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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262368'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.305 Report
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT029_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.342 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT088_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.94 Note
RESPONSE: The data/parameter ratio is affected by the access
 limits of the DAC.
;
_vrf_PLAT026_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        35% Check
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT341_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0475 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_0_7_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        215 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2021-08-18
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2 Cu F8 N6'
_chemical_formula_weight         551.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         C6H13BCuF3N2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.23(3)
_cell_length_b                   13.517(6)
_cell_length_c                   26.501(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4737(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    422
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6340
_cell_measurement_theta_min      3.0620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.07
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3050
_diffrn_reflns_av_unetI/netI     0.2442
_diffrn_reflns_Laue_measured_fraction_full 0.342
_diffrn_reflns_Laue_measured_fraction_max 0.258
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            2412
_diffrn_reflns_point_group_measured_fraction_full 0.342
_diffrn_reflns_point_group_measured_fraction_max 0.258
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.547
_diffrn_reflns_theta_min         3.075
_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 0.342
_diffrn_measured_fraction_theta_max 0.258
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 0.70(2) GPa
 (700000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega    4.40   23.90   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -16.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega    4.40   23.90   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  164.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -63.00   -8.25   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -33.0000 73

#__ type_ start__ end____ width___ exp.time_
 10 omega  -63.00   -8.25   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  147.0000 73

#__ type_ start__ end____ width___ exp.time_
 11 omega   -3.10   11.90   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  147.0000 20

#__ type_ start__ end____ width___ exp.time_
 12 omega   -3.10   11.90   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -33.0000 20

#__ type_ start__ end____ width___ exp.time_
 13 omega  -34.00  -18.25   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -60.0000 21

#__ type_ start__ end____ width___ exp.time_
 14 omega  -34.00  -18.25   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  120.0000 21

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -57.75   0.7500   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  120.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0518931000
_diffrn_orient_matrix_UB_12      0.0136249000
_diffrn_orient_matrix_UB_13      0.0000357000
_diffrn_orient_matrix_UB_21      -0.0045695000
_diffrn_orient_matrix_UB_22      0.0166670000
_diffrn_orient_matrix_UB_23      -0.0251938000
_diffrn_orient_matrix_UB_31      -0.0133604000
_diffrn_orient_matrix_UB_32      0.0476749000
_diffrn_orient_matrix_UB_33      0.0088350000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                135
_reflns_number_total             390
_reflns_odcompleteness_completeness 33.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         390
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.2445
_refine_ls_R_factor_gt           0.0869
_refine_ls_restrained_S_all      0.841
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1521P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2116
_refine_ls_wR_factor_ref         0.2934
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C3_$1
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(F1) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, B1, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.375000 0.375000 0.375000 0.093(5) Uani 1 4 d S T P . .
N1 N 0.487(2) 0.3886(10) 0.4284(5) 0.105(7) Uani 1 1 d . U . . .
H1A H 0.529911 0.435028 0.417542 0.126 Uiso 1 1 calc R U . . .
H1B H 0.458757 0.411878 0.456379 0.126 Uiso 1 1 calc R U . . .
C3 C 0.7024(18) 0.241(2) 0.4875(14) 0.163(18) Uani 1 1 d D U . . .
H3A H 0.663270 0.198432 0.509629 0.196 Uiso 1 1 calc R U . . .
H3B H 0.717534 0.202151 0.457578 0.196 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.5597(16) 0.375000 0.11(2) Uani 1 2 d S TU P . .
C1 C 0.548(4) 0.3034(16) 0.4430(8) 0.105(11) Uani 1 1 d . U . . .
H1C H 0.505404 0.258609 0.461918 0.126 Uiso 1 1 calc R U . . .
H1D H 0.568485 0.269238 0.412398 0.126 Uiso 1 1 calc R U . . .
C2 C 0.635(4) 0.3213(18) 0.4715(9) 0.128(12) Uani 1 1 d . U . . .
H2A H 0.613464 0.355383 0.501836 0.153 Uiso 1 1 calc R U . . .
H2B H 0.675958 0.367757 0.452478 0.153 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.7538(19) 0.375000 0.19(4) Uani 1 2 d S TU P . .
H5A H 0.364012 0.777432 0.341290 0.290 Uiso 0.5 1 calc R U P A -1
H5B H 0.438994 0.777432 0.387106 0.290 Uiso 0.5 1 calc R U P A -1
H5C H 0.321993 0.777432 0.396603 0.290 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.641(2) 0.375000 0.13(3) Uani 1 2 d S TU P . .
B1 B 0.625000 0.125000 0.3107(18) 0.134(14) Uani 1 2 d S TU P . .
F1 F 0.668(3) 0.1947(11) 0.3451(5) 0.201(17) Uani 1 1 d . U . . .
F2 F 0.557(2) 0.1698(11) 0.2870(4) 0.166(11) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.06(2) . ?
Cu1 N1 2.06(2) 7 ?
Cu1 N1 2.06(2) 12 ?
Cu1 N1 2.06(2) 14 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.46(3) . ?
C3 C3 1.44(2) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.47(4) . ?
N2 C4 1.10(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.39(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 1.0663 . ?
C5 H5B 1.0663 . ?
C5 H5C 1.0663 . ?
C5 C4 1.52(4) . ?
B1 F1 1.43(4) . ?
B1 F1 1.43(4) 2_655 ?
B1 F2 1.25(3) 2_655 ?
B1 F2 1.25(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 169.8(8) . 12 ?
N1 Cu1 N1 169.8(8) 14 7 ?
N1 Cu1 N1 93.3(13) 12 7 ?
N1 Cu1 N1 93.3(13) . 14 ?
N1 Cu1 N1 87.7(14) 12 14 ?
N1 Cu1 N1 87.7(14) . 7 ?
Cu1 N1 H1A 107.2 . . ?
Cu1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C1 N1 Cu1 120.6(16) . . ?
C1 N1 H1A 107.2 . . ?
C1 N1 H1B 107.2 . . ?
C3 C3 H3A 106.8 29_656 . ?
C3 C3 H3B 106.8 29_656 . ?
C3 C3 C2 122(3) 29_656 . ?
H3A C3 H3B 106.6 . . ?
C2 C3 H3A 106.7 . . ?
C2 C3 H3B 106.8 . . ?
N1 C1 H1C 107.9 . . ?
N1 C1 H1D 108.0 . . ?
H1C C1 H1D 107.2 . . ?
C2 C1 N1 117(2) . . ?
C2 C1 H1C 107.9 . . ?
C2 C1 H1D 108.0 . . ?
C3 C2 H2A 106.9 . . ?
C3 C2 H2B 106.9 . . ?
C1 C2 C3 122(2) . . ?
C1 C2 H2A 107.0 . . ?
C1 C2 H2B 106.8 . . ?
H2A C2 H2B 106.7 . . ?
H5A C5 H5B 97.3 . . ?
H5A C5 H5C 97.3 . . ?
H5B C5 H5C 97.3 . . ?
C4 C5 H5A 119.9 . . ?
C4 C5 H5B 119.9 . . ?
C4 C5 H5C 119.9 . . ?
N2 C4 C5 180.000(12) . . ?
F1 B1 F1 101(3) . 2_655 ?
F2 B1 F1 106.5(13) 2_655 2_655 ?
F2 B1 F1 106.5(13) . . ?
F2 B1 F1 111(2) . 2_655 ?
F2 B1 F1 111(2) 2_655 . ?
F2 B1 F2 120(5) . 2_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 168(3) . . . . ?
N1 C1 C2 C3 -179(3) . . . . ?
C3 C3 C2 C1 174(5) 29_656 . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 14 43 0.1000 -0.0095 13.9491 42.9022 0.1911 -0.8483 1.0442
21 0 27 0.1000 20.9241 0.0869 27.0259 1.0880 -0.7751 -0.0366
21 0 -27 0.1000 20.9489 0.2148 -26.8994 1.0891 0.5856 -0.5073
0 14 -43 0.1000 0.0300 14.1529 -42.9789 0.1929 1.3186 0.2946
-13 22 0 0.1000 -12.9445 21.9868 -0.0994 -0.3722 0.4281 1.2203
0 -14 43 0.1000 -0.0300 -14.1529 42.9789 -0.1929 -1.3186 -0.2946
13 -22 0 0.1000 12.9445 -21.9868 0.0994 0.3722 -0.4281 -1.2203
0 -14 -43 0.1000 0.0095 -13.9491 -42.9022 -0.1911 0.8483 -1.0442
-21 0 -27 0.1000 -20.9241 -0.0869 -27.0259 -1.0880 0.7751 0.0366
-21 0 27 0.1000 -20.9489 -0.2148 26.8994 -1.0891 -0.5856 0.5073
13 22 0 0.1000 12.9769 22.1735 -0.0211 0.9755 0.3108 0.8836
-13 -22 0 0.1000 -12.9769 -22.1735 0.0211 -0.9755 -0.3108 -0.8836

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100_K_Cu_HDA_2_MeCN_2x2BF4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262370'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_100_K_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.901 Why?
RESPONSE: These reflections were probably affected by unexpected 
deviations in their intensities for symmetry equivalent measurements 
and omitted during initial data reduction.
;
_vrf_PLAT911_100_K_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        111 Report
RESPONSE: These reflections were probably affected by unexpected 
deviations in their intensities for symmetry equivalent measurements
 and omitted during initial data reduction.
;
_audit_creation_date             2021-08-18
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2.07 Cu F8.02 N6'
_chemical_formula_weight         552.87
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.084(2)
_cell_length_b                   13.9110(14)
_cell_length_c                   27.113(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4934.9(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1082
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      27.5110
_cell_measurement_theta_min      3.2700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.34a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.111
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3465
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.921
_diffrn_reflns_theta_min         3.005
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00  82.00   1.00    5.00    --   17.63  57.00-180.00   60
  2  ω    -21.00  36.00   1.00    5.00    --  -18.72  57.00 -60.00   57
  3  ω     -5.00  23.00   1.00    5.00    --  -18.72 -99.00-120.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315292000
_diffrn_orient_matrix_UB_12      -0.0345211000
_diffrn_orient_matrix_UB_13      0.0118035000
_diffrn_orient_matrix_UB_21      -0.0436780000
_diffrn_orient_matrix_UB_22      0.0284158000
_diffrn_orient_matrix_UB_23      -0.0053847000
_diffrn_orient_matrix_UB_31      -0.0061532000
_diffrn_orient_matrix_UB_32      -0.0245471000
_diffrn_orient_matrix_UB_33      -0.0227021000
_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                1115
_reflns_number_total             1277
_reflns_odcompleteness_completeness 77.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.86
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.34a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.067
_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)+(0.0560P)²+33.8820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1229
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.375000 0.375000 0.375000 0.0133(2) Uani 1 4 d S T P . .
N1 N 0.4864(2) 0.38904(16) 0.42707(8) 0.0177(6) Uani 1 1 d . . . . .
H1A H 0.531368 0.431645 0.415717 0.021 Uiso 1 1 calc R U . . .
H1B H 0.457583 0.414975 0.453660 0.021 Uiso 1 1 calc R U . . .
C3 C 0.6997(3) 0.2395(2) 0.48736(13) 0.0296(8) Uani 1 1 d . . . . .
H3A H 0.656370 0.204152 0.510026 0.036 Uiso 1 1 calc R U . . .
H3B H 0.712668 0.198285 0.459175 0.036 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.5559(2) 0.375000 0.0236(9) Uani 1 2 d S T P . .
C1 C 0.5448(3) 0.30399(19) 0.44365(12) 0.0231(7) Uani 1 1 d . . . . .
H1C H 0.560549 0.264495 0.415172 0.028 Uiso 1 1 calc R U . . .
H1D H 0.501957 0.266234 0.465523 0.028 Uiso 1 1 calc R U . . .
C2 C 0.6424(3) 0.3278(2) 0.46990(12) 0.0251(7) Uani 1 1 d . . . . .
H2A H 0.627041 0.368089 0.498129 0.030 Uiso 1 1 calc R U . . .
H2B H 0.686095 0.364254 0.447878 0.030 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.7416(4) 0.375000 0.0541(18) Uani 1 2 d S T P . .
H5A H 0.433699 0.764587 0.357336 0.081 Uiso 0.5 1 calc R U P A -1
H5B H 0.377351 0.764587 0.408363 0.081 Uiso 0.5 1 calc R U P A -1
H5C H 0.313950 0.764587 0.359301 0.081 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.6367(4) 0.375000 0.0320(12) Uani 1 2 d S T P . .
B1 B 0.625000 0.125000 0.31443(17) 0.0233(11) Uani 1 2 d S T P . .
F1 F 0.6558(2) 0.19936(16) 0.34424(9) 0.0547(7) Uani 1 1 d . . . . .
F2 F 0.5486(2) 0.15935(19) 0.28529(9) 0.0620(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.039(2) 12 ?
Cu1 N1 2.039(2) . ?
Cu1 N1 2.039(2) 7 ?
Cu1 N1 2.039(2) 14 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.478(4) . ?
C3 C3 1.512(7) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.515(4) . ?
N2 C4 1.125(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.500(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C5 C4 1.458(8) . ?
B1 F1 1.373(3) 2_655 ?
B1 F1 1.373(3) . ?
B1 F2 1.361(4) . ?
B1 F2 1.361(4) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 92.34(15) 12 7 ?
N1 Cu1 N1 88.72(15) 7 . ?
N1 Cu1 N1 169.00(12) 12 . ?
N1 Cu1 N1 88.72(15) 12 14 ?
N1 Cu1 N1 169.00(12) 7 14 ?
N1 Cu1 N1 92.34(15) 14 . ?
Cu1 N1 H1A 107.3 . . ?
Cu1 N1 H1B 107.3 . . ?
H1A N1 H1B 106.9 . . ?
C1 N1 Cu1 120.22(18) . . ?
C1 N1 H1A 107.3 . . ?
C1 N1 H1B 107.3 . . ?
C3 C3 H3A 108.6 29_656 . ?
C3 C3 H3B 108.6 29_656 . ?
C3 C3 C2 114.5(3) 29_656 . ?
H3A C3 H3B 107.6 . . ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
N1 C1 H1C 108.7 . . ?
N1 C1 H1D 108.7 . . ?
N1 C1 C2 114.1(2) . . ?
H1C C1 H1D 107.6 . . ?
C2 C1 H1C 108.7 . . ?
C2 C1 H1D 108.7 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 C3 113.0(3) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
N2 C4 C5 180.0 . . ?
F1 B1 F1 107.9(4) 2_655 . ?
F2 B1 F1 112.96(18) . 2_655 ?
F2 B1 F1 107.04(15) . . ?
F2 B1 F1 112.97(18) 2_655 . ?
F2 B1 F1 107.04(15) 2_655 2_655 ?
F2 B1 F2 109.0(4) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 162.8(2) . . . . ?
N1 C1 C2 C3 178.9(3) . . . . ?
C3 C3 C2 C1 178.2(4) 29_656 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.724
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_0_0001_GPa_Cd_HDA_2_NO3_2
_database_code_depnum_ccdc_archive 'CCDC 2262371'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-09-26 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# Added during the CSD deposition process: Thursday 11 May 2023 01:25 PM
# end Validation Reply Form
_audit_creation_date             2023-05-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_chemical_name_common            Cd_HDA_2_NO3_2
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H16 Cd0.5 N2, N O3'
_chemical_formula_sum            'C6 H16 Cd0.50 N3 O3'
_chemical_formula_weight         234.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cd C6 H12 N2 N O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   9.7855(7)
_cell_length_b                   9.7855(7)
_cell_length_c                   21.071(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2017.7(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    949
_cell_measurement_temperature    293.1(2)
_cell_measurement_theta_max      21.9700
_cell_measurement_theta_min      3.5050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 2 -12 0.0524
-12 -2 13 0.0443
7 -7 22 0.0312
-6 7 -22 0.0328
-1 -12 -15 0.0246
1 12 16 0.0295

_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.056
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.3796 2.2253 -12.2433 0.0051 0.0077 1.0000
-12.1524 -2.4819 13.0593 -0.0138 -0.0437 -0.9989
6.5518 -6.8455 21.5993 -0.2338 -0.9704 0.0613
-5.6900 7.0110 -22.4850 0.2344 0.9721 0.0089
-0.9708 -11.9700 -14.9572 0.9703 -0.2664 0.0021
0.9705 11.9700 15.9606 -0.9934 0.2460 -0.0156

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.843
_diffrn_reflns_Laue_measured_fraction_max 0.719
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1809
_diffrn_reflns_point_group_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.719
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.783
_diffrn_reflns_theta_min         3.523
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.719
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  91.00   1.00    5.00    --   17.63   0.00   0.00  146
  2  ω    -25.00  23.00   1.00    5.00    --  -18.80 -99.00 -30.00   48
  3  ω    -40.00   1.00   1.00    5.00    --  -18.80  57.00 -90.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0131812000
_diffrn_orient_matrix_UB_12      -0.0511887000
_diffrn_orient_matrix_UB_13      -0.0230481000
_diffrn_orient_matrix_UB_21      -0.0285479000
_diffrn_orient_matrix_UB_22      0.0500642000
_diffrn_orient_matrix_UB_23      -0.0203990000
_diffrn_orient_matrix_UB_31      0.0654555000
_diffrn_orient_matrix_UB_32      0.0113070000
_diffrn_orient_matrix_UB_33      -0.0134345000
_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                678
_reflns_number_total             949
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         949
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      1.078
_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)+(0.0341P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0944
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C3A_$1-C2_$1 \\sim C3A-C3A_$1
 with sigma of 0.02
2. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2AA,H2AB), C2(H2BC,H2BD), C3B(H3BA,H3BB),
 C3A(H3AA,H3AB)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.000000 0.750000 0.375000 0.0606(3) Uani 1 4 d S T P . .
N1 N 0.8201(4) 0.5948(4) 0.35983(19) 0.0774(12) Uani 1 1 d . . . . .
H1A H 0.798822 0.561294 0.397837 0.093 Uiso 1 1 calc R U . . .
H1B H 0.748224 0.643066 0.346847 0.093 Uiso 1 1 calc R U . . .
N2 N 1.000000 0.750000 0.5257(3) 0.0818(18) Uani 1 2 d S T P . .
O1 O 1.0675(4) 0.8347(4) 0.4946(2) 0.1102(14) Uani 1 1 d . . . . .
O2 O 1.000000 0.750000 0.5823(3) 0.158(3) Uani 1 2 d S T P . .
C1 C 0.8330(6) 0.4793(5) 0.3171(3) 0.0866(16) Uani 1 1 d . . . . .
H1C H 0.916548 0.430683 0.327275 0.104 Uiso 1 1 calc R U . . .
H1D H 0.841695 0.513501 0.274097 0.104 Uiso 1 1 calc R U . . .
C2 C 0.7155(6) 0.3793(5) 0.3192(3) 0.0906(17) Uani 1 1 d . . . . .
H2AA H 0.633795 0.429649 0.330675 0.109 Uiso 0.28(2) 1 calc R U P A 1
H2AB H 0.733386 0.314793 0.353133 0.109 Uiso 0.28(2) 1 calc R U P A 1
H2BC H 0.635260 0.421677 0.300682 0.109 Uiso 0.72(2) 1 calc R U P A 2
H2BD H 0.694802 0.357740 0.363074 0.109 Uiso 0.72(2) 1 calc R U P A 2
C3B C 0.748(2) 0.2430(13) 0.2823(4) 0.101(5) Uani 0.72(2) 1 d . . P A 2
H3BA H 0.836109 0.208760 0.296561 0.122 Uiso 0.72(2) 1 calc R U P A 2
H3BB H 0.679803 0.175355 0.293238 0.122 Uiso 0.72(2) 1 calc R U P A 2
C3A C 0.682(2) 0.293(2) 0.2559(16) 0.092(9) Uani 0.28(2) 1 d D . P A 1
H3AA H 0.604307 0.233736 0.262298 0.111 Uiso 0.28(2) 1 calc R U P A 1
H3AB H 0.663913 0.353537 0.220404 0.111 Uiso 0.28(2) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.347(4) 6_664 ?
Cd1 N1 2.347(4) 16_756 ?
Cd1 N1 2.347(4) 11_676 ?
Cd1 N1 2.347(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.451(6) . ?
N2 O1 1.246(4) . ?
N2 O1 1.246(4) 6_664 ?
N2 O2 1.193(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.509(6) . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 C3B 1.576(13) . ?
C2 C3A 1.61(3) . ?
C3B C3B 1.37(2) 13_655 ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3A C3A 1.59(3) 13_655 ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 91.06(3) 6_664 16_756 ?
N1 Cd1 N1 91.06(3) 16_756 . ?
N1 Cd1 N1 91.06(3) 6_664 11_676 ?
N1 Cd1 N1 91.06(3) 11_676 . ?
N1 Cd1 N1 164.3(2) 6_664 . ?
N1 Cd1 N1 164.3(2) 16_756 11_676 ?
Cd1 N1 H1A 106.9 . . ?
Cd1 N1 H1B 106.9 . . ?
H1A N1 H1B 106.7 . . ?
C1 N1 Cd1 121.6(3) . . ?
C1 N1 H1A 106.9 . . ?
C1 N1 H1B 106.9 . . ?
O1 N2 O1 116.6(7) . 6_664 ?
O2 N2 O1 121.7(3) . . ?
O2 N2 O1 121.7(3) . 6_664 ?
N1 C1 H1C 108.5 . . ?
N1 C1 H1D 108.5 . . ?
N1 C1 C2 114.9(5) . . ?
H1C C1 H1D 107.5 . . ?
C2 C1 H1C 108.5 . . ?
C2 C1 H1D 108.5 . . ?
C1 C2 H2AA 107.8 . . ?
C1 C2 H2AB 107.8 . . ?
C1 C2 H2BC 109.2 . . ?
C1 C2 H2BD 109.2 . . ?
C1 C2 C3B 112.3(7) . . ?
C1 C2 C3A 117.9(9) . . ?
H2AA C2 H2AB 107.2 . . ?
H2BC C2 H2BD 107.9 . . ?
C3B C2 H2BC 109.2 . . ?
C3B C2 H2BD 109.2 . . ?
C3A C2 H2AA 107.8 . . ?
C3A C2 H2AB 107.8 . . ?
C2 C3B H3BA 108.7 . . ?
C2 C3B H3BB 108.7 . . ?
C3B C3B C2 114.3(16) 13_655 . ?
C3B C3B H3BA 108.7 13_655 . ?
C3B C3B H3BB 108.7 13_655 . ?
H3BA C3B H3BB 107.6 . . ?
C2 C3A H3AA 111.0 . . ?
C2 C3A H3AB 111.0 . . ?
C3A C3A C2 104(3) 13_655 . ?
C3A C3A H3AA 111.0 13_655 . ?
C3A C3A H3AB 111.0 13_655 . ?
H3AA C3A H3AB 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 N1 C1 C2 172.3(3) . . . . ?
N1 C1 C2 C3B -168.8(8) . . . . ?
N1 C1 C2 C3A 151.9(12) . . . . ?
C1 C2 C3B C3B -72(2) . . . 13_655 ?
C1 C2 C3A C3A 62(3) . . . 13_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   3097
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.889
# start Validation Reply Form
_vrf_PLAT029_0_0001_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.843 Why?
RESPONSE: These reflections were probably affected by
 unexpected deviations in their intensities for symmetry 
 equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT242_0_0001_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N2 Check
RESPONSE: RIGU restraints were applied to atoms in the disordered
 molecules. Several of the atoms were still not ideally shaped, 
 however, this does not indicate an incorrect atom-type assignment.
;
_vrf_PLAT911_0_0001_GPa_Cd_HDA_2_NO3_2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        144 Report
RESPONSE: These reflections were probably affected by unexpected 
deviations in their intensities for symmetry equivalent 
measurements and omitted during initial data reduction.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4
# Added during the CSD deposition process: Friday 12 May 2023 12:20 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2262369'
loop_
_audit_author_name
_audit_author_address
'Aleksandra Polrolniczak'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2023-05-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.386 Why?
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_RINTA01_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT020_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.205 Report
RESPONSE: We made several attempts to obtain better quality data
 for this structure however, due to absorption of the sample, disorder,
 poor crystal quality etc. crystal diffracted weakly. Furthermore the data
 come from high-pressure studies and are limited by the DAC opening angle.
;
_vrf_PLAT026_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        39% Check
RESPONSE: The data come from high-pressure studies and are limited by 
the DAC opening angle.
;
_vrf_PLAT088_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.29 Note
RESPONSE: The data/parameter ratio is affected by the access 
limits of the DAC.
;
_vrf_PLAT341_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0525 Ang.
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_vrf_PLAT911_1_0_GPa_Cu_HDA_2_MeCN_2x2BF4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        204 Report
RESPONSE: The data come from high-pressure studies and are limited by
 the DAC opening angle.
;
_audit_creation_date             2021-08-18
_chemical_name_common            Cu_HDA_2_MeCN_2x2BF4
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H32 Cu N4, C4 H6 N2, 2(B F4)'
_chemical_formula_sum            'C16 H38 B2 Cu F8 N6'
_chemical_formula_weight         551.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu NC3H8BF2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.220(10)
_cell_length_b                   13.480(3)
_cell_length_c                   26.429(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4710(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    450
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3030
_cell_measurement_theta_min      4.3880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.427
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.07
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.389     0.454
         range of gasket transmission (min-max)           0.971     1.000
         range of P media transmission (min-max)          1.000     1.000

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

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

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

    Absorption coeff of pressure medium =   0.00 mm-1
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2052
_diffrn_reflns_av_unetI/netI     0.1827
_diffrn_reflns_Laue_measured_fraction_full 0.386
_diffrn_reflns_Laue_measured_fraction_max 0.333
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            4151
_diffrn_reflns_point_group_measured_fraction_full 0.386
_diffrn_reflns_point_group_measured_fraction_max 0.333
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.460
_diffrn_reflns_theta_min         4.419
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.386
_diffrn_measured_fraction_theta_max 0.333
_diffrn_measurement_details      
;
Data were collected at room temperature and pressure of 1.00(2) GPa
 (1000000 kPa).
 Pressure was determined by monitoring the shift of the ruby R1-fluorescence line.
#__ type_ start__ end____ width___ exp.time_
  1 phi    -35.00   19.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  2 phi    140.00  200.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

#__ type_ start__ end____ width___ exp.time_
  3 phi    160.00  217.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

#__ type_ start__ end____ width___ exp.time_
  4 phi    -20.00   34.75   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

#__ type_ start__ end____ width___ exp.time_
  5 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   24.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   10.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

#__ type_ start__ end____ width___ exp.time_
 10 omega  -64.00   -8.50   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    8.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega  -43.00  -21.25   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

#__ type_ start__ end____ width___ exp.time_
 15 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

#__ type_ start__ end____ width___ exp.time_
 16 omega  -90.00  -36.00   0.7500   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0519029000
_diffrn_orient_matrix_UB_12      -0.0133048000
_diffrn_orient_matrix_UB_13      -0.0001598000
_diffrn_orient_matrix_UB_21      0.0046634000
_diffrn_orient_matrix_UB_22      -0.0161911000
_diffrn_orient_matrix_UB_23      -0.0254276000
_diffrn_orient_matrix_UB_31      0.0127604000
_diffrn_orient_matrix_UB_32      -0.0482667000
_diffrn_orient_matrix_UB_33      0.0085828000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                196
_reflns_number_total             497
_reflns_odcompleteness_completeness 9.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         497
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.2296
_refine_ls_R_factor_gt           0.0770
_refine_ls_restrained_S_all      0.920
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1462P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2656
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(F1) \\sim
Ueq, Uanis(B1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N1, C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, B1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.375000 0.375000 0.375000 0.062(4) Uani 1 4 d S T P . .
N1 N 0.4831(17) 0.3867(8) 0.4278(3) 0.074(11) Uani 1 1 d . U . . .
H1A H 0.524980 0.434272 0.417436 0.088 Uiso 1 1 calc R U . . .
H1B H 0.453208 0.409128 0.455683 0.088 Uiso 1 1 calc R U . . .
C3 C 0.708(4) 0.2401(15) 0.4854(6) 0.10(3) Uani 1 1 d . . . . .
H3A H 0.667886 0.191090 0.503396 0.121 Uiso 1 1 calc R U . . .
H3B H 0.731074 0.209038 0.454445 0.121 Uiso 1 1 calc R U . . .
N2 N 0.375000 0.5591(18) 0.375000 0.117(9) Uani 1 2 d S TU P . .
C1 C 0.547(3) 0.3017(14) 0.4431(6) 0.086(11) Uani 1 1 d . U . . .
H1C H 0.505555 0.257780 0.463617 0.103 Uiso 1 1 calc R U . . .
H1D H 0.565225 0.265451 0.412804 0.103 Uiso 1 1 calc R U . . .
C2 C 0.639(3) 0.3223(14) 0.4710(6) 0.089(11) Uani 1 1 d . U . . .
H2A H 0.619550 0.356172 0.501894 0.107 Uiso 1 1 calc R U . . .
H2B H 0.677975 0.369034 0.451114 0.107 Uiso 1 1 calc R U . . .
C5 C 0.375000 0.7532(19) 0.375000 0.14(4) Uani 1 2 d S T P . .
H5A H 0.437557 0.776968 0.388913 0.207 Uiso 0.5 1 calc R U P A -1
H5B H 0.319633 0.776968 0.395143 0.207 Uiso 0.5 1 calc R U P A -1
H5C H 0.367810 0.776968 0.340944 0.207 Uiso 0.5 1 calc R U P A -1
C4 C 0.375000 0.639(3) 0.375000 0.14(3) Uani 1 2 d S TU P . .
B1 B 0.625000 0.125000 0.3153(7) 0.096(12) Uani 1 2 d S TU P . .
F1 F 0.659(2) 0.1946(11) 0.3461(4) 0.181(15) Uani 1 1 d . U . . .
F2 F 0.558(2) 0.1676(8) 0.2871(3) 0.124(10) 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
Cu1 N1 2.003(17) . ?
Cu1 N1 2.003(17) 7 ?
Cu1 N1 2.003(17) 12 ?
Cu1 N1 2.003(17) 14 ?
Cu1 N2 2.48(2) . ?
Cu1 N2 2.48(2) 14 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.48(3) . ?
C3 C3 1.38(7) 29_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.48(4) . ?
N2 C4 1.08(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.45(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 1.1044 . ?
C5 H5B 1.1044 . ?
C5 H5C 1.1044 . ?
C5 C4 1.54(4) . ?
B1 F1 1.322(19) 2_655 ?
B1 F1 1.322(19) . ?
B1 F2 1.292(18) . ?
B1 F2 1.292(18) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 171.0(6) . 12 ?
N1 Cu1 N1 89.0(10) 12 14 ?
N1 Cu1 N1 91.8(10) . 14 ?
N1 Cu1 N1 89.0(10) . 7 ?
N1 Cu1 N1 91.8(10) 12 7 ?
N1 Cu1 N1 171.0(6) 7 14 ?
N1 Cu1 N2 85.5(3) 14 14 ?
N1 Cu1 N2 94.5(3) . 14 ?
N1 Cu1 N2 94.5(3) 14 . ?
N1 Cu1 N2 85.5(3) 12 . ?
N1 Cu1 N2 85.5(3) 7 14 ?
N1 Cu1 N2 94.5(3) 7 . ?
N1 Cu1 N2 85.5(3) . . ?
N1 Cu1 N2 94.5(3) 12 14 ?
N2 Cu1 N2 180.0 . 14 ?
Cu1 N1 H1A 106.7 . . ?
Cu1 N1 H1B 106.7 . . ?
H1A N1 H1B 106.6 . . ?
C1 N1 Cu1 122.5(13) . . ?
C1 N1 H1A 106.7 . . ?
C1 N1 H1B 106.7 . . ?
C3 C3 H3A 107.4 29_656 . ?
C3 C3 H3B 107.4 29_656 . ?
C3 C3 C2 120(3) 29_656 . ?
H3A C3 H3B 106.9 . . ?
C2 C3 H3A 107.4 . . ?
C2 C3 H3B 107.4 . . ?
C4 N2 Cu1 180.0 . . ?
N1 C1 H1C 107.8 . . ?
N1 C1 H1D 107.8 . . ?
H1C C1 H1D 107.1 . . ?
C2 C1 N1 118.0(19) . . ?
C2 C1 H1C 107.8 . . ?
C2 C1 H1D 107.8 . . ?
C3 C2 H2A 107.3 . . ?
C3 C2 H2B 107.3 . . ?
C1 C2 C3 120(2) . . ?
C1 C2 H2A 107.2 . . ?
C1 C2 H2B 107.2 . . ?
H2A C2 H2B 106.9 . . ?
H5A C5 H5B 92.4 . . ?
H5A C5 H5C 92.4 . . ?
H5B C5 H5C 92.4 . . ?
C4 C5 H5A 123.6 . . ?
C4 C5 H5B 123.6 . . ?
C4 C5 H5C 123.6 . . ?
N2 C4 C5 180.000(13) . . ?
F1 B1 F1 104.2(19) . 2_655 ?
F2 B1 F1 115.7(16) . 2_655 ?
F2 B1 F1 106.0(10) 2_655 2_655 ?
F2 B1 F1 115.7(16) 2_655 . ?
F2 B1 F1 106.0(10) . . ?
F2 B1 F2 109.5(18) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 164.0(19) . . . . ?
N1 C1 C2 C3 -177(2) . . . . ?
C3 C3 C2 C1 -176(4) 29_656 . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 13 43 0.1000 -0.0279 12.9749 42.9610 -0.1780 -1.3026 -0.2579
21 0 26 0.1000 20.9878 -0.0347 26.1758 -1.0930 -0.5672 0.4941
21 0 -26 0.1000 21.0549 -0.0272 -25.8600 -1.0883 0.7562 0.0480
0 13 -43 0.1000 0.0831 12.9872 -43.0981 -0.1702 0.8860 -0.9957
-13 22 0 0.1000 -12.9665 21.9871 -0.2137 0.3805 -0.4110 -1.2285
0 -13 43 0.1000 -0.0831 -12.9872 43.0981 0.1702 -0.8860 0.9957
13 -22 0 0.1000 12.9665 -21.9871 0.2137 -0.3805 0.4110 1.2285
0 -13 -43 0.1000 0.0279 -12.9749 -42.9610 0.1780 1.3026 0.2579
-21 0 -26 0.1000 -20.9878 0.0347 -26.1758 1.0930 0.5672 -0.4941
-21 0 26 0.1000 -21.0549 0.0272 25.8600 1.0883 -0.7562 -0.0480
13 22 0 0.1000 13.0599 21.9488 -0.0182 -0.9699 -0.2940 -0.8929
-13 -22 0 0.1000 -13.0599 -21.9488 0.0182 0.9699 0.2940 0.8929

_olex2_submission_special_instructions 'No special instructions were received'
