 Cd1 O1 142.5(15) . 4_566 ?
N1" Cd1 O4 84(5) 1_454 3 ?
N1" Cd1 O4 88(4) 1_454 . ?
N1" Cd1 N1' 168(5) 1_454 . ?
N1" Cd1 C7 93(4) 1_454 4_566 ?
N1" Cd1 O2 96(5) 1_454 4_566 ?
N1" Cd1 C8 93(3) 1_454 . ?
N1" Cd1 O1 89(3) 1_454 4_566 ?
C7 Cd1 C8 140.0(10) 4_566 . ?
O2 Cd1 O4 138.2(15) 4_566 . ?
O2 Cd1 C7 28.1(9) 4_566 4_566 ?
O2 Cd1 C8 112.0(11) 4_566 . ?
O1 Cd1 O4 165.2(18) 4_566 . ?
O1 Cd1 C7 28.4(9) 4_566 4_566 ?
O1 Cd1 O2 56.5(17) 4_566 4_566 ?
O1 Cd1 C8 168.4(15) 4_566 . ?
Cd1 O4 Cd1 103.9(14) 3 . ?
C8 O4 Cd1 165(3) . 3 ?
C8 O4 Cd1 90(3) . . ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 126(2) . . ?
C5' C4' N2' 114(2) . . ?
C4' C5' H5' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 120.3(10) . . ?
C6' N1' Cd1 119.4(11) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.9(8) . . ?
C3 C4 C8 119.1(8) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C9 120.0 . . ?
C9 C5 H5 120.0 . . ?
C5 C9 H9 120.0 . . ?
C1 C9 C5 120.0 . . ?
C1 C9 H9 120.0 . . ?
C9 C1 C2 120.0 . . ?
C9 C1 C7 121.1(8) . . ?
C2 C1 C7 118.8(8) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 102(3) . . ?
N2" N2' C4' 108(3) . . ?
N2' N2" C4" 102(3) . . ?
C3" C4" N2" 111(2) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 128(2) . . ?
C4" C3" H3" 120.0 . . ?
C4" C3" C2" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
N1" C2" C3" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 120.2(10) . 1_656 ?
C2" N1" C6" 120.0 . . ?
C6" N1" Cd1 119.1(11) . 1_656 ?
N1" C6" H6" 120.0 . . ?
C5" C6" N1" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 177.0(15) . 4_665 ?
O2 C7 Cd1 62(2) . 4_665 ?
O2 C7 C1 115(3) . . ?
O2 C7 O1 122(4) . . ?
O1 C7 Cd1 60(2) . 4_665 ?
O1 C7 C1 122(2) . . ?
C7 O2 Cd1 90(3) . 4_665 ?
O4 C8 Cd1 63(2) . . ?
O4 C8 C4 123(2) . . ?
O4 C8 O3 115(4) . . ?
C4 C8 Cd1 173.6(14) . . ?
O3 C8 Cd1 52(3) . . ?
O3 C8 C4 122(3) . . ?
C7 O1 Cd1 91(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 Cd1 -161(14) 3 . . . ?
Cd1 O4 C8 C4 179(3) . . . . ?
Cd1 O4 C8 C4 18(17) 3 . . . ?
Cd1 O4 C8 O3 -162(11) 3 . . . ?
Cd1 O4 C8 O3 -1(4) . . . . ?
Cd1 O3 C8 O4 2(5) . . . . ?
Cd1 O3 C8 C4 -179(3) . . . . ?
Cd1 N1" C6" C5" -170.5(17) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' -177(3) . . . . ?
C3' C2' N1' Cd1 -173.9(15) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -21(4) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" -169(3) . . . . ?
C5' C4' N2' N2" 162(3) . . . . ?
C5' C6' N1' Cd1 174.0(14) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C9 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 -3(5) . . . . ?
C5 C4 C8 O3 177(3) . . . . ?
C5 C9 C1 C2 0.0 . . . . ?
C5 C9 C1 C7 -179(2) . . . . ?
C9 C1 C2 C3 0.0 . . . . ?
C9 C1 C7 O2 0(5) . . . . ?
C9 C1 C7 O1 176(4) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 179(3) . . . 4_665 ?
C1 C7 O1 Cd1 -179(4) . . . 4_665 ?
C2 C1 C7 O2 -178(2) . . . . ?
C2 C1 C7 O1 -3(6) . . . . ?
C3 C4 C5 C9 0.0 . . . . ?
C3 C4 C8 O4 176(4) . . . . ?
C3 C4 C8 O3 -3(4) . . . . ?
N2' C4' C5' C6' 178(2) . . . . ?
N2' N2" C4" C3" -163(3) . . . . ?
N2' N2" C4" C5" 4(5) . . . . ?
N2" C4" C3" C2" 168(3) . . . . ?
N2" C4" C5" C6" -166(4) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 170.4(18) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 179(2) . . . . ?
O2 C7 O1 Cd1 -4(5) . . . 4_665 ?
C8 C4 C5 C9 179(2) . . . . ?
C8 C4 C3 C2 -179(2) . . . . ?
O1 C7 O2 Cd1 4(5) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.485 0.500 239.2 69.8 ?
2 0.500 -0.084 0.000 239.2 69.8 ?

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_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 2.005
_oxdiff_exptl_absorpt_empirical_full_min 0.619
####################################################################### 
# 
# 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_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046203'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2020-11-24 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT029_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.580 Why?
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT088_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.13 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_RINTA01_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.230 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT084_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT342_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.05438 Ang.
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT910_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT911_Cd(BDC)(AZPY)DMF_2_69_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.417        292 Report
RESPONSE: The data come from high-pressure studies and are limited by the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 24 November 2020 05:18 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        Cd(BDC)(AZPY)*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_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                   11.600(4)
_cell_length_b                   13.487(18)
_cell_length_c                   13.080(5)
_cell_angle_alpha                90
_cell_angle_beta                 114.57(4)
_cell_angle_gamma                90
_cell_volume                     1861(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.2640
_cell_measurement_theta_min      4.1230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.938
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -4 -11 0.0433
-15 2 14 0.0479
14 -3 -15 0.0214
-2 19 0 0.0135
10 0 18 0.2440
2 -19 -1 0.0254

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2298
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 0.580
_diffrn_reflns_Laue_measured_fraction_max 0.580
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5230
_diffrn_reflns_point_group_measured_fraction_full 0.580
_diffrn_reflns_point_group_measured_fraction_max 0.580
_diffrn_reflns_theta_full        17.223
_diffrn_reflns_theta_max         17.223
_diffrn_reflns_theta_min         4.236
_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 0.580
_diffrn_measured_fraction_theta_max 0.580
_diffrn_measurement_details      
;
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      0.0117337000
_diffrn_orient_matrix_UB_12      -0.0500826000
_diffrn_orient_matrix_UB_13      0.0174256000
_diffrn_orient_matrix_UB_21      -0.0661207000
_diffrn_orient_matrix_UB_22      -0.0096738000
_diffrn_orient_matrix_UB_23      -0.0253308000
_diffrn_orient_matrix_UB_31      0.0039513000
_diffrn_orient_matrix_UB_32      -0.0120995000
_diffrn_orient_matrix_UB_33      -0.0513067000
_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                355
_reflns_number_total             652
_reflns_special_details          
;
Data were collected at room temperature and pressure of 2.69(2) GPa (2690000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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 1.3 (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         0.738
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         652
_refine_ls_number_restraints     391
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.1298
_refine_ls_restrained_S_all      1.001
_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          0.3112
_refine_ls_wR_factor_ref         0.3737
_refine_special_details          ?
_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 -0.0587(3) 0.0962(6) 0.0699(3) 0.114(5) Uani 1 1 d . . . . .
O4 O 0.058(3) 0.086(3) -0.045(3) 0.083(12) Uani 1 1 d D U . . .
C2' C 0.113(3) 0.021(5) 0.318(3) 0.15(2) Uani 1 1 d G U . . .
H2' H 0.039328 -0.011454 0.310302 0.182 Uiso 1 1 calc R U . . .
C3' C 0.217(4) 0.023(5) 0.421(3) 0.17(2) Uani 1 1 d G U . . .
H3' H 0.213356 -0.008022 0.482865 0.199 Uiso 1 1 calc R U . . .
C4' C 0.328(3) 0.072(5) 0.432(2) 0.15(2) Uani 1 1 d G U . . .
C5' C 0.333(3) 0.118(5) 0.339(3) 0.14(2) Uani 1 1 d G U . . .
H5' H 0.407230 0.150524 0.346508 0.171 Uiso 1 1 calc R U . . .
C6' C 0.229(4) 0.116(4) 0.236(3) 0.13(2) Uani 1 1 d G U . . .
H6' H 0.233204 0.147094 0.173944 0.160 Uiso 1 1 calc R U . . .
N1' N 0.119(3) 0.067(4) 0.225(2) 0.13(2) Uani 1 1 d G U . . .
C4 C 0.139(2) 0.207(2) -0.115(2) 0.088(12) Uani 1 1 d DG U . . .
C5 C 0.190(2) 0.147(2) -0.172(2) 0.078(12) Uani 1 1 d DG U . . .
H5 H 0.181763 0.078320 -0.170066 0.094 Uiso 1 1 calc R U . . .
C6 C 0.252(2) 0.189(2) -0.232(2) 0.083(13) Uani 1 1 d DG U . . .
H6 H 0.285308 0.148499 -0.270622 0.099 Uiso 1 1 calc R U . . .
C1 C 0.263(2) 0.291(2) -0.235(2) 0.084(11) Uani 1 1 d DG U . . .
C2 C 0.213(3) 0.352(2) -0.178(3) 0.094(13) Uani 1 1 d DG U . . .
H2 H 0.220897 0.420201 -0.179522 0.113 Uiso 1 1 calc R U . . .
C3 C 0.151(3) 0.310(2) -0.117(2) 0.105(12) Uani 1 1 d DG U . . .
H3 H 0.117352 0.350024 -0.078964 0.125 Uiso 1 1 calc R U . . .
O3 O 0.036(2) 0.208(3) -0.002(2) 0.082(12) Uani 1 1 d D U . . .
N2' N 0.447(4) 0.088(2) 0.542(3) 0.15(2) Uani 1 1 d . U . . .
N2" N 0.417(5) 0.062(7) 0.627(4) 0.16(2) Uani 1 1 d . U . . .
C4" C 0.528(3) 0.068(5) 0.720(3) 0.15(2) Uani 1 1 d G U . . .
C3" C 0.549(3) 0.016(5) 0.818(3) 0.15(2) Uani 1 1 d G U . . .
H3" H 0.487702 -0.028201 0.819913 0.176 Uiso 1 1 calc R U . . .
C2" C 0.661(4) 0.030(5) 0.914(3) 0.15(2) Uani 1 1 d G U . . .
H2" H 0.674440 -0.005143 0.979394 0.180 Uiso 1 1 calc R U . . .
N1" N 0.752(3) 0.095(5) 0.912(3) 0.14(2) Uani 1 1 d G U . . .
C6" C 0.731(4) 0.147(5) 0.814(4) 0.18(3) Uani 1 1 d G U . . .
H6" H 0.791839 0.191406 0.812114 0.214 Uiso 1 1 calc R U . . .
C5" C 0.619(4) 0.134(5) 0.718(3) 0.18(3) Uani 1 1 d G U . . .
H5" H 0.605102 0.168350 0.652631 0.218 Uiso 1 1 calc R U . . .
C7 C 0.332(5) 0.336(3) -0.298(5) 0.097(13) Uani 1 1 d D U . . .
O2 O 0.378(3) 0.292(4) -0.343(3) 0.103(13) Uani 1 1 d D U . . .
C8 C 0.091(5) 0.163(2) -0.035(4) 0.083(14) Uani 1 1 d D U . . .
O1 O 0.324(4) 0.415(3) -0.325(3) 0.108(13) 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 O4 2.41(2) . ?
Cd1 O4 2.48(4) 3 ?
Cd1 N1' 2.24(2) . ?
Cd1 O3 2.29(3) . ?
Cd1 N1" 2.31(5) 1_454 ?
Cd1 C7 2.69(3) 4_566 ?
Cd1 O2 2.19(4) 4_566 ?
Cd1 O1 2.31(3) 4_566 ?
O4 C8 1.10(3) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.54(5) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.49(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.49(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.10(3) . ?
N2' N2" 1.34(7) . ?
N2" C4" 1.36(5) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.12(3) . ?
C7 O1 1.11(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
O4 Cd1 O4 80.1(12) . 3 ?
O4 Cd1 C7 163.1(13) . 4_566 ?
O4 Cd1 C7 116.6(10) 3 4_566 ?
N1' Cd1 O4 90.5(12) . . ?
N1' Cd1 O4 84.1(16) . 3 ?
N1' Cd1 O3 93.9(14) . . ?
N1' Cd1 N1" 170(8) . 1_454 ?
N1' Cd1 C7 88.7(17) . 4_566 ?
N1' Cd1 O1 89.8(15) . 4_566 ?
O3 Cd1 O4 125.1(10) . 3 ?
O3 Cd1 O4 45.0(14) . . ?
O3 Cd1 N1" 94(7) . 1_454 ?
O3 Cd1 C7 118.2(12) . 4_566 ?
O3 Cd1 O1 142.2(14) . 4_566 ?
N1" Cd1 O4 86(8) 1_454 3 ?
N1" Cd1 O4 91(7) 1_454 . ?
N1" Cd1 C7 93(7) 1_454 4_566 ?
O2 Cd1 O4 140.3(14) 4_566 3 ?
O2 Cd1 O4 139.5(17) 4_566 . ?
O2 Cd1 N1' 91.8(15) 4_566 . ?
O2 Cd1 O3 94.6(16) 4_566 . ?
O2 Cd1 N1" 94(7) 4_566 1_454 ?
O2 Cd1 C7 23.7(10) 4_566 4_566 ?
O2 Cd1 O1 47.7(17) 4_566 4_566 ?
O1 Cd1 O4 92.7(13) 4_566 3 ?
O1 Cd1 O4 172.7(15) 4_566 . ?
O1 Cd1 N1" 88(7) 4_566 1_454 ?
O1 Cd1 C7 24.2(8) 4_566 4_566 ?
Cd1 O4 Cd1 99.9(12) . 3 ?
C8 O4 Cd1 98(2) . . ?
C8 O4 Cd1 159(3) . 3 ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 126(3) . . ?
C5' C4' N2' 113(3) . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
N1' C6' C5' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 120(2) . . ?
C6' N1' Cd1 118(2) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.2(9) . . ?
C3 C4 C8 119.1(9) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 C5 120.0 . . ?
C1 C6 H6 120.0 . . ?
C6 C1 C2 120.0 . . ?
C6 C1 C7 119.9(9) . . ?
C2 C1 C7 120.1(9) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 105(3) . . ?
N2" N2' C4' 107(4) . . ?
N2' N2" C4" 105(5) . . ?
C3" C4" N2" 123(5) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 117(5) . . ?
C4" C3" H3" 120.0 . . ?
C2" C3" C4" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
C3" C2" N1" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 116(2) . 1_656 ?
C2" N1" C6" 120.0 . . ?
C6" N1" Cd1 124(2) . 1_656 ?
N1" C6" H6" 120.0 . . ?
N1" C6" C5" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 174(3) . 4_665 ?
O2 C7 Cd1 52(3) . 4_665 ?
O2 C7 C1 124(3) . . ?
O1 C7 Cd1 58(2) . 4_665 ?
O1 C7 C1 125(3) . . ?
O1 C7 O2 110(4) . . ?
C7 O2 Cd1 104(4) . 4_665 ?
O4 C8 C4 121(3) . . ?
O4 C8 O3 110(5) . . ?
O3 C8 C4 120(3) . . ?
C7 O1 Cd1 98(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 C4 50(15) 3 . . . ?
Cd1 O4 C8 C4 -162(4) . . . . ?
Cd1 O4 C8 O3 -163(7) 3 . . . ?
Cd1 O4 C8 O3 -16(6) . . . . ?
Cd1 O3 C8 O4 17(6) . . . . ?
Cd1 O3 C8 C4 164(3) . . . . ?
Cd1 N1" C6" C5" 172(3) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' 174(5) . . . . ?
C3' C2' N1' Cd1 -166(3) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -10(6) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" 173(5) . . . . ?
C5' C4' N2' N2" 165(4) . . . . ?
C5' C6' N1' Cd1 166(3) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 -25(7) . . . . ?
C5 C4 C8 O3 -169(4) . . . . ?
C5 C6 C1 C2 0.0 . . . . ?
C5 C6 C1 C7 179(3) . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C1 C7 O2 0(8) . . . . ?
C6 C1 C7 O1 162(6) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 174(4) . . . 4_665 ?
C1 C7 O1 Cd1 -173(5) . . . 4_665 ?
C2 C1 C7 O2 178(5) . . . . ?
C2 C1 C7 O1 -19(9) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C8 O4 164(5) . . . . ?
C3 C4 C8 O3 21(6) . . . . ?
N2' C4' C5' C6' -175(4) . . . . ?
N2' N2" C4" C3" -157(4) . . . . ?
N2' N2" C4" C5" 27(7) . . . . ?
N2" C4" C3" C2" -175(5) . . . . ?
N2" C4" C5" C6" 176(5) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 -173(3) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 -179(3) . . . . ?
O2 C7 O1 Cd1 -8(7) . . . 4_665 ?
C8 C4 C5 C6 -170(3) . . . . ?
C8 C4 C3 C2 170(3) . . . . ?
O1 C7 O2 Cd1 9(8) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 189.1 89.5 ?
2 0.500 0.500 0.000 189.1 89.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
####################################################################### 
# 
# 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_CdBDCAZPYDMF_0_55_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046204'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.443 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT088_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.12 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT084_CdBDCAZPYDMF_0_55_GPa_MEW 
;
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_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03812 Ang.
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT911_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526        209 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT930_CdBDCAZPYDMF_0_55_GPa_MEW 
;
PROBLEM: FCF-based   Twin Law ( 1 0-1)         Est.d BASF       0.27 Check
RESPONSE: For this compound, we observed the phase transition from phase \a of  orthorhombic space-group Cmce to phase \b of monoclinic P21/n.  This phase transition may entail this alert.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C18H12CdN4O4
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                   12.230(3)
_cell_length_b                   14.03(2)
_cell_length_c                   12.539(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.56(2)
_cell_angle_gamma                90
_cell_volume                     1973(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.4680
_cell_measurement_theta_min      3.5720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.817
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 -2 8 0.0886
-10 2 -9 0.0177
16 -7 -8 0.0723
1 20 2 0.0527
-17 3 8 0.1038
0 -20 -2 0.0263

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1594
_diffrn_reflns_av_unetI/netI     0.1170
_diffrn_reflns_Laue_measured_fraction_full 0.443
_diffrn_reflns_Laue_measured_fraction_max 0.443
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8399
_diffrn_reflns_point_group_measured_fraction_full 0.443
_diffrn_reflns_point_group_measured_fraction_max 0.443
_diffrn_reflns_theta_full        21.934
_diffrn_reflns_theta_max         21.934
_diffrn_reflns_theta_min         3.336
_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 0.443
_diffrn_measured_fraction_theta_max 0.443
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.30(2) GPa (300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      0.0008061000
_diffrn_orient_matrix_UB_12      -0.0503207000
_diffrn_orient_matrix_UB_13      -0.0049481000
_diffrn_orient_matrix_UB_21      -0.0271981000
_diffrn_orient_matrix_UB_22      0.0039678000
_diffrn_orient_matrix_UB_23      -0.0614825000
_diffrn_orient_matrix_UB_31      0.0571366000
_diffrn_orient_matrix_UB_32      0.0025199000
_diffrn_orient_matrix_UB_33      -0.0018671000
_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                565
_reflns_number_total             1065
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         1.607
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1065
_refine_ls_number_restraints     370
_refine_ls_R_factor_all          0.1924
_refine_ls_R_factor_gt           0.1385
_refine_ls_restrained_S_all      1.128
_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          0.3414
_refine_ls_wR_factor_ref         0.3887
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4-C8
 1.35 with sigma of 0.02
 O3-O4
 2.1 with sigma of 0.02
 N2'_$1-N2'_$2
 3 with sigma of 0.02
 O3-C8 \\sim C8-O4
 with sigma of 0.02
 C3-C8 \\sim C8-C5
 with sigma of 0.02
 C2-C7 \\sim C7-C9
 with sigma of 0.02
 O2-C7 \\sim C7-O1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1" \\sim C2" \\sim C3" \\sim C4" \\sim C5" \\sim C6": within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C4' \\sim C3' \\sim C2' \\sim N1' \\sim C6' \\sim C5': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
O3 \\sim O4 \\sim C8: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
O4 \\sim C4 \\sim C5 \\sim C9 \\sim C1 \\sim C2 \\sim C3 \\sim O3 \\sim C7
\\sim O2 \\sim C8 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(N2") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1") \\sim Ueq, Uanis(C4") \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C5', Cd1, O3, N1', O4, C8, C2', C6', C4, C3', C5, C3, C4', C9, C2, N2', C1,
 N2", C7, C4", O2, O1, C3", C5", C2", C6", N1"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6'), C5(H5), C9(H9), C2(H2), C3(H3),
 C3"(H3"), C2"(H2"), C6"(H6"), C5"(H5")
5.b Fitted hexagon refined as free rotating group:
 C2'(C3',C4',C5',C6',N1'), C4(C5,C9,C1,C2,C3), C4"(C3",C2",N1",C6",C5")
;
_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 -0.0627(2) 0.0965(5) 0.06466(19) 0.072(5) Uani 1 1 d . . . . .
O4 O 0.047(3) 0.070(2) -0.055(2) 0.087(15) Uani 1 1 d D U . . .
C2' C 0.1210(19) 0.033(3) 0.318(2) 0.12(2) Uani 1 1 d G U . . .
H2' H 0.056209 -0.004341 0.312077 0.139 Uiso 1 1 calc R U . . .
C3' C 0.225(2) 0.030(3) 0.4185(19) 0.12(2) Uani 1 1 d G U . . .
H3' H 0.230486 -0.009527 0.479633 0.146 Uiso 1 1 calc R U . . .
C4' C 0.3223(17) 0.086(4) 0.4274(18) 0.12(2) Uani 1 1 d G U . . .
C5' C 0.315(2) 0.146(4) 0.336(2) 0.13(2) Uani 1 1 d G U . . .
H5' H 0.379461 0.183425 0.341937 0.159 Uiso 1 1 calc R U . . .
C6' C 0.210(2) 0.149(3) 0.2356(19) 0.11(2) Uani 1 1 d G U . . .
H6' H 0.205186 0.188612 0.174380 0.137 Uiso 1 1 calc R U . . .
N1' N 0.1134(16) 0.093(3) 0.2266(15) 0.09(2) Uani 1 1 d G U . . .
C4 C 0.1290(13) 0.199(2) -0.1296(13) 0.073(15) Uani 1 1 d DG U . . .
C5 C 0.1858(16) 0.1420(19) -0.1824(15) 0.059(15) Uani 1 1 d DG U . . .
H5 H 0.181407 0.075988 -0.178525 0.071 Uiso 1 1 calc R U . . .
C9 C 0.2490(13) 0.183(2) -0.2411(12) 0.069(16) Uani 1 1 d DG U . . .
H9 H 0.286973 0.145138 -0.276423 0.083 Uiso 1 1 calc R U . . .
C1 C 0.2555(12) 0.282(2) -0.2469(12) 0.062(15) Uani 1 1 d G U . . .
C2 C 0.1988(15) 0.3392(19) -0.1941(16) 0.069(15) Uani 1 1 d DG U . . .
H2 H 0.203124 0.405238 -0.197997 0.083 Uiso 1 1 calc R U . . .
C3 C 0.1355(14) 0.298(2) -0.1354(14) 0.079(16) Uani 1 1 d DG U . . .
H3 H 0.097557 0.336090 -0.100099 0.095 Uiso 1 1 calc R U . . .
O3 O 0.0207(18) 0.208(2) -0.0103(17) 0.096(15) Uani 1 1 d D U . . .
N2' N 0.438(3) 0.083(2) 0.526(3) 0.13(4) Uani 1 1 d . . . . .
N2" N 0.427(3) 0.068(5) 0.613(3) 0.092(9) Uani 1 1 d . U . . .
C4" C 0.5457(17) 0.078(4) 0.713(2) 0.096(9) Uani 1 1 d G U . . .
C3" C 0.559(2) 0.029(4) 0.814(2) 0.098(13) Uani 1 1 d G U . . .
H3" H 0.494225 -0.002407 0.818710 0.118 Uiso 1 1 calc R U . . .
C2" C 0.669(2) 0.027(3) 0.9075(18) 0.097(13) Uani 1 1 d G U . . .
H2" H 0.678304 -0.006052 0.974922 0.116 Uiso 1 1 calc R U . . .
N1" N 0.7663(16) 0.074(4) 0.9004(16) 0.071(8) Uani 1 1 d G U . . .
C6" C 0.753(2) 0.123(4) 0.800(2) 0.100(13) Uani 1 1 d G U . . .
H6" H 0.817828 0.154192 0.794844 0.120 Uiso 1 1 calc R U . . .
C5" C 0.643(2) 0.125(4) 0.7060(18) 0.105(13) Uani 1 1 d G U . . .
H5" H 0.633750 0.157838 0.638629 0.126 Uiso 1 1 calc R U . . .
C7 C 0.324(4) 0.325(3) -0.301(4) 0.082(16) Uani 1 1 d D U . . .
O2 O 0.368(2) 0.269(4) -0.356(2) 0.093(17) Uani 1 1 d D U . . .
C8 C 0.065(3) 0.158(2) -0.070(3) 0.066(15) Uani 1 1 d D U . . .
O1 O 0.325(2) 0.417(4) -0.318(2) 0.077(15) 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 O4 2.34(3) 3 ?
Cd1 O4 2.42(2) . ?
Cd1 N1' 2.296(16) . ?
Cd1 O3 2.27(3) . ?
Cd1 N1" 2.30(4) 1_454 ?
Cd1 O2 2.43(5) 4_566 ?
Cd1 O1 2.39(2) 4_566 ?
O4 C8 1.29(2) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.46(4) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.407(19) . ?
C5 H5 0.9300 . ?
C5 C9 1.3900 . ?
C9 H9 0.9300 . ?
C9 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.41(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.285(19) . ?
N2' N2" 1.17(5) . ?
N2" C4" 1.50(4) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.30(4) . ?
C7 O1 1.31(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
O4 Cd1 O4 74.8(12) 3 . ?
O4 Cd1 O2 147.0(11) 3 4_566 ?
O4 Cd1 O2 138.2(13) . 4_566 ?
O4 Cd1 O1 91.7(15) 3 4_566 ?
N1' Cd1 O4 87.4(13) . 3 ?
N1' Cd1 O4 89.3(9) . . ?
N1' Cd1 O2 90.7(11) . 4_566 ?
N1' Cd1 O1 91.1(9) . 4_566 ?
O3 Cd1 O4 127.3(10) . 3 ?
O3 Cd1 O4 52.7(6) . . ?
O3 Cd1 N1' 88.0(10) . . ?
O3 Cd1 N1" 97(4) . 1_454 ?
O3 Cd1 O2 85.5(13) . 4_566 ?
O3 Cd1 O1 140.8(14) . 4_566 ?
N1" Cd1 O4 83(7) 1_454 3 ?
N1" Cd1 O4 87(5) 1_454 . ?
N1" Cd1 N1' 170(7) 1_454 . ?
N1" Cd1 O2 98(7) 1_454 4_566 ?
N1" Cd1 O1 90(4) 1_454 4_566 ?
O1 Cd1 O4 166.5(15) 4_566 . ?
O1 Cd1 O2 55.3(19) 4_566 4_566 ?
Cd1 O4 Cd1 105.2(12) 3 . ?
C8 O4 Cd1 95.8(16) . . ?
C8 O4 Cd1 159(2) . 3 ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 124(3) . . ?
C5' C4' N2' 116(3) . . ?
C4' C5' H5' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 118.3(14) . . ?
C6' N1' Cd1 121.7(14) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.7(9) . . ?
C3 C4 C8 119.3(9) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C9 120.0 . . ?
C9 C5 H5 120.0 . . ?
C5 C9 H9 120.0 . . ?
C1 C9 C5 120.0 . . ?
C1 C9 H9 120.0 . . ?
C9 C1 C2 120.0 . . ?
C9 C1 C7 120.7(9) . . ?
C2 C1 C7 119.2(8) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 103.3(17) . . ?
N2" N2' C4' 111(4) . . ?
N2' N2" C4" 109(4) . . ?
C3" C4" N2" 116(3) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 124(3) . . ?
C4" C3" H3" 120.0 . . ?
C4" C3" C2" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
N1" C2" C3" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 120.2(12) . 1_656 ?
C2" N1" C6" 120.0 . . ?
C6" N1" Cd1 118.7(14) . 1_656 ?
N1" C6" H6" 120.0 . . ?
N1" C6" C5" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
O2 C7 C1 117(3) . . ?
O2 C7 O1 118(4) . . ?
O1 C7 C1 123(2) . . ?
C7 O2 Cd1 92(3) . 4_665 ?
O4 C8 C4 128.9(19) . . ?
O3 C8 O4 108(2) . . ?
O3 C8 C4 122.8(18) . . ?
C7 O1 Cd1 94(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 C4 178(3) . . . . ?
Cd1 O4 C8 C4 5(13) 3 . . . ?
Cd1 O4 C8 O3 3(4) . . . . ?
Cd1 O4 C8 O3 -170(7) 3 . . . ?
Cd1 O3 C8 O4 -3(4) . . . . ?
Cd1 O3 C8 C4 -178(3) . . . . ?
Cd1 N1" C6" C5" -168(2) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' -176(3) . . . . ?
C3' C2' N1' Cd1 -178.9(18) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -34(5) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" -172(4) . . . . ?
C5' C4' N2' N2" 150(4) . . . . ?
C5' C6' N1' Cd1 178.9(18) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C9 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 -1(6) . . . . ?
C5 C4 C8 O3 173(2) . . . . ?
C5 C9 C1 C2 0.0 . . . . ?
C5 C9 C1 C7 177(3) . . . . ?
C9 C1 C2 C3 0.0 . . . . ?
C9 C1 C7 O2 7(5) . . . . ?
C9 C1 C7 O1 174(4) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 173(3) . . . 4_665 ?
C1 C7 O1 Cd1 -172(4) . . . 4_665 ?
C2 C1 C7 O2 -176(3) . . . . ?
C2 C1 C7 O1 -9(6) . . . . ?
C3 C4 C5 C9 0.0 . . . . ?
C3 C4 C8 O4 179(4) . . . . ?
C3 C4 C8 O3 -7(4) . . . . ?
N2' C4' C5' C6' 176(3) . . . . ?
N2' N2" C4" C3" -156(4) . . . . ?
N2' N2" C4" C5" 17(7) . . . . ?
N2" C4" C3" C2" 174(4) . . . . ?
N2" C4" C5" C6" -173(5) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 168(2) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 -177(3) . . . . ?
O2 C7 O1 Cd1 -5(5) . . . 4_665 ?
C8 C4 C5 C9 -180(2) . . . . ?
C8 C4 C3 C2 180(2) . . . . ?
O1 C7 O2 Cd1 5(5) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.974 0.500 248.4 8.8 ?
2 0.500 -0.807 0.000 248.4 8.8 ?

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_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 2.205
_oxdiff_exptl_absorpt_empirical_full_min 0.729
####################################################################### 
# 
# 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_CdBDCAZPYDMF_1_7_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046205'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.450 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT084_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT088_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.60 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT342_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03687 Ang.
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT911_CdBDCAZPYDMF_1_7_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526        219 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_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                   11.854(3)
_cell_length_b                   13.68(2)
_cell_length_c                   12.773(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.04(3)
_cell_angle_gamma                90
_cell_volume                     1891(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1036
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0360
_cell_measurement_theta_min      3.4770
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.841
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -3 -12 0.1174
14 -2 -15 0.0264
-15 2 14 0.0465
8 3 11 0.1105
0 19 -3 0.0344
0 -19 3 0.0295

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1680
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.450
_diffrn_reflns_Laue_measured_fraction_max 0.450
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8417
_diffrn_reflns_point_group_measured_fraction_full 0.450
_diffrn_reflns_point_group_measured_fraction_max 0.450
_diffrn_reflns_theta_full        21.949
_diffrn_reflns_theta_max         21.949
_diffrn_reflns_theta_min         3.044
_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 0.450
_diffrn_measured_fraction_theta_max 0.450
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.30(2) GPa (300000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      0.0018012000
_diffrn_orient_matrix_UB_12      -0.0516980000
_diffrn_orient_matrix_UB_13      0.0064185000
_diffrn_orient_matrix_UB_21      0.0281061000
_diffrn_orient_matrix_UB_22      0.0054641000
_diffrn_orient_matrix_UB_23      0.0603900000
_diffrn_orient_matrix_UB_31      -0.0590630000
_diffrn_orient_matrix_UB_32      0.0011089000
_diffrn_orient_matrix_UB_33      0.0014529000
_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                580
_reflns_number_total             1034
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         0.784
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1034
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.1182
_refine_ls_restrained_S_all      1.087
_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          0.3253
_refine_ls_wR_factor_ref         0.3782
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2'_$1-O3_$2
 3 with sigma of 0.02
 O4_$2-N1"_$3
 3 with sigma of 0.02
 O3-C8 \\sim C8-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2' \\sim C3' \\sim C4' \\sim C5' \\sim C6' \\sim N1' \\sim N2' \\sim N2" \\sim
C4" \\sim C3" \\sim C2" \\sim N1" \\sim C6" \\sim C5": within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
O4 \\sim C4 \\sim C5 \\sim C9 \\sim C1 \\sim C2 \\sim C3 \\sim O3 \\sim C7
\\sim O2 \\sim C8 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) = Uanis(C4) = Uanis(C5) = Uanis(C9) = Uanis(C1) = Uanis(C2) =
Uanis(C3) = Uanis(C7) = Uanis(C8) = Uanis(O1) = Uanis(O3) = Uanis(O2)
Uanis(O4) = Uanis(Cd1)
4. Rigid body (RIGU) restrains
 C6', Cd1, N1', O4, O3, C2', C8, C3', C5', C4, C4', C5, C3, N2', C9, C2, N2",
 C1, C4", C7, C3", C5", O2, O1, C2", C6", N1"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6'), C5(H5), C9(H9), C2(H2), C3(H3),
 C3"(H3"), C2"(H2"), C6"(H6"), C5"(H5")
5.b Fitted hexagon refined as free rotating group:
 C2'(C3',C4',C5',C6',N1'), C4(C5,C9,C1,C2,C3), C4"(C3",C2",N1",C6",C5")
;
_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 -0.05928(17) 0.0975(5) 0.06655(17) 0.067(3) Uani 1 1 d . . . . .
O4 O 0.0614(17) 0.071(3) -0.0495(16) 0.067(3) Uani 1 1 d D U . . .
C2' C 0.1235(16) 0.012(3) 0.3133(18) 0.086(17) Uani 1 1 d G U . . .
H2' H 0.055869 -0.027323 0.302838 0.103 Uiso 1 1 calc R U . . .
C3' C 0.225(2) 0.013(3) 0.4182(16) 0.103(18) Uani 1 1 d G U . . .
H3' H 0.225533 -0.026317 0.477930 0.123 Uiso 1 1 calc R U . . .
C4' C 0.3263(18) 0.072(3) 0.4338(16) 0.107(17) Uani 1 1 d G U . . .
C5' C 0.3257(19) 0.130(3) 0.345(2) 0.13(2) Uani 1 1 d G U . . .
H5' H 0.393383 0.169514 0.354955 0.161 Uiso 1 1 calc R U . . .
C6' C 0.224(2) 0.129(3) 0.2396(18) 0.106(18) Uani 1 1 d G U . . .
H6' H 0.223721 0.168510 0.179862 0.127 Uiso 1 1 calc R U . . .
N1' N 0.1230(15) 0.070(3) 0.2240(13) 0.081(16) Uani 1 1 d G U . . .
C4 C 0.1393(13) 0.200(2) -0.1194(13) 0.067(3) Uani 1 1 d G U . . .
C5 C 0.1917(17) 0.141(2) -0.1758(17) 0.067(3) Uani 1 1 d G U . . .
H5 H 0.186092 0.073331 -0.172190 0.080 Uiso 1 1 calc R U . . .
C9 C 0.2526(14) 0.183(2) -0.2376(14) 0.067(3) Uani 1 1 d G U . . .
H9 H 0.287725 0.142837 -0.275296 0.080 Uiso 1 1 calc R U . . .
C1 C 0.2610(14) 0.284(3) -0.2429(13) 0.067(3) Uani 1 1 d G U . . .
C2 C 0.2086(17) 0.343(2) -0.1865(17) 0.067(3) Uani 1 1 d G U . . .
H2 H 0.214204 0.410785 -0.190128 0.080 Uiso 1 1 calc R U . . .
C3 C 0.1477(14) 0.302(2) -0.1248(13) 0.067(3) Uani 1 1 d G U . . .
H3 H 0.112570 0.341281 -0.087021 0.080 Uiso 1 1 calc R U . . .
O3 O 0.0272(16) 0.222(3) -0.0040(16) 0.067(3) Uani 1 1 d D U . . .
N2' N 0.440(3) 0.082(3) 0.537(2) 0.114(18) Uani 1 1 d . U . . .
N2" N 0.427(3) 0.059(5) 0.618(3) 0.117(18) Uani 1 1 d . U . . .
C4" C 0.5400(16) 0.069(3) 0.7203(17) 0.113(19) Uani 1 1 d G U . . .
C3" C 0.563(2) 0.012(3) 0.817(2) 0.11(2) Uani 1 1 d G U . . .
H3" H 0.502513 -0.031090 0.818678 0.131 Uiso 1 1 calc R U . . .
C2" C 0.676(2) 0.019(3) 0.9111(16) 0.103(19) Uani 1 1 d G U . . .
H2" H 0.690739 -0.019442 0.975761 0.124 Uiso 1 1 calc R U . . .
N1" N 0.7656(14) 0.083(3) 0.9085(12) 0.084(18) Uani 1 1 d G U . . .
C6" C 0.7428(19) 0.139(3) 0.8118(17) 0.10(2) Uani 1 1 d G U . . .
H6" H 0.803072 0.182137 0.810114 0.120 Uiso 1 1 calc R U . . .
C5" C 0.630(2) 0.132(3) 0.7177(16) 0.12(2) Uani 1 1 d G U . . .
H5" H 0.614847 0.170491 0.653029 0.140 Uiso 1 1 calc R U . . .
C7 C 0.318(3) 0.325(6) -0.319(3) 0.067(3) Uani 1 1 d . U . . .
O2 O 0.3757(16) 0.271(3) -0.3535(15) 0.067(3) Uani 1 1 d . U . . .
C8 C 0.066(3) 0.165(3) -0.062(3) 0.067(3) Uani 1 1 d D U . . .
O1 O 0.3318(19) 0.413(4) -0.3148(17) 0.067(3) 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
Cd1 O4 2.31(4) 3 ?
Cd1 O4 2.47(2) . ?
Cd1 N1' 2.304(15) . ?
Cd1 O3 2.35(3) . ?
Cd1 N1" 2.24(2) 1_454 ?
Cd1 C7 2.68(4) 4_566 ?
Cd1 O2 2.35(4) 4_566 ?
Cd1 C8 2.79(4) . ?
Cd1 O1 2.36(2) 4_566 ?
O4 C8 1.30(3) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.46(3) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.42(4) . ?
C5 H5 0.9300 . ?
C5 C9 1.3900 . ?
C9 H9 0.9300 . ?
C9 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.49(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.29(3) . ?
N2' N2" 1.15(5) . ?
N2" C4" 1.45(3) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.21(6) . ?
C7 O1 1.22(10) . ?

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 O4 77.6(13) 3 . ?
O4 Cd1 N1' 83.9(11) 3 . ?
O4 Cd1 O3 132.5(9) 3 . ?
O4 Cd1 N1" 82(5) 3 1_454 ?
O4 Cd1 C7 117.4(18) 3 4_566 ?
O4 Cd1 C7 165(2) . 4_566 ?
O4 Cd1 O2 144.2(10) 3 4_566 ?
O4 Cd1 C8 27.7(6) . . ?
O4 Cd1 C8 105.2(10) 3 . ?
O4 Cd1 O1 90.7(13) 3 4_566 ?
N1' Cd1 O4 86.2(7) . . ?
N1' Cd1 O3 92.9(9) . . ?
N1' Cd1 C7 96.5(9) . 4_566 ?
N1' Cd1 O2 95.8(9) . 4_566 ?
N1' Cd1 C8 91.8(8) . . ?
N1' Cd1 O1 89.6(7) . 4_566 ?
O3 Cd1 O4 54.9(13) . . ?
O3 Cd1 C7 110.1(19) . 4_566 ?
O3 Cd1 C8 27.4(7) . . ?
N1" Cd1 O4 90(4) 1_454 . ?
N1" Cd1 N1' 165(5) 1_454 . ?
N1" Cd1 O3 96(4) 1_454 . ?
N1" Cd1 C7 91(5) 1_454 4_566 ?
N1" Cd1 O2 97(5) 1_454 4_566 ?
N1" Cd1 C8 91(4) 1_454 . ?
N1" Cd1 O1 91(4) 1_454 4_566 ?
C7 Cd1 C8 137.2(19) 4_566 . ?
O2 Cd1 O4 138.2(14) 4_566 . ?
O2 Cd1 O3 83.3(12) 4_566 . ?
O2 Cd1 C7 26.9(18) 4_566 4_566 ?
O2 Cd1 C8 110.6(12) 4_566 . ?
O2 Cd1 O1 53.5(15) 4_566 4_566 ?
O1 Cd1 O4 167.9(16) 4_566 . ?
O1 Cd1 O3 136.8(13) 4_566 . ?
O1 Cd1 C7 27(2) 4_566 4_566 ?
O1 Cd1 C8 164.1(14) 4_566 . ?
Cd1 O4 Cd1 102.4(13) 3 . ?
C8 O4 Cd1 166(2) . 3 ?
C8 O4 Cd1 90(2) . . ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 128(2) . . ?
C5' C4' N2' 112(2) . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 119.8(12) . . ?
C6' N1' Cd1 118.7(13) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 124(2) . . ?
C3 C4 C8 116(2) . . ?
C4 C5 H5 120.0 . . ?
C9 C5 C4 120.0 . . ?
C9 C5 H5 120.0 . . ?
C5 C9 H9 120.0 . . ?
C5 C9 C1 120.0 . . ?
C1 C9 H9 120.0 . . ?
C9 C1 C7 118(3) . . ?
C2 C1 C9 120.0 . . ?
C2 C1 C7 122(3) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 96(2) . . ?
N2" N2' C4' 112(3) . . ?
N2' N2" C4" 112(4) . . ?
C3" C4" N2" 122(3) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 118(3) . . ?
C4" C3" H3" 120.0 . . ?
C4" C3" C2" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
N1" C2" C3" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 118.4(11) . 1_656 ?
C6" N1" Cd1 121.5(12) . 1_656 ?
C6" N1" C2" 120.0 . . ?
N1" C6" H6" 120.0 . . ?
C5" C6" N1" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 174(2) . 4_665 ?
O2 C7 Cd1 61(3) . 4_665 ?
O2 C7 C1 119(6) . . ?
O1 C7 Cd1 62(2) . 4_665 ?
O1 C7 C1 116(5) . . ?
O1 C7 O2 122(4) . . ?
C7 O2 Cd1 92(4) . 4_665 ?
O4 C8 Cd1 62(2) . . ?
O4 C8 C4 118(3) . . ?
C4 C8 Cd1 175.3(18) . . ?
O3 C8 Cd1 56.9(18) . . ?
O3 C8 O4 119(3) . . ?
O3 C8 C4 122(3) . . ?
C7 O1 Cd1 91(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 Cd1 156(9) 3 . . . ?
Cd1 O4 C8 C4 175(2) . . . . ?
Cd1 O4 C8 C4 -30(11) 3 . . . ?
Cd1 O4 C8 O3 8(3) . . . . ?
Cd1 O4 C8 O3 164(7) 3 . . . ?
Cd1 O3 C8 O4 -9(3) . . . . ?
Cd1 O3 C8 C4 -175(2) . . . . ?
Cd1 N1" C6" C5" -176.1(19) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' 180(4) . . . . ?
C3' C2' N1' Cd1 -165.8(19) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -21(6) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" 179(4) . . . . ?
C5' C4' N2' N2" 158(5) . . . . ?
C5' C6' N1' Cd1 165.9(17) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C9 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 9(3) . . . . ?
C5 C4 C8 O3 174.8(19) . . . . ?
C5 C9 C1 C2 0.0 . . . . ?
C5 C9 C1 C7 -174.7(19) . . . . ?
C9 C1 C2 C3 0.0 . . . . ?
C9 C1 C7 O2 -15(3) . . . . ?
C9 C1 C7 O1 -175(3) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 -173(2) . . . 4_665 ?
C1 C7 O1 Cd1 173(2) . . . 4_665 ?
C2 C1 C7 O2 171(2) . . . . ?
C2 C1 C7 O1 11(4) . . . . ?
C3 C4 C5 C9 0.0 . . . . ?
C3 C4 C8 O4 -176(2) . . . . ?
C3 C4 C8 O3 -10(3) . . . . ?
N2' C4' C5' C6' -180(3) . . . . ?
N2' N2" C4" C3" -154(4) . . . . ?
N2' N2" C4" C5" 22(7) . . . . ?
N2" C4" C3" C2" 176(4) . . . . ?
N2" C4" C5" C6" -176(4) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 176.2(19) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 174.5(19) . . . . ?
O2 C7 O1 Cd1 14(3) . . . 4_665 ?
C8 C4 C5 C9 174.5(19) . . . . ?
C8 C4 C3 C2 -174.9(18) . . . . ?
O1 C7 O2 Cd1 -14(3) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 225.5 60.3 ?
2 0.500 0.500 0.000 225.5 60.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.845
_oxdiff_exptl_absorpt_empirical_full_min 0.749
####################################################################### 
# 
# 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_CdBDCAZPYDMF_1_27_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046201'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.430 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT088_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.84 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT084_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT342_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04125 Ang.
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT911_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526        254 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT930_CdBDCAZPYDMF_1_27_GPa_MEW 
;
PROBLEM: FCF-based   Twin Law ( 1 0-1)         Est.d BASF       0.34 Check
RESPONSE: For this compound, we observed the phase transition from phase \a of  orthorhombic space-group Cmce to phase \b of monoclinic P21/n.  This phase transition may entail this alert.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C18H12CdN4O4
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                   11.996(4)
_cell_length_b                   13.77(3)
_cell_length_c                   12.629(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.84(4)
_cell_angle_gamma                90
_cell_volume                     1908(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    941
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3240
_cell_measurement_theta_min      3.5220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.881
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 -4 -7 0.1001
15 -3 -14 0.0594
-13 4 15 0.0492
-2 -18 6 0.0413
28 4 17 0.1704
8 16 -8 0.0564

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1749
_diffrn_reflns_av_unetI/netI     0.1738
_diffrn_reflns_Laue_measured_fraction_full 0.430
_diffrn_reflns_Laue_measured_fraction_max 0.430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4710
_diffrn_reflns_point_group_measured_fraction_full 0.430
_diffrn_reflns_point_group_measured_fraction_max 0.430
_diffrn_reflns_theta_full        21.957
_diffrn_reflns_theta_max         21.957
_diffrn_reflns_theta_min         3.034
_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 0.430
_diffrn_measured_fraction_theta_max 0.430
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.270(2) GPa (1270000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      0.0002628000
_diffrn_orient_matrix_UB_12      -0.0513476000
_diffrn_orient_matrix_UB_13      0.0060638000
_diffrn_orient_matrix_UB_21      0.0279933000
_diffrn_orient_matrix_UB_22      0.0051533000
_diffrn_orient_matrix_UB_23      0.0609668000
_diffrn_orient_matrix_UB_31      -0.0582281000
_diffrn_orient_matrix_UB_32      0.0020668000
_diffrn_orient_matrix_UB_33      0.0017812000
_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                494
_reflns_number_total             1006
_reflns_odcompleteness_completeness 45.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     21.92
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         0.996
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         1006
_refine_ls_number_restraints     373
_refine_ls_R_factor_all          0.2013
_refine_ls_R_factor_gt           0.1215
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3063
_refine_ls_wR_factor_ref         0.3686
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-C1 \\sim C1-O2
 with sigma of 0.02
 C2-C7 \\sim C7-C9
 with sigma of 0.02
 C3-C8 \\sim C8-C5
 with sigma of 0.02
 O3-C8 \\sim C8-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C4 \\sim C5 \\sim C9 \\sim C1 \\sim C2 \\sim C3 \\sim O3 \\sim C7
\\sim O2 \\sim C8 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C2' \\sim C3' \\sim C4' \\sim C5' \\sim C6' \\sim N1' \\sim N2' \\sim N2" \\sim
C4" \\sim C3" \\sim C2" \\sim N1" \\sim C6" \\sim C5": within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O3, Cd1, O4, N1', C8, C2', C6', C4, C3', C5', C5, C3, C4', C9, C2, N2', C1,
 N2", C7, C4", O2, O1, C3", C5", C2", C6", N1"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6'), C5(H5), C9(H9), C2(H2), C3(H3),
 C3"(H3"), C2"(H2"), C6"(H6"), C5"(H5")
5.b Fitted hexagon refined as free rotating group:
 C2'(C3',C4',C5',C6',N1'), C4(C5,C9,C1,C2,C3), C4"(C3",C2",N1",C6",C5")
;
_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 -0.0598(2) 0.0974(6) 0.0660(2) 0.054(5) Uani 1 1 d . . . . .
O4 O 0.053(3) 0.077(5) -0.057(3) 0.083(15) Uani 1 1 d D U . . .
C2' C 0.124(2) 0.021(3) 0.315(2) 0.10(2) Uani 1 1 d G U . . .
H2' H 0.057421 -0.017470 0.307192 0.115 Uiso 1 1 calc R U . . .
C3' C 0.227(2) 0.021(4) 0.418(2) 0.09(2) Uani 1 1 d G U . . .
H3' H 0.230585 -0.018311 0.479075 0.104 Uiso 1 1 calc R U . . .
C4' C 0.3264(19) 0.079(4) 0.4297(16) 0.10(2) Uani 1 1 d G U . . .
C5' C 0.3216(19) 0.138(4) 0.338(2) 0.09(2) Uani 1 1 d G U . . .
H5' H 0.387821 0.176791 0.346282 0.112 Uiso 1 1 calc R U . . .
C6' C 0.218(2) 0.138(4) 0.2355(18) 0.08(2) Uani 1 1 d G U . . .
H6' H 0.214659 0.177633 0.174399 0.099 Uiso 1 1 calc R U . . .
N1' N 0.1189(14) 0.080(3) 0.2238(15) 0.061(19) Uani 1 1 d G U . . .
C4 C 0.1341(14) 0.205(2) -0.1233(14) 0.063(15) Uani 1 1 d G U . . .
C5 C 0.1856(18) 0.145(2) -0.1800(18) 0.063(15) Uani 1 1 d DG U . . .
H5 H 0.178186 0.078155 -0.177212 0.075 Uiso 1 1 calc R U . . .
C9 C 0.2481(15) 0.186(3) -0.2410(15) 0.058(15) Uani 1 1 d DG U . . .
H9 H 0.282569 0.145634 -0.278941 0.070 Uiso 1 1 calc R U . . .
C1 C 0.2591(15) 0.286(3) -0.2452(15) 0.064(15) Uani 1 1 d DG U . . .
C2 C 0.208(2) 0.346(2) -0.188(2) 0.068(15) Uani 1 1 d DG U . . .
H2 H 0.215015 0.412781 -0.191215 0.081 Uiso 1 1 calc R U . . .
C3 C 0.1451(17) 0.305(2) -0.1275(17) 0.078(15) Uani 1 1 d DG U . . .
H3 H 0.110632 0.345304 -0.089485 0.094 Uiso 1 1 calc R U . . .
O3 O 0.028(2) 0.209(5) -0.0008(19) 0.079(14) Uani 1 1 d D U . . .
N2' N 0.448(3) 0.092(7) 0.537(3) 0.11(2) Uani 1 1 d . U . . .
N2" N 0.422(3) 0.057(6) 0.616(3) 0.09(2) Uani 1 1 d . U . . .
C4" C 0.5372(18) 0.070(4) 0.7147(19) 0.09(2) Uani 1 1 d G U . . .
C3" C 0.555(2) 0.015(4) 0.813(2) 0.10(2) Uani 1 1 d G U . . .
H3" H 0.491996 -0.023166 0.814867 0.122 Uiso 1 1 calc R U . . .
C2" C 0.667(2) 0.017(3) 0.9070(18) 0.08(2) Uani 1 1 d G U . . .
H2" H 0.678839 -0.019773 0.972501 0.102 Uiso 1 1 calc R U . . .
N1" N 0.7611(14) 0.074(4) 0.9035(16) 0.06(2) Uani 1 1 d G U . . .
C6" C 0.743(2) 0.129(4) 0.806(2) 0.08(2) Uani 1 1 d G U . . .
H6" H 0.806350 0.166781 0.803326 0.102 Uiso 1 1 calc R U . . .
C5" C 0.631(2) 0.127(4) 0.711(2) 0.09(2) Uani 1 1 d G U . . .
H5" H 0.619507 0.163390 0.645690 0.114 Uiso 1 1 calc R U . . .
C7 C 0.318(4) 0.328(4) -0.314(4) 0.066(16) Uani 1 1 d D U . . .
O2 O 0.368(2) 0.276(5) -0.3568(18) 0.070(16) Uani 1 1 d D U . . .
C8 C 0.069(4) 0.164(3) -0.061(4) 0.070(15) Uani 1 1 d D U . . .
O1 O 0.334(3) 0.415(3) -0.313(3) 0.070(15) 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 O4 2.40(6) 3 ?
Cd1 O4 2.45(2) . ?
Cd1 N1' 2.273(16) . ?
Cd1 O3 2.22(5) . ?
Cd1 N1" 2.32(4) 1_454 ?
Cd1 C7 2.71(5) 4_566 ?
Cd1 O2 2.33(5) 4_566 ?
Cd1 O1 2.36(2) 4_566 ?
O4 C8 1.22(4) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.54(4) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.43(5) . ?
C5 H5 0.9300 . ?
C5 C9 1.3900 . ?
C9 H9 0.9300 . ?
C9 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.44(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O3 C8 1.23(4) . ?
N2' N2" 1.26(6) . ?
N2" C4" 1.45(4) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.20(6) . ?
C7 O1 1.20(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
O4 Cd1 O4 79.3(18) 3 . ?
O4 Cd1 C7 116.2(12) 3 4_566 ?
O4 Cd1 C7 164(2) . 4_566 ?
N1' Cd1 O4 88.8(10) . . ?
N1' Cd1 O4 84.1(15) . 3 ?
N1' Cd1 N1" 166(6) . 1_454 ?
N1' Cd1 C7 94.6(13) . 4_566 ?
N1' Cd1 O2 95.1(11) . 4_566 ?
N1' Cd1 O1 89.5(9) . 4_566 ?
O3 Cd1 O4 130.2(13) . 3 ?
O3 Cd1 O4 51(2) . . ?
O3 Cd1 N1' 89.0(11) . . ?
O3 Cd1 N1" 100(4) . 1_454 ?
O3 Cd1 C7 113.5(16) . 4_566 ?
O3 Cd1 O2 87.2(18) . 4_566 ?
O3 Cd1 O1 139.4(15) . 4_566 ?
N1" Cd1 O4 88(5) 1_454 . ?
N1" Cd1 O4 82(6) 1_454 3 ?
N1" Cd1 C7 92(5) 1_454 4_566 ?
N1" Cd1 O2 96(6) 1_454 4_566 ?
N1" Cd1 O1 91(4) 1_454 4_566 ?
O2 Cd1 O4 138(2) 4_566 . ?
O2 Cd1 O4 142.5(13) 4_566 3 ?
O2 Cd1 C7 26.4(15) 4_566 4_566 ?
O2 Cd1 O1 52.5(17) 4_566 4_566 ?
O1 Cd1 O4 90.0(13) 4_566 3 ?
O1 Cd1 O4 169.3(19) 4_566 . ?
O1 Cd1 C7 26.3(11) 4_566 4_566 ?
Cd1 O4 Cd1 100.6(18) 3 . ?
C8 O4 Cd1 166(3) . 3 ?
C8 O4 Cd1 93(3) . . ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' N2' 128(3) . . ?
C5' C4' N2' 112(3) . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 119.7(13) . . ?
C6' N1' Cd1 119.7(14) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.5(9) . . ?
C3 C4 C8 119.5(9) . . ?
C4 C5 H5 120.0 . . ?
C9 C5 C4 120.0 . . ?
C9 C5 H5 120.0 . . ?
C5 C9 H9 120.0 . . ?
C5 C9 C1 120.0 . . ?
C1 C9 H9 120.0 . . ?
C9 C1 C7 120.2(9) . . ?
C2 C1 C9 120.0 . . ?
C2 C1 C7 119.7(9) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O3 Cd1 104(4) . . ?
N2" N2' C4' 102(4) . . ?
N2' N2" C4" 101(4) . . ?
C3" C4" N2" 117(3) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 123(3) . . ?
C4" C3" H3" 120.0 . . ?
C4" C3" C2" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
N1" C2" C3" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 121.7(14) . 1_656 ?
C2" N1" C6" 120.0 . . ?
C6" N1" Cd1 117.7(15) . 1_656 ?
N1" C6" H6" 120.0 . . ?
N1" C6" C5" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 177(3) . 4_665 ?
O2 C7 Cd1 59(3) . 4_665 ?
O2 C7 C1 119(4) . . ?
O1 C7 Cd1 61(3) . 4_665 ?
O1 C7 C1 121(3) . . ?
O1 C7 O2 119(5) . . ?
C7 O2 Cd1 95(4) . 4_665 ?
O4 C8 C4 122(3) . . ?
O4 C8 O3 112(5) . . ?
O3 C8 C4 126(4) . . ?
C7 O1 Cd1 93(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 C4 180(4) . . . . ?
Cd1 O4 C8 C4 17(22) 3 . . . ?
Cd1 O4 C8 O3 3(5) . . . . ?
Cd1 O4 C8 O3 -160(15) 3 . . . ?
Cd1 O3 C8 O4 -3(6) . . . . ?
Cd1 O3 C8 C4 180(4) . . . . ?
Cd1 N1" C6" C5" -172(2) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' 178(5) . . . . ?
C3' C2' N1' Cd1 -171.2(19) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -16(8) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" 180(6) . . . . ?
C5' C4' N2' N2" 162(5) . . . . ?
C5' C6' N1' Cd1 171.2(18) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C9 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 -2(7) . . . . ?
C5 C4 C8 O3 174(4) . . . . ?
C5 C9 C1 C2 0.0 . . . . ?
C5 C9 C1 C7 -176(3) . . . . ?
C9 C1 C2 C3 0.0 . . . . ?
C9 C1 C7 O2 -8(6) . . . . ?
C9 C1 C7 O1 -176(4) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 -177(4) . . . 4_665 ?
C1 C7 O1 Cd1 176(4) . . . 4_665 ?
C2 C1 C7 O2 176(3) . . . . ?
C2 C1 C7 O1 7(7) . . . . ?
C3 C4 C5 C9 0.0 . . . . ?
C3 C4 C8 O4 178(5) . . . . ?
C3 C4 C8 O3 -6(6) . . . . ?
N2' C4' C5' C6' -178(4) . . . . ?
N2' N2" C4" C3" -162(5) . . . . ?
N2' N2" C4" C5" 13(7) . . . . ?
N2" C4" C3" C2" 175(4) . . . . ?
N2" C4" C5" C6" -175(5) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 171(2) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 176(3) . . . . ?
O2 C7 O1 Cd1 8(6) . . . 4_665 ?
C8 C4 C5 C9 180(3) . . . . ?
C8 C4 C3 C2 -180(3) . . . . ?
O1 C7 O2 Cd1 -8(6) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.149 0.500 251.7 69.8 ?
2 0.500 -0.252 0.000 251.7 69.8 ?

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_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 2.608
_oxdiff_exptl_absorpt_empirical_full_min 0.656
####################################################################### 
# 
# 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_CdBDCAZPYDMF_0_8_GPa_MEW
_database_code_depnum_ccdc_archive 'CCDC 2046199'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-05-18 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT023_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..       0.53 Ang-1
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT029_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.442 Why?
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_RINTA01_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT020_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.220 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT084_CdBDCAZPYDMF_0_8_GPa_MEW 
;
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_PLAT088_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.35 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT342_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0375 Ang.
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT910_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         39 Note
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
_vrf_PLAT911_CdBDCAZPYDMF_0_8_GPa_MEW 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.526        186 Report
RESPONSE: The data come from high-pressure studies and are limited by  the DAC opening angle.
;
# Added during the CSD deposition process: Tuesday 18 May 2021 12:14 PM
# end Validation Reply Form

_audit_creation_date             2020-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_name_common            AMU3
_chemical_name_systematic        CdBDCAZPY*DMF
_chemical_formula_moiety         'C18 H12 Cd N4 O4'
_chemical_formula_sum            'C18 H12 Cd N4 O4'
_chemical_formula_weight         460.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H16N6O5Cd
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                   12.162(3)
_cell_length_b                   13.928(18)
_cell_length_c                   12.574(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.67(3)
_cell_angle_gamma                90
_cell_volume                     1951(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.4630
_cell_measurement_theta_min      5.8450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.911
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -4 9 0.0855
-42 9 -14 0.1945
-3 19 6 0.0396
2 -19 -5 0.0279
14 4 -14 0.0405
-15 -3 14 0.0718

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.076
loop_
_exptl_transmission_factor_max
?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2204
_diffrn_reflns_av_unetI/netI     0.1506
_diffrn_reflns_Laue_measured_fraction_full 0.442
_diffrn_reflns_Laue_measured_fraction_max 0.442
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7377
_diffrn_reflns_point_group_measured_fraction_full 0.442
_diffrn_reflns_point_group_measured_fraction_max 0.442
_diffrn_reflns_theta_full        21.965
_diffrn_reflns_theta_max         21.965
_diffrn_reflns_theta_min         5.510
_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 0.442
_diffrn_measured_fraction_theta_max 0.442
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.80(2) GPa (800000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
;
_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      0.0005681000
_diffrn_orient_matrix_UB_12      -0.0507098000
_diffrn_orient_matrix_UB_13      -0.0056568000
_diffrn_orient_matrix_UB_21      -0.0274425000
_diffrn_orient_matrix_UB_22      0.0046584000
_diffrn_orient_matrix_UB_23      -0.0612795000
_diffrn_orient_matrix_UB_31      0.0574242000
_diffrn_orient_matrix_UB_32      0.0026884000
_diffrn_orient_matrix_UB_33      -0.0017787000
_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                519
_reflns_number_total             1054
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.3 (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         0.948
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1054
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.1962
_refine_ls_R_factor_gt           0.1204
_refine_ls_restrained_S_all      0.995
_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          0.2983
_refine_ls_wR_factor_ref         0.3597
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O6-C8 \\sim C8-O4
 with sigma of 0.02
 C2-C7 \\sim C7-C9
 with sigma of 0.02
 C3-C8 \\sim C8-C5
 with sigma of 0.02
 O1-C7 \\sim C7-O2
 with sigma of 0.02
 O6-C4 \\sim C4-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1" \\sim C2" \\sim C3" \\sim C4" \\sim C5" \\sim C6": within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N1") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2") = Uanis(N2') = Uanis(C4') = Uanis(C3') = Uanis(C2') = Uanis(N1') =
Uanis(C6') = Uanis(C5')
4. Rigid body (RIGU) restrains
 O6, Cd1, N1', O4, C2', C6', C8, C3', C5', C4, C4', C5, C3, N2', C9, C2, N2",
 C1, C4", C7, C3", C5", O2, O1, C2", C6", N1"
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C3'(H3'), C5'(H5'), C6'(H6'), C5(H5), C9(H9), C2(H2), C3(H3),
 C3"(H3"), C2"(H2"), C6"(H6"), C5"(H5")
5.b Fitted hexagon refined as free rotating group:
 C2'(C3',C4',C5',C6',N1'), C4(C5,C9,C1,C2,C3), C4"(C3",C2",N1",C6",C5")
;
_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 -0.0617(2) 0.0978(5) 0.06538(19) 0.076(5) Uani 1 1 d . . . . .
O4 O 0.054(3) 0.070(3) -0.057(3) 0.075(15) Uani 1 1 d D . . . .
C2' C 0.1215(19) 0.026(3) 0.321(2) 0.084(15) Uani 1 1 d G . . . .
H2' H 0.056650 -0.012280 0.315859 0.101 Uiso 1 1 calc R U . . .
C3' C 0.226(2) 0.026(3) 0.4221(19) 0.084(15) Uani 1 1 d G . . . .
H3' H 0.230287 -0.010786 0.485183 0.101 Uiso 1 1 calc R U . . .
C4' C 0.3225(17) 0.083(3) 0.4292(17) 0.084(15) Uani 1 1 d G . . . .
C5' C 0.3153(18) 0.139(3) 0.335(2) 0.084(15) Uani 1 1 d G . . . .
H5' H 0.380193 0.176331 0.339597 0.101 Uiso 1 1 calc R U . . .
C6' C 0.211(2) 0.138(3) 0.2334(18) 0.084(15) Uani 1 1 d G . . . .
H6' H 0.206558 0.174839 0.170273 0.101 Uiso 1 1 calc R U . . .
N1' N 0.1144(16) 0.081(3) 0.2263(16) 0.084(15) Uani 1 1 d G . . . .
C4 C 0.1314(14) 0.1993(19) -0.1269(13) 0.061(15) Uani 1 1 d DG . . . .
C5 C 0.1859(15) 0.1412(18) -0.1816(15) 0.042(14) Uani 1 1 d DG . . . .
H5 H 0.181470 0.074727 -0.177274 0.051 Uiso 1 1 calc R U . . .
C9 C 0.2471(13) 0.1824(19) -0.2427(13) 0.054(16) Uani 1 1 d DG . . . .
H9 H 0.283527 0.143564 -0.279254 0.065 Uiso 1 1 calc R U . . .
C1 C 0.2537(13) 0.2818(19) -0.2491(12) 0.038(14) Uani 1 1 d G . . . .
C2 C 0.1992(15) 0.3398(18) -0.1945(15) 0.053(15) Uani 1 1 d DG . . . .
H2 H 0.203659 0.406292 -0.198761 0.064 Uiso 1 1 calc R U . . .
C3 C 0.1381(14) 0.2986(19) -0.1334(14) 0.052(15) Uani 1 1 d DG . . . .
H3 H 0.101601 0.337457 -0.096780 0.063 Uiso 1 1 calc R U . . .
O6 O 0.0183(19) 0.204(4) -0.0113(19) 0.081(14) Uani 1 1 d D . . . .
N2' N 0.440(2) 0.079(5) 0.530(3) 0.084(15) Uani 1 1 d . . . . .
N2" N 0.426(3) 0.052(5) 0.622(3) 0.084(15) Uani 1 1 d . . . . .
C4" C 0.5450(17) 0.076(4) 0.7127(18) 0.096(15) Uani 1 1 d G U . . .
C3" C 0.560(2) 0.022(4) 0.810(2) 0.108(15) Uani 1 1 d G U . . .
H3" H 0.496990 -0.015386 0.811547 0.130 Uiso 1 1 calc R U . . .
C2" C 0.669(2) 0.023(3) 0.9061(18) 0.101(13) Uani 1 1 d G U . . .
H2" H 0.679461 -0.013551 0.971360 0.121 Uiso 1 1 calc R U . . .
N1" N 0.7636(15) 0.078(3) 0.9042(14) 0.064(7) Uani 1 1 d G U . . .
C6" C 0.7485(19) 0.133(3) 0.8066(18) 0.094(13) Uani 1 1 d G U . . .
H6" H 0.811564 0.169759 0.805395 0.112 Uiso 1 1 calc R U . . .
C5" C 0.639(2) 0.132(3) 0.7109(17) 0.089(14) Uani 1 1 d G U . . .
H5" H 0.629094 0.167925 0.645581 0.107 Uiso 1 1 calc R U . . .
C7 C 0.325(4) 0.327(3) -0.308(3) 0.057(16) Uani 1 1 d D . . . .
O2 O 0.366(2) 0.265(3) -0.3595(17) 0.070(15) Uani 1 1 d D . . . .
C8 C 0.063(4) 0.156(3) -0.064(4) 0.050(15) Uani 1 1 d D . . . .
O1 O 0.327(3) 0.419(4) -0.320(3) 0.070(14) Uani 1 1 d 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
Cd1 O4 2.50(2) . ?
Cd1 O4 2.35(4) 3 ?
Cd1 N1' 2.292(16) . ?
Cd1 O6 2.20(4) . ?
Cd1 N1" 2.29(3) 1_454 ?
Cd1 C7 2.70(4) 4_566 ?
Cd1 O2 2.45(4) 4_566 ?
Cd1 O1 2.35(2) 4_566 ?
O4 C8 1.21(3) . ?
C2' H2' 0.9300 . ?
C2' C3' 1.3900 . ?
C2' N1' 1.3900 . ?
C3' H3' 0.9300 . ?
C3' C4' 1.3900 . ?
C4' C5' 1.3900 . ?
C4' N2' 1.49(3) . ?
C5' H5' 0.9300 . ?
C5' C6' 1.3900 . ?
C6' H6' 0.9300 . ?
C6' N1' 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C4 C8 1.48(5) . ?
C5 H5 0.9300 . ?
C5 C9 1.3900 . ?
C9 H9 0.9300 . ?
C9 C1 1.3900 . ?
C1 C2 1.3900 . ?
C1 C7 1.49(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.3900 . ?
C3 H3 0.9300 . ?
O6 C8 1.21(3) . ?
N2' N2" 1.29(5) . ?
N2" C4" 1.47(4) . ?
C4" C3" 1.3900 . ?
C4" C5" 1.3900 . ?
C3" H3" 0.9300 . ?
C3" C2" 1.3900 . ?
C2" H2" 0.9300 . ?
C2" N1" 1.3900 . ?
N1" C6" 1.3900 . ?
C6" H6" 0.9300 . ?
C6" C5" 1.3900 . ?
C5" H5" 0.9300 . ?
C7 O2 1.29(4) . ?
C7 O1 1.30(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
O4 Cd1 O4 77.1(11) 3 . ?
O4 Cd1 C7 116.9(9) 3 4_566 ?
O4 Cd1 C7 165.9(13) . 4_566 ?
O4 Cd1 O2 145.3(10) 3 4_566 ?
N1' Cd1 O4 84.3(14) . 3 ?
N1' Cd1 O4 88.2(11) . . ?
N1' Cd1 C7 92.0(12) . 4_566 ?
N1' Cd1 O2 95.3(11) . 4_566 ?
N1' Cd1 O1 90.7(10) . 4_566 ?
O6 Cd1 O4 128.3(11) . 3 ?
O6 Cd1 O4 51.2(16) . . ?
O6 Cd1 N1' 92.0(10) . . ?
O6 Cd1 N1" 96(4) . 1_454 ?
O6 Cd1 C7 114.7(12) . 4_566 ?
O6 Cd1 O2 86.4(14) . 4_566 ?
O6 Cd1 O1 143.4(17) . 4_566 ?
N1" Cd1 O4 83(6) 1_454 3 ?
N1" Cd1 O4 89(4) 1_454 . ?
N1" Cd1 N1' 167(6) 1_454 . ?
N1" Cd1 C7 93(5) 1_454 4_566 ?
N1" Cd1 O2 95(6) 1_454 4_566 ?
N1" Cd1 O1 88(4) 1_454 4_566 ?
O2 Cd1 O4 137.6(13) 4_566 . ?
O2 Cd1 C7 28.4(9) 4_566 4_566 ?
O1 Cd1 O4 165.4(19) 4_566 . ?
O1 Cd1 O4 88.3(16) 4_566 3 ?
O1 Cd1 C7 28.7(10) 4_566 4_566 ?
O1 Cd1 O2 57.0(19) 4_566 4_566 ?
Cd1 O4 Cd1 102.9(11) 3 . ?
C8 O4 Cd1 89(3) . . ?
C8 O4 Cd1 168(3) . 3 ?
C3' C2' H2' 120.0 . . ?
C3' C2' N1' 120.0 . . ?
N1' C2' H2' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' N2' 122(3) . . ?
C5' C4' C3' 120.0 . . ?
C5' C4' N2' 117(3) . . ?
C4' C5' H5' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C5' C6' N1' 120.0 . . ?
N1' C6' H6' 120.0 . . ?
C2' N1' Cd1 121.7(13) . . ?
C6' N1' Cd1 117.8(14) . . ?
C6' N1' C2' 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.5(8) . . ?
C3 C4 C8 119.4(7) . . ?
C4 C5 H5 120.0 . . ?
C9 C5 C4 120.0 . . ?
C9 C5 H5 120.0 . . ?
C5 C9 H9 120.0 . . ?
C1 C9 C5 120.0 . . ?
C1 C9 H9 120.0 . . ?
C9 C1 C2 120.0 . . ?
C9 C1 C7 120.6(8) . . ?
C2 C1 C7 119.3(8) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C8 O6 Cd1 104(3) . . ?
N2" N2' C4' 110(3) . . ?
N2' N2" C4" 101(3) . . ?
C3" C4" N2" 107(3) . . ?
C3" C4" C5" 120.0 . . ?
C5" C4" N2" 132(2) . . ?
C4" C3" H3" 120.0 . . ?
C2" C3" C4" 120.0 . . ?
C2" C3" H3" 120.0 . . ?
C3" C2" H2" 120.0 . . ?
C3" C2" N1" 120.0 . . ?
N1" C2" H2" 120.0 . . ?
C2" N1" Cd1 122.0(12) . 1_656 ?
C2" N1" C6" 120.0 . . ?
C6" N1" Cd1 117.6(13) . 1_656 ?
N1" C6" H6" 120.0 . . ?
C5" C6" N1" 120.0 . . ?
C5" C6" H6" 120.0 . . ?
C4" C5" H5" 120.0 . . ?
C6" C5" C4" 120.0 . . ?
C6" C5" H5" 120.0 . . ?
C1 C7 Cd1 174(3) . 4_665 ?
O2 C7 Cd1 65(2) . 4_665 ?
O2 C7 C1 113(3) . . ?
O2 C7 O1 125(4) . . ?
O1 C7 Cd1 60(2) . 4_665 ?
O1 C7 C1 121(2) . . ?
C7 O2 Cd1 87(3) . 4_665 ?
O4 C8 C4 122(2) . . ?
O4 C8 O6 115(5) . . ?
O6 C8 C4 123(3) . . ?
C7 O1 Cd1 91(3) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O4 C8 C4 178(4) . . . . ?
Cd1 O4 C8 C4 -1(26) 3 . . . ?
Cd1 O4 C8 O6 -177(18) 3 . . . ?
Cd1 O4 C8 O6 2(5) . . . . ?
Cd1 O6 C8 O4 -2(6) . . . . ?
Cd1 O6 C8 C4 -178(3) . . . . ?
Cd1 N1" C6" C5" -173.0(19) 1_656 . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' N2' -173(4) . . . . ?
C3' C2' N1' Cd1 -172(2) . . . . ?
C3' C2' N1' C6' 0.0 . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C3' C4' N2' N2" -27(6) . . . . ?
C4' C5' C6' N1' 0.0 . . . . ?
C4' N2' N2" C4" -166(5) . . . . ?
C5' C4' N2' N2" 160(4) . . . . ?
C5' C6' N1' Cd1 172.5(19) . . . . ?
C5' C6' N1' C2' 0.0 . . . . ?
N1' C2' C3' C4' 0.0 . . . . ?
C4 C5 C9 C1 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C5 C4 C8 O4 1(7) . . . . ?
C5 C4 C8 O6 177(3) . . . . ?
C5 C9 C1 C2 0.0 . . . . ?
C5 C9 C1 C7 176(2) . . . . ?
C9 C1 C2 C3 0.0 . . . . ?
C9 C1 C7 O2 7(4) . . . . ?
C9 C1 C7 O1 176(4) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C1 C7 O2 Cd1 174(3) . . . 4_665 ?
C1 C7 O1 Cd1 -174(3) . . . 4_665 ?
C2 C1 C7 O2 -177(2) . . . . ?
C2 C1 C7 O1 -7(6) . . . . ?
C3 C4 C5 C9 0.0 . . . . ?
C3 C4 C8 O4 180(5) . . . . ?
C3 C4 C8 O6 -4(5) . . . . ?
N2' C4' C5' C6' 173(4) . . . . ?
N2' N2" C4" C3" -159(3) . . . . ?
N2' N2" C4" C5" 14(6) . . . . ?
N2" C4" C3" C2" 174(3) . . . . ?
N2" C4" C5" C6" -172(5) . . . . ?
C4" C3" C2" N1" 0.0 . . . . ?
C3" C4" C5" C6" 0.0 . . . . ?
C3" C2" N1" Cd1 173(2) . . . 1_656 ?
C3" C2" N1" C6" 0.0 . . . . ?
C2" N1" C6" C5" 0.0 . . . . ?
N1" C6" C5" C4" 0.0 . . . . ?
C5" C4" C3" C2" 0.0 . . . . ?
C7 C1 C2 C3 -176(2) . . . . ?
O2 C7 O1 Cd1 -6(5) . . . 4_665 ?
C8 C4 C5 C9 178(2) . . . . ?
C8 C4 C3 C2 -178(2) . . . . ?
O1 C7 O2 Cd1 5(5) . . . 4_665 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.484 0.500 255.9 62.2 ?
2 0.500 -0.577 0.000 255.9 62.2 ?

_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.0
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   207
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.064
_oxdiff_exptl_absorpt_empirical_full_min 0.562
