# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_CuForm_RT
_database_code_depnum_ccdc_archive 'CCDC 2067545'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C6 H6 Cu2 O12), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_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'
Cu Cu 0.3201 1.2651 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.8330(4)
_cell_length_b                   8.7093(4)
_cell_length_c                   11.4145(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.224(4)
_cell_angle_gamma                90
_cell_volume                     872.93(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5164
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.3900
_cell_measurement_theta_min      4.6160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.501
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.331
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8550
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.579
_diffrn_reflns_theta_min         3.591
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 10.4015
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                998
_reflns_number_total             1133
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.141(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1133
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.136
_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)+(0.0315P)²+0.3730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0614
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.2500 0.2500 0.7500 0.01849(15) Uani 1 2 d S T P . .
O3 O -0.12562(14) -0.01696(14) 0.67759(10) 0.0293(3) Uani 1 1 d . . . . .
O2 O 0.05249(13) 0.16134(13) 0.68894(10) 0.0273(3) Uani 1 1 d . . . . .
O1 O 0.25617(13) 0.35289(12) 0.59692(9) 0.0232(3) Uani 1 1 d . . . . .
N1 N -0.2500 0.1859(3) 0.5000 0.0286(5) Uani 1 2 d S T P . .
C1 C 0.2500 0.2860(3) 0.5000 0.0190(4) Uani 1 2 d S T P . .
H1 H 0.2500 0.1792 0.5000 0.023 Uiso 1 2 calc RS T P . .
C2 C -0.00327(19) 0.03816(18) 0.72145(14) 0.0232(3) Uani 1 1 d . . . . .
H2 H 0.0510 -0.0155 0.7827 0.028 Uiso 1 1 calc R . . . .
C3 C -0.1417(3) 0.2787(3) 0.4421(2) 0.0408(5) Uani 1 1 d . . . . .
H3A H -0.0737 0.2123 0.4057 0.061 Uiso 1 1 calc R . . . .
H3B H -0.1961 0.3423 0.3830 0.061 Uiso 1 1 calc R . . . .
H3C H -0.0842 0.3423 0.4995 0.061 Uiso 1 1 calc R . . . .
H1A H -0.292(3) 0.132(3) 0.4513(19) 0.039(6) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0194(2) 0.0241(2) 0.01147(19) 0.00192(8) -0.00066(11) -0.00429(9)
O3 0.0279(6) 0.0288(6) 0.0297(6) 0.0024(5) -0.0038(5) -0.0080(5)
O2 0.0233(6) 0.0317(7) 0.0253(6) 0.0064(5) -0.0043(5) -0.0074(5)
O1 0.0336(7) 0.0236(6) 0.0124(5) 0.0003(4) 0.0020(4) -0.0018(5)
N1 0.0353(12) 0.0250(11) 0.0235(11) 0.000 -0.0058(9) 0.000
C1 0.0203(11) 0.0200(10) 0.0162(10) 0.000 -0.0006(8) 0.000
C2 0.0258(8) 0.0235(8) 0.0194(7) -0.0004(6) -0.0011(6) 0.0002(6)
C3 0.0368(12) 0.0456(11) 0.0425(12) 0.0030(9) 0.0151(10) 0.0029(9)

_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 O2 1.9652(11) . ?
Cu1 O2 1.9652(11) 7_556 ?
Cu1 O1 1.9697(10) . ?
Cu1 O1 1.9698(10) 7_556 ?
O3 C2 1.238(2) . ?
O2 C2 1.253(2) . ?
O1 C1 1.2463(15) . ?
N1 C3 1.464(3) . ?
N1 C3 1.464(3) 2_456 ?
C1 O1 1.2463(15) 2_556 ?

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
O2 Cu1 O2 180.0 . 7_556 ?
O2 Cu1 O1 88.45(5) 7_556 7_556 ?
O2 Cu1 O1 91.55(5) . 7_556 ?
O2 Cu1 O1 88.45(5) . . ?
O2 Cu1 O1 91.55(5) 7_556 . ?
O1 Cu1 O1 180.0 . 7_556 ?
C2 O2 Cu1 126.41(11) . . ?
C1 O1 Cu1 124.89(12) . . ?
C3 N1 C3 113.0(2) 2_456 . ?
O1 C1 O1 124.2(2) 2_556 . ?
O3 C2 O2 124.48(16) . . ?

_shelx_res_file                  
;
    cuform_rt.res created by SHELXL-2014/7

TITL CuForm_RT in I2/a
CELL 0.71073 8.833 8.7093 11.4145 90 96.224 90
ZERR 4 0.0004 0.0004 0.0005 0 0.004 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
UNIT 20 44 4 4 24

L.S. 10
PLAN  25
TEMP 25
fmap 2
acta
MERG 2
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_RT.hkl">
REM </olex2.extras>

WGHT    0.031500    0.373000
EXTI    0.141004
FVAR       9.72464
CU1   3    0.250000    0.250000    0.750000    10.50000    0.01936    0.02412 =
         0.01147    0.00192   -0.00066   -0.00429
O3    5   -0.125618   -0.016956    0.677585    11.00000    0.02786    0.02884 =
         0.02970    0.00239   -0.00383   -0.00798
O2    5    0.052491    0.161345    0.688940    11.00000    0.02327    0.03174 =
         0.02527    0.00642   -0.00430   -0.00745
O1    5    0.256167    0.352890    0.596917    11.00000    0.03357    0.02363 =
         0.01237    0.00025    0.00199   -0.00181
N1    4   -0.250000    0.185942    0.500000    10.50000    0.03534    0.02501 =
         0.02354    0.00000   -0.00583    0.00000
C1    1    0.250000    0.285977    0.500000    10.50000    0.02029    0.01997 =
         0.01625    0.00000   -0.00061    0.00000
AFIX  43
H1    2    0.249998    0.179195    0.500000    10.50000   -1.20000
AFIX   0
C2    1   -0.003271    0.038159    0.721453    11.00000    0.02576    0.02354 =
         0.01937   -0.00036   -0.00113    0.00019
AFIX  43
H2    2    0.051007   -0.015502    0.782737    11.00000   -1.20000
AFIX   0

C3    1   -0.141661    0.278702    0.442064    11.00000    0.03680    0.04557 =
         0.04250    0.00303    0.01509    0.00288
AFIX  33
H3A   2   -0.073651    0.212315    0.405695    11.00000   -1.50000
H3B   2   -0.196085    0.342310    0.383045    11.00000   -1.50000
H3C   2   -0.084201    0.342313    0.499457    11.00000   -1.50000
AFIX   0
H1A   2   -0.292086    0.131747    0.451325    11.00000    0.03884
HKLF 4

REM  CuForm_RT in I2/a
REM R1 =  0.0236 for     998 Fo > 4sig(Fo)  and  0.0290 for all    1133 data
REM     67 parameters refined using      0 restraints

END

WGHT      0.0317      0.3657

REM Highest difference peak  0.322,  deepest hole -0.588,  1-sigma level  0.082
Q1    1   0.0584  0.3365  0.6962  11.00000  0.05    0.32
Q2    1   0.2440  0.1374  0.4014  11.00000  0.05    0.28
Q3    1   0.1267  0.0198  0.8233  11.00000  0.05    0.28
Q4    1   0.2198  0.3380  0.5680  11.00000  0.05    0.25
Q5    1  -0.1461 -0.0532  0.6836  11.00000  0.05    0.24
Q6    1   0.2956  0.3602  0.5912  11.00000  0.05    0.23
Q7    1   0.2725  0.2358  0.5013  11.00000  0.05    0.23
Q8    1  -0.0737  0.1925  0.6826  11.00000  0.05    0.23
Q9    1   0.0203  0.1804  0.6647  11.00000  0.05    0.22
Q10   1   0.1122  0.1776  0.7054  11.00000  0.05    0.20
Q11   1   0.0846  0.4126  0.5506  11.00000  0.05    0.20
Q12   1  -0.0197  0.2559  0.7323  11.00000  0.05    0.20
Q13   1  -0.0594  0.2732  0.3293  11.00000  0.05    0.19
Q14   1   0.0987  0.1289  0.6726  11.00000  0.05    0.18
Q15   1  -0.1592  0.0024  0.6495  11.00000  0.05    0.18
Q16   1  -0.2553  0.4716  0.4511  11.00000  0.05    0.18
Q17   1  -0.1775  0.2909  0.3904  11.00000  0.05    0.18
Q18   1   0.0532  0.2500  0.5650  11.00000  0.05    0.18
Q19   1  -0.2616 -0.0186  0.6756  11.00000  0.05    0.17
Q20   1   0.0365  0.1494  0.7238  11.00000  0.05    0.17
Q21   1  -0.0243  0.2482  0.4825  11.00000  0.05    0.17
Q22   1  -0.0416  0.2389  0.6288  11.00000  0.05    0.17
Q23   1  -0.0164  0.4047  0.5726  11.00000  0.05    0.17
Q24   1  -0.1198  0.4256  0.4468  11.00000  0.05    0.17
Q25   1  -0.1147  0.2289  0.7453  11.00000  0.05    0.17
;
_shelx_res_checksum              86731
_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
;
####################################################################### 
# 
# 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_CuForm_5_2GPa
_database_code_depnum_ccdc_archive 'CCDC 2067550'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C12 H12 Cu4 O24), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_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'
Cu Cu 0.3201 1.2651 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.086(4)
_cell_length_b                   8.466(2)
_cell_length_c                   10.9541(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.215(17)
_cell_angle_gamma                90
_cell_volume                     747.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    204
_cell_measurement_temperature    293.6(3)
_cell_measurement_pressure       5.20(0.03)
_cell_measurement_theta_max      23.4570
_cell_measurement_theta_min      3.0440
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.759
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.175
_diffrn_reflns_Laue_measured_fraction_max 0.172
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            350
_diffrn_reflns_point_group_measured_fraction_full 0.175
_diffrn_reflns_point_group_measured_fraction_max 0.172
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.481
_diffrn_reflns_theta_min         3.044
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.175
_diffrn_measured_fraction_theta_max 0.172
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -40.00   1.00   30.00    --  -25.00 134.00 -57.00   57
  2  φ    -90.00 -27.00   1.00   30.00 -82.00 -25.00 134.00    --    63
  3  ω     40.00  97.00   1.00   30.00    --   25.00-134.00  57.00   57
  4  φ     27.00  90.00   1.00   30.00  82.00  25.00-134.00    --    63
  5  φ    -40.00  40.00   1.00   30.00   0.00   0.00   0.00    --    80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                102
_reflns_number_total             120
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         120
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      0.845
_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)+(0.0605P)²+10.3900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0887
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(Cu1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1) = Uanis(O3)
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.7500 0.7500 0.7500 0.0133(14) Uani 1 2 d S TU P . .
O3 O 0.3614(19) 0.4679(14) 0.6645(8) 0.021(3) Uani 1 1 d . U . . .
O1 O 0.7533(17) 0.8716(12) 0.6007(6) 0.013(3) Uani 1 1 d . U . . .
C1 C 0.7500 0.798(3) 0.5000 0.021(3) Uani 1 2 d S TU P . .
H1 H 0.7500 0.6879 0.5000 0.025 Uiso 1 2 calc RS T P . .
O2 O 0.5373(19) 0.6650(17) 0.6844(7) 0.022(4) Uani 1 1 d . U . . .
N1 N 0.2500 0.697(3) 0.5000 0.027(5) Uani 1 2 d S TU P . .
H1A H 0.3111 0.6345 0.5509 0.032 Uiso 0.5 1 calc R . . . .
H1B H 0.1889 0.6345 0.4491 0.032 Uiso 0.5 1 calc R . . . .
C4 C 0.359(3) 0.786(2) 0.4299(14) 0.041(6) Uani 1 1 d . U . . .
H4A H 0.2959 0.8410 0.3655 0.061 Uiso 1 1 calc GR . . . .
H4B H 0.4365 0.7164 0.3950 0.061 Uiso 1 1 calc GR . . . .
H4C H 0.4186 0.8614 0.4820 0.061 Uiso 1 1 calc GR . . . .
C2 C 0.488(3) 0.529(2) 0.7150(12) 0.016(4) Uani 1 1 d . U . . .
H2 H 0.5488 0.4746 0.7768 0.019 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.014(2) 0.0134(18) 0.0126(14) 0.0006(9) 0.0004(11) -0.0003(11)
O3 0.021(3) 0.021(3) 0.021(3) -0.0002(10) 0.0014(10) -0.0002(10)
O1 0.013(3) 0.013(3) 0.013(3) 0.0002(14) 0.0009(14) 0.0003(14)
C1 0.021(3) 0.021(3) 0.021(3) -0.0002(10) 0.0014(10) -0.0002(10)
O2 0.022(4) 0.022(4) 0.023(4) 0.0003(14) 0.0014(14) 0.0000(14)
N1 0.027(6) 0.027(6) 0.027(5) 0.000 0.0017(14) 0.000
C4 0.041(7) 0.041(7) 0.040(6) 0.000(3) 0.003(3) 0.000(3)
C2 0.016(5) 0.016(5) 0.016(4) -0.0001(14) 0.0012(14) 0.0001(14)

_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 O3 2.284(12) 6_665 ?
Cu1 O3 2.284(12) 4_556 ?
Cu1 O1 1.934(8) 7_666 ?
Cu1 O1 1.934(8) . ?
Cu1 O2 1.952(15) . ?
Cu1 O2 1.952(15) 7_666 ?
O3 Cu1 2.284(12) 4_546 ?
O3 C2 1.24(2) . ?
O1 C1 1.267(15) . ?
C1 O1 1.267(15) 2_656 ?
C1 H1 0.9300 . ?
O2 C2 1.268(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C4 1.43(2) 2_556 ?
N1 C4 1.43(2) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2 0.9300 . ?

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
O3 Cu1 O3 180.0 4_556 6_665 ?
O1 Cu1 O3 93.0(4) 7_666 4_556 ?
O1 Cu1 O3 87.0(4) 7_666 6_665 ?
O1 Cu1 O3 93.0(4) . 6_665 ?
O1 Cu1 O3 87.0(4) . 4_556 ?
O1 Cu1 O1 180.0 7_666 . ?
O1 Cu1 O2 92.8(5) 7_666 . ?
O1 Cu1 O2 92.8(5) . 7_666 ?
O1 Cu1 O2 87.2(5) . . ?
O1 Cu1 O2 87.2(5) 7_666 7_666 ?
O2 Cu1 O3 94.9(6) 7_666 6_665 ?
O2 Cu1 O3 85.1(6) . 6_665 ?
O2 Cu1 O3 94.9(6) . 4_556 ?
O2 Cu1 O3 85.1(6) 7_666 4_556 ?
O2 Cu1 O2 180.0 7_666 . ?
C2 O3 Cu1 119.5(11) . 4_546 ?
C1 O1 Cu1 118.2(12) . . ?
O1 C1 O1 121(2) . 2_656 ?
O1 C1 H1 119.6 . . ?
O1 C1 H1 119.6 2_656 . ?
C2 O2 Cu1 121.4(12) . . ?
H1A N1 H1B 107.4 . . ?
C4 N1 H1A 108.3 . . ?
C4 N1 H1A 108.3 2_556 . ?
C4 N1 H1B 108.3 2_556 . ?
C4 N1 H1B 108.3 . . ?
C4 N1 C4 116(2) . 2_556 ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C2 O2 121.7(16) . . ?
O3 C2 H2 119.2 . . ?
O2 C2 H2 119.1 . . ?

_shelx_res_file                  
;
    cuform_5_2gpa.res created by SHELXL-2014/7

TITL CuForm_5_2GPa_a.res in I2/a
REM Old TITL CuForm_5_2GPa in I2/a
REM SHELXT solution in I2/a
REM R1 0.173, Rweak 0.010, Alpha 0.143, Orientation as input
REM Formula found by SHELXT: C7 O4 Cu
CELL 0.71073 8.0857 8.4663 10.9541 90 94.215 90
ZERR 4 0.0036 0.0024 0.0009 0 0.017 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 0.5-X,+Y,1-Z
EQIV $2 1-X,2-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
ISOR 0.001 0.002 Cu1 C1 O1 O3
ISOR 0.001 0.002 N1
ISOR 0.001 0.002 C4
ISOR 0.001 0.002 O2 C2
EADP C1 O3

L.S. 44
PLAN  5
SIZE 0.1 0.08 0.05
RTAB NO N1 O3_$1
RTAB NO N1 O2_$1
RTAB CO C4 O1_$2
RTAB CO C4 O3_$3
RTAB HO H1b O3_$1
RTAB HO H1b O2_$1
RTAB HO H4a O1_$2
RTAB HO H4b O3_$3
RTAB NHO N1 H1b O3_$1
RTAB NHO N1 H1b O2_$1
RTAB CHO C4 H4a O1_$2
RTAB CHO C4 H4b O3_$3
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_5_2GPa.hkl">
REM </olex2.extras>

WGHT    0.060500   10.390000
FVAR       0.68963
CU1   3    0.750000    0.750000    0.750000    10.50000    0.01401    0.01336 =
         0.01257    0.00055    0.00035   -0.00034
O3    5    0.361367    0.467885    0.664475    11.00000    0.02052    0.02051 =
         0.02075   -0.00022    0.00137   -0.00019
O1    5    0.753251    0.871620    0.600718    11.00000    0.01273    0.01267 =
         0.01283    0.00018    0.00094    0.00031
C1    1    0.750000    0.797773    0.500000    10.50000    0.02052    0.02051 =
         0.02075   -0.00022    0.00137   -0.00019
AFIX  43
H1    2    0.750000    0.687925    0.500001    10.50000   -1.20000
AFIX   0
O2    5    0.537347    0.665041    0.684415    11.00000    0.02213    0.02209 =
         0.02262    0.00028    0.00137   -0.00001
N1    4    0.250000    0.696776    0.500000    10.50000    0.02687    0.02677 =
         0.02698    0.00000    0.00168    0.00000
AFIX  23
H1A   2    0.311122    0.634539    0.550886    10.50000   -1.20000
H1B   2    0.188878    0.634539    0.449115    10.50000   -1.20000
AFIX   0
C4    1    0.359226    0.786255    0.429871    11.00000    0.04055    0.04072 =
         0.04031    0.00000    0.00308   -0.00024
AFIX 137
H4A   2    0.295873    0.841040    0.365503    11.00000   -1.50000
H4B   2    0.436531    0.716389    0.395000    11.00000   -1.50000
H4C   2    0.418621    0.861423    0.482018    11.00000   -1.50000
AFIX   0
C2    1    0.488306    0.529437    0.715017    11.00000    0.01605    0.01615 =
         0.01567   -0.00014    0.00125    0.00007
AFIX  43
H2    2    0.548775    0.474552    0.776838    11.00000   -1.20000
AFIX   0
HKLF 4

REM  CuForm_5_2GPa_a.res in I2/a
REM R1 =  0.0336 for     102 Fo > 4sig(Fo)  and  0.0395 for all     120 data
REM     59 parameters refined using     48 restraints

END

WGHT      0.0605     10.3900

REM Highest difference peak  0.187,  deepest hole -0.223,  1-sigma level  0.056
Q1    1   0.3579  0.5271  0.6135  11.00000  0.05    0.19
Q2    1   0.6704  0.7408  0.6463  11.00000  0.05    0.18
Q3    1   0.5317  0.6384  0.6332  11.00000  0.05    0.18
Q4    1   0.2866  0.3661  0.6893  11.00000  0.05    0.17
Q5    1   0.6449  0.5357  0.6657  11.00000  0.05    0.16
;
_shelx_res_checksum              44461

# start Validation Reply Form
_vrf_PLAT029_CuForm_5_2GPa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.175 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_5_2GPa       
;
PROBLEM: Poor Data / Parameter Ratio ....................       2.03 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_5_2GPa       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        267 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;
####################################################################### 
# 
# 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_CuForm_3_8GPa_synchr
_database_code_depnum_ccdc_archive 'CCDC 2067549'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C12 H12 Cu4 O24), C2 H7 N'
_chemical_formula_sum            'C5 H10 Cu N O6'
_chemical_formula_weight         243.68
_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 0.0008 0.0007 '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'
Cu Cu 0.3132 0.6683 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0043 0.0027 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.2878(9)
_cell_length_b                   8.4645(6)
_cell_length_c                   11.0942(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.521(4)
_cell_angle_gamma                90
_cell_volume                     775.86(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    629
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2390
_cell_measurement_theta_min      2.1130
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.893
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.506
_diffrn_reflns_Laue_measured_fraction_max 0.293
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1139
_diffrn_reflns_point_group_measured_fraction_full 0.506
_diffrn_reflns_point_group_measured_fraction_max 0.293
_diffrn_reflns_theta_full        17.330
_diffrn_reflns_theta_max         26.472
_diffrn_reflns_theta_min         2.573
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.506
_diffrn_measured_fraction_theta_max 0.293
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ     17.00  97.00   0.50    1.00  57.05   0.00-134.76    --   160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0467912000
_diffrn_orient_matrix_UB_12      0.0368295000
_diffrn_orient_matrix_UB_13      0.0016556000
_diffrn_orient_matrix_UB_21      0.0087595000
_diffrn_orient_matrix_UB_22      -0.0083579000
_diffrn_orient_matrix_UB_23      0.0443130000
_diffrn_orient_matrix_UB_31      0.0366892000
_diffrn_orient_matrix_UB_32      -0.0448864000
_diffrn_orient_matrix_UB_33      -0.0068922000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.49647
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                560
_reflns_number_total             688
_reflns_odcompleteness_completeness 28.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.47
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         688
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.091
_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)+(0.0818P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1125
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4(0.5)
3.a Riding coordinates:
 N1(H4)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H006), C2(H007)
3.c Idealised Me refined as rotating group:
 C3(H00A,H00B,H00C)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu1 Cu 0.7500 0.2500 0.7500 0.0199(2) Uani 1 2 d S T P . .
O1 O 0.7582(3) 0.1314(3) 0.59938(14) 0.0259(6) Uani 1 1 d . . . . .
O3 O 0.3632(4) 0.5288(3) 0.66991(18) 0.0300(6) Uani 1 1 d . . . . .
O2 O 0.5398(3) 0.3342(3) 0.68611(16) 0.0279(6) Uani 1 1 d . . . . .
N1 N 0.2500 0.3072(6) 0.5000 0.0319(10) Uani 1 2 d S T P . .
H4 H 0.2024 0.3791 0.4554 0.038 Uiso 0.5 1 d R . . . .
C1 C 0.7500 0.2027(6) 0.5000 0.0204(9) Uani 1 2 d S T P . .
H006 H 0.7500 0.3126 0.5000 0.025 Uiso 1 2 calc RS T P . .
C2 C 0.4895(5) 0.4671(4) 0.7159(2) 0.0265(8) Uani 1 1 d . . . . .
H007 H 0.5502 0.5228 0.7758 0.032 Uiso 1 1 calc R . . . .
C3 C 0.1384(6) 0.2145(7) 0.5642(3) 0.0399(10) Uani 1 1 d . . . . .
H00A H 0.0821 0.1419 0.5092 0.060 Uiso 1 1 calc GR . . . .
H00B H 0.0618 0.2832 0.5981 0.060 Uiso 1 1 calc GR . . . .
H00C H 0.1972 0.1566 0.6278 0.060 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0239(6) 0.0225(4) 0.0129(2) -0.00081(12) -0.00147(17) 0.00181(16)
O1 0.035(2) 0.0288(14) 0.0128(6) 0.0009(6) -0.0015(7) -0.0004(9)
O3 0.034(2) 0.0284(16) 0.0264(8) -0.0033(8) -0.0052(8) 0.0084(10)
O2 0.028(2) 0.0303(18) 0.0244(8) -0.0059(7) -0.0045(8) 0.0073(9)
N1 0.043(4) 0.029(3) 0.0222(13) 0.000 -0.0075(15) 0.000
C1 0.024(3) 0.021(2) 0.0161(12) 0.000 -0.0033(13) 0.000
C2 0.030(3) 0.029(2) 0.0191(9) 0.0026(9) -0.0028(10) -0.0026(13)
C3 0.030(4) 0.047(3) 0.0444(18) 0.0027(15) 0.0146(18) 0.007(2)

_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 O1 1.9551(19) 7_656 ?
Cu1 O1 1.9551(19) . ?
Cu1 O3 2.303(3) 4_546 ?
Cu1 O3 2.303(3) 6_665 ?
Cu1 O2 1.962(3) . ?
Cu1 O2 1.962(3) 7_656 ?
O1 C1 1.254(3) . ?
O3 Cu1 2.303(2) 4_556 ?
O3 C2 1.243(4) . ?
O2 C2 1.253(4) . ?
N1 H4 0.8600 . ?
N1 C3 1.443(5) 2_556 ?
N1 C3 1.443(5) . ?
C1 O1 1.254(3) 2_656 ?
C1 H006 0.9300 . ?
C2 H007 0.9300 . ?
C3 H00A 0.9600 . ?
C3 H00B 0.9600 . ?
C3 H00C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 7_656 . ?
O1 Cu1 O3 92.58(9) . 6_665 ?
O1 Cu1 O3 87.42(9) . 4_546 ?
O1 Cu1 O3 87.42(9) 7_656 6_665 ?
O1 Cu1 O3 92.58(9) 7_656 4_546 ?
O1 Cu1 O2 88.13(10) 7_656 7_656 ?
O1 Cu1 O2 91.87(10) . 7_656 ?
O1 Cu1 O2 91.87(10) 7_656 . ?
O1 Cu1 O2 88.13(10) . . ?
O3 Cu1 O3 180.00(7) 4_546 6_665 ?
O2 Cu1 O3 93.30(12) . 4_546 ?
O2 Cu1 O3 93.30(12) 7_656 6_665 ?
O2 Cu1 O3 86.70(12) . 6_665 ?
O2 Cu1 O3 86.70(12) 7_656 4_546 ?
O2 Cu1 O2 180.0 7_656 . ?
C1 O1 Cu1 120.1(3) . . ?
C2 O3 Cu1 122.6(2) . 4_556 ?
C2 O2 Cu1 122.4(2) . . ?
C3 N1 H4 112.5 2_556 . ?
C3 N1 H4 112.7 . . ?
C3 N1 C3 114.1(5) . 2_556 ?
O1 C1 O1 122.4(5) 2_656 . ?
O1 C1 H006 118.8 . . ?
O1 C1 H006 118.8 2_656 . ?
O3 C2 O2 123.8(3) . . ?
O3 C2 H007 118.1 . . ?
O2 C2 H007 118.1 . . ?
N1 C3 H00A 109.5 . . ?
N1 C3 H00B 109.5 . . ?
N1 C3 H00C 109.5 . . ?
H00A C3 H00B 109.5 . . ?
H00A C3 H00C 109.5 . . ?
H00B C3 H00C 109.5 . . ?

_shelx_res_file                  
;
    CuForm_3_8GPa_synchr.res created by SHELXL-2014/7

TITL CuForm_3_8GPa_synchr_a.res in I2/a
REM Old TITL CuForm_3_8GPa_synchr in I2/a
REM SHELXT solution in I2/a
REM R1 0.095, Rweak 0.238, Alpha 0.048, Orientation as input
REM Formula found by SHELXT: C8 O4 Cu
CELL 0.49647 8.2878 8.4645 11.0942 90 94.521 90
ZERR 4 0.0009 0.0006 0.0003 0 0.004 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
DISP C 0.0008 0.0007 6.2498
DISP Cu 0.3132 0.6683 1903.5186
DISP H -0 0 0.6077
DISP O 0.0043 0.0027 13.9729
UNIT 20 40 4 4 24

L.S. 40
PLAN  5
SIZE 0.056 0.072 0.11
BOND $H
list 4
fmap 2 53
ACTA
OMIT -1 5 12
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_3_8GPa_synchr.hkl">
REM </olex2.extras>

WGHT    0.081800
FVAR       0.74964
CU1   3    0.750000    0.250000    0.750000    10.50000    0.02393    0.02250 =
         0.01289   -0.00081   -0.00147    0.00181
O1    5    0.758200    0.131400    0.599380    11.00000    0.03544    0.02883 =
         0.01281    0.00090   -0.00146   -0.00045
O3    5    0.363210    0.528830    0.669909    11.00000    0.03398    0.02844 =
         0.02645   -0.00335   -0.00520    0.00844
O2    5    0.539841    0.334201    0.686109    11.00000    0.02800    0.03034 =
         0.02445   -0.00591   -0.00453    0.00728
N1    4    0.250000    0.307213    0.500000    10.50000    0.04305    0.02879 =
         0.02218    0.00000   -0.00755    0.00000
AFIX   3
H4    2    0.202430    0.379053    0.455370    10.50000   -1.20000
AFIX   0

C1    1    0.750000    0.202729    0.500000    10.50000    0.02354    0.02087 =
         0.01615    0.00000   -0.00332    0.00000
AFIX  43
H006  2    0.750003    0.312599    0.500000    10.50000   -1.20000
AFIX   0
C2    1    0.489484    0.467125    0.715868    11.00000    0.03049    0.02898 =
         0.01915    0.00257   -0.00282   -0.00264
AFIX  43
H007  2    0.550157    0.522810    0.775835    11.00000   -1.20000
AFIX   0

C3    1    0.138438    0.214473    0.564168    11.00000    0.03005    0.04716 =
         0.04437    0.00271    0.01461    0.00714
AFIX 137
H00A  2    0.082111    0.141917    0.509240    11.00000   -1.50000
H00B  2    0.061816    0.283221    0.598133    11.00000   -1.50000
H00C  2    0.197156    0.156574    0.627827    11.00000   -1.50000
AFIX   0
HKLF 4

REM  CuForm_3_8GPa_synchr_a.res in I2/a
REM R1 =  0.0359 for     560 Fo > 4sig(Fo)  and  0.0415 for all     688 data
REM     63 parameters refined using      0 restraints

END

WGHT      0.0818      0.0000

REM Highest difference peak  0.389,  deepest hole -0.406,  1-sigma level  0.090
Q1    1   0.4187  0.5854  0.6821  11.00000  0.05    0.39
Q2    1   0.4964  0.4370  0.6832  11.00000  0.05    0.31
Q3    1   0.5145  0.5440  0.8276  11.00000  0.05    0.30
Q4    1   0.5734  0.4117  0.8183  11.00000  0.05    0.30
Q5    1   0.8044  0.1473  0.6132  11.00000  0.05    0.29
;
_shelx_res_checksum              7056

# start Validation Reply Form
_vrf_PLAT029_CuForm_3_8GPa_synchr 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.506 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT660_CuForm_3_8GPa_synchr 
;
PROBLEM: No Valid _diffrn_radiation_type Value Reported .     Please Do !  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_3_8GPa_synchr 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        346 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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 1.978
_oxdiff_exptl_absorpt_empirical_full_min 0.351
####################################################################### 
# 
# 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_CuForm_1GPa
_database_code_depnum_ccdc_archive 'CCDC 2067546'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C12 H12 Cu4 O24), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_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'
Cu Cu 0.3201 1.2651 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.6895(13)
_cell_length_b                   8.5925(10)
_cell_length_c                   11.3323(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.623(7)
_cell_angle_gamma                90
_cell_volume                     842.05(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    464
_cell_measurement_temperature    294.44(12)
_cell_measurement_pressure       1.00(0.03)
_cell_measurement_theta_max      26.1060
_cell_measurement_theta_min      3.3290
_shelx_estimated_absorpt_T_max   0.881
_shelx_estimated_absorpt_T_min   0.782
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.328
_diffrn_reflns_Laue_measured_fraction_max 0.293
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            838
_diffrn_reflns_point_group_measured_fraction_full 0.328
_diffrn_reflns_point_group_measured_fraction_max 0.293
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         3.342
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.328
_diffrn_measured_fraction_theta_max 0.293
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -40.00   1.00   30.00    --  -25.00 134.00 -57.00   57
  2  φ    -90.00 -27.00   1.00   30.00 -82.00 -25.00 134.00    --    63
  3  ω     40.00  97.00   1.00   30.00    --   25.00-134.00  57.00   57
  4  φ     27.00  90.00   1.00   30.00  82.00  25.00-134.00    --    63
  5  φ    -40.00  40.00   1.00   30.00   0.00   0.00   0.00    --    80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                207
_reflns_number_total             254
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         254
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0339
_refine_ls_restrained_S_all      1.050
_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)+(0.0597P)²+1.3970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0937
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.7500 0.7500 0.7500 0.0189(9) Uani 1 2 d S T P . .
O1 O 0.7564(7) 0.8570(7) 0.5974(3) 0.0222(19) Uani 1 1 d . . . . .
O3 O 0.3709(9) 0.4781(7) 0.6758(4) 0.0272(16) Uani 1 1 d . U . . .
O2 O 0.5495(8) 0.6632(8) 0.6893(4) 0.024(2) Uani 1 1 d . . . . .
C1 C 0.7500 0.7895(14) 0.5000 0.017(3) Uani 1 2 d S TU P . .
H1 H 0.7500 0.6813 0.5000 0.021 Uiso 1 2 calc RS T P . .
N1 N 0.2500 0.6859(12) 0.5000 0.022(2) Uani 1 2 d S TU P . .
H1A H 0.1983 0.6249 0.4465 0.027 Uiso 0.5 1 calc R . . . .
H1B H 0.3017 0.6249 0.5535 0.027 Uiso 0.5 1 calc R . . . .
C4 C 0.3605(14) 0.7798(10) 0.4412(7) 0.039(3) Uani 1 1 d . U . . .
H4A H 0.3064 0.8384 0.3780 0.058 Uiso 1 1 calc GR . . . .
H4B H 0.4346 0.7127 0.4095 0.058 Uiso 1 1 calc GR . . . .
H4C H 0.4131 0.8499 0.4976 0.058 Uiso 1 1 calc GR . . . .
C2 C 0.4941(12) 0.5368(11) 0.7191(6) 0.022(2) Uani 1 1 d . U . . .
H2 H 0.5504 0.4814 0.7792 0.027 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.017(2) 0.0252(17) 0.0134(6) 0.0011(5) -0.0013(9) -0.0028(8)
O1 0.024(6) 0.023(5) 0.0186(19) 0.003(3) 0.001(3) 0.000(4)
O3 0.0269(19) 0.0274(19) 0.0273(16) -0.0009(10) 0.0029(11) -0.0010(11)
O2 0.024(7) 0.020(6) 0.029(2) 0.003(3) 0.001(3) -0.005(4)
C1 0.017(3) 0.017(3) 0.017(3) 0.000 0.0013(11) 0.000
N1 0.022(3) 0.022(3) 0.022(2) 0.000 0.0015(11) 0.000
C4 0.038(4) 0.040(3) 0.038(3) 0.002(2) 0.006(2) 0.001(2)
C2 0.022(2) 0.023(2) 0.022(2) -0.0008(11) 0.0021(11) 0.0003(11)

_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 O1 1.965(4) . ?
Cu1 O1 1.965(4) 7_666 ?
Cu1 O3 2.414(6) 4_556 ?
Cu1 O3 2.414(6) 6_665 ?
Cu1 O2 1.957(6) . ?
Cu1 O2 1.957(6) 7_666 ?
O1 C1 1.243(7) . ?
O3 Cu1 2.414(6) 4_546 ?
O3 C2 1.240(10) . ?
O2 C2 1.248(10) . ?
C1 O1 1.243(7) 2_656 ?
C1 H1 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C4 1.464(11) . ?
N1 C4 1.464(11) 2_556 ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 7_666 ?
O1 Cu1 O3 88.7(2) 7_666 6_665 ?
O1 Cu1 O3 91.3(2) 7_666 4_556 ?
O1 Cu1 O3 91.3(2) . 6_665 ?
O1 Cu1 O3 88.7(2) . 4_556 ?
O3 Cu1 O3 180.0 4_556 6_665 ?
O2 Cu1 O1 91.7(2) 7_666 . ?
O2 Cu1 O1 91.7(2) . 7_666 ?
O2 Cu1 O1 88.3(2) 7_666 7_666 ?
O2 Cu1 O1 88.3(2) . . ?
O2 Cu1 O3 88.3(3) 7_666 4_556 ?
O2 Cu1 O3 91.7(3) . 4_556 ?
O2 Cu1 O3 88.3(3) . 6_665 ?
O2 Cu1 O3 91.7(3) 7_666 6_665 ?
O2 Cu1 O2 180.0 7_666 . ?
C1 O1 Cu1 124.1(6) . . ?
C2 O3 Cu1 125.5(6) . 4_546 ?
C2 O2 Cu1 126.2(5) . . ?
O1 C1 O1 124.3(11) 2_656 . ?
O1 C1 H1 117.8 2_656 . ?
O1 C1 H1 117.8 . . ?
H1A N1 H1B 107.8 . . ?
C4 N1 H1A 109.0 2_556 . ?
C4 N1 H1A 109.0 . . ?
C4 N1 H1B 109.0 . . ?
C4 N1 H1B 109.0 2_556 . ?
C4 N1 C4 113.1(11) 2_556 . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C2 O2 126.0(8) . . ?
O3 C2 H2 117.0 . . ?
O2 C2 H2 117.0 . . ?

_shelx_res_file                  
;
    CuForm_1GPa.res created by SHELXL-2014/7

TITL CuForm_1GPa_a.res in I2/a
REM Old TITL CuForm_1GPa_a.res in I2/a
REM SHELXT solution in I2/a
REM R1 0.113, Rweak 0.002, Alpha 0.042, Orientation as input
REM Formula found by SHELXT: C6 O6 Cu
CELL 0.71073 8.6895 8.5925 11.3323 90 95.623 90
ZERR 4 0.0013 0.001 0.0004 0 0.007 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 0.5-X,+Y,1-Z
EQIV $2 1-X,2-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
ISOR 0.001 0.002 O3 C2 C1 N1
ISOR 0.001 0.002 C4

L.S. 44
PLAN  5
SIZE 0.1 0.08 0.05
RTAB NO N1 O3_$1
RTAB NO N1 O2_$1
RTAB CO C4 O1_$2
RTAB CO C4 O3_$3
RTAB HO H1a O3_$1
RTAB HO H1a O2_$1
RTAB HO H4a O1_$2
RTAB HO H4b O3_$3
RTAB NHO N1 H1a O3_$1
RTAB NHO N1 H1a O2_$1
RTAB CHO C4 H4a O1_$2
RTAB CHO C4 H4b O3_$3
BOND $H
list 4
fmap 2
acta
OMIT 3 1 2
OMIT 4 2 4
OMIT 4 2 6
OMIT 6 5 7
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_1GPa.hkl">
REM </olex2.extras>

WGHT    0.059700    1.397000
FVAR       0.68002
CU1   3    0.750000    0.750000    0.750000    10.50000    0.01748    0.02523 =
         0.01337    0.00111   -0.00132   -0.00276
O1    5    0.756412    0.857041    0.597357    11.00000    0.02439    0.02349 =
         0.01864    0.00277    0.00134   -0.00050
O3    5    0.370907    0.478125    0.675847    11.00000    0.02692    0.02736 =
         0.02730   -0.00087    0.00286   -0.00105
O2    5    0.549531    0.663192    0.689314    11.00000    0.02412    0.01972 =
         0.02889    0.00278    0.00061   -0.00467
C1    1    0.750000    0.789521    0.500000    10.50000    0.01700    0.01711 =
         0.01721    0.00000    0.00132    0.00000
AFIX  43
H1    2    0.749999    0.681287    0.500000    10.50000   -1.20000
AFIX   0
N1    4    0.250000    0.685910    0.500000    10.50000    0.02238    0.02201 =
         0.02239    0.00000    0.00155    0.00000
AFIX  23
H1A   2    0.198258    0.624854    0.446455    10.50000   -1.20000
H1B   2    0.301742    0.624855    0.553545    10.50000   -1.20000
AFIX   0
C4    1    0.360548    0.779803    0.441229    11.00000    0.03815    0.03955 =
         0.03832    0.00188    0.00632    0.00087
AFIX 137
H4A   2    0.306439    0.838438    0.378045    11.00000   -1.50000
H4B   2    0.434630    0.712686    0.409503    11.00000   -1.50000
H4C   2    0.413076    0.849865    0.497593    11.00000   -1.50000
AFIX   0
C2    1    0.494093    0.536776    0.719057    11.00000    0.02242    0.02272 =
         0.02219   -0.00084    0.00212    0.00028
AFIX  43
H2    2    0.550411    0.481439    0.779212    11.00000   -1.20000
AFIX   0
HKLF 4

REM  CuForm_1GPa_a.res in I2/a
REM R1 =  0.0339 for     207 Fo > 4sig(Fo)  and  0.0429 for all     254 data
REM     63 parameters refined using     30 restraints

END

WGHT      0.0597      1.3970

REM Highest difference peak  0.246,  deepest hole -0.275,  1-sigma level  0.074
Q1    1   0.2877  0.4962  0.6188  11.00000  0.05    0.25
Q2    1   0.3379  0.7437  0.3808  11.00000  0.05    0.23
Q3    1   0.6634  0.7408  0.6820  11.00000  0.05    0.22
Q4    1   0.8781  0.7463  0.6244  11.00000  0.05    0.20
Q5    1   0.7283  0.9722  0.6120  11.00000  0.05    0.20
;
_shelx_res_checksum              9243

# start Validation Reply Form
_vrf_PLAT029_CuForm_1GPa         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.328 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_1GPa         
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.03 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_1GPa         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        339 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;
####################################################################### 
# 
# 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_CuForm_8_3GPa_synchr
_database_code_depnum_ccdc_archive 'CCDC 2067552'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H6 Cu2 O12, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H22 Cu2 N2 O12'
_chemical_formula_weight         489.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         Cu2C10H20N2O5
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0008 0.0007 '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'
Cu Cu 0.3132 0.6683 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0020 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0043 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.2432(13)
_cell_length_b                   8.5444(11)
_cell_length_c                   11.2169(19)
_cell_angle_alpha                92.441(13)
_cell_angle_beta                 102.055(15)
_cell_angle_gamma                91.298(13)
_cell_volume                     677.92(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7580
_cell_measurement_theta_min      2.1260
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.879
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.471
_diffrn_reflns_Laue_measured_fraction_max 0.262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3954
_diffrn_reflns_point_group_measured_fraction_full 0.471
_diffrn_reflns_point_group_measured_fraction_max 0.262
_diffrn_reflns_theta_full        17.330
_diffrn_reflns_theta_max         27.656
_diffrn_reflns_theta_min         1.667
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.471
_diffrn_measured_fraction_theta_max 0.262
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ     17.00  97.00   0.50    1.00  57.05   0.00-134.76    --   160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0385007000
_diffrn_orient_matrix_UB_12      0.0180568000
_diffrn_orient_matrix_UB_13      -0.0386279000
_diffrn_orient_matrix_UB_21      -0.0303063000
_diffrn_orient_matrix_UB_22      -0.0530758000
_diffrn_orient_matrix_UB_23      -0.0091302000
_diffrn_orient_matrix_UB_31      -0.0501671000
_diffrn_orient_matrix_UB_32      0.0155798000
_diffrn_orient_matrix_UB_33      0.0218562000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.49647
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1297
_reflns_number_total             2430
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.109
_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     227
_refine_ls_number_reflns         2430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0508
_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)+(0.0554P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1309
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(O2A) = Uanis(N1)
Uanis(O1A) = Uanis(O1B)
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C1(H1), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C)
;
_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
Cu2 Cu 0.74504(10) 0.75491(6) 0.73291(11) 0.0284(5) Uani 1 1 d . . . . .
Cu1 Cu 0.74164(9) 0.75320(6) 0.23285(10) 0.0296(5) Uani 1 1 d . . . . .
O1A O 0.7128(6) 0.8000(4) 0.5600(7) 0.035(2) Uani 1 1 d . . . . .
O4A O 0.5975(6) 0.6567(4) 0.0425(6) 0.035(3) Uani 1 1 d . . . . .
O1B O 0.8638(7) 0.8671(4) 0.4165(7) 0.035(2) Uani 1 1 d . . . . .
O4B O 0.7600(6) 0.7167(4) 0.9015(6) 0.024(3) Uani 1 1 d . . . . .
O3B O 0.6235(6) 0.5507(3) 0.6789(6) 0.029(3) Uani 1 1 d . . . . .
C6 C 1.1342(8) 0.5639(5) 0.7763(9) 0.036(4) Uani 1 1 d . . . . .
H6 H 1.2482 0.5849 0.8312 0.043 Uiso 1 1 calc R . . . .
O2A O 0.9493(6) 0.8493(3) 0.1752(6) 0.0338(19) Uani 1 1 d . . . . .
O2B O 0.8241(6) 0.9708(4) 0.7794(6) 0.032(2) Uani 1 1 d . . . . .
O3A O 0.5395(6) 0.6594(4) 0.2965(6) 0.030(3) Uani 1 1 d . . . . .
C2 C 1.0094(9) 0.9820(5) 0.2199(9) 0.040(4) Uani 1 1 d . . . . .
H2 H 0.9300 1.0470 0.2531 0.047 Uiso 1 1 calc R . . . .
N1 N 0.3476(7) 0.6846(4) 0.4997(7) 0.0338(19) Uani 1 1 d . . . . .
H1A H 0.3982 0.7229 0.5747 0.041 Uiso 1 1 calc R . . . .
H1B H 0.4379 0.6373 0.4702 0.041 Uiso 1 1 calc R . . . .
C3 C 0.4657(8) 0.5272(5) 0.2581(8) 0.031(4) Uani 1 1 d . . . . .
H3 H 0.4774 0.4867 0.1819 0.037 Uiso 1 1 calc R . . . .
N2 N 0.2643(7) 0.7680(4) 0.0856(8) 0.031(3) Uani 1 1 d . . . . .
H2A H 0.3856 0.7464 0.0927 0.037 Uiso 1 1 calc R . . . .
H2B H 0.2511 0.8171 0.1548 0.037 Uiso 1 1 calc R . . . .
O5B O 0.5943(6) 0.9435(3) 0.1903(6) 0.031(3) Uani 1 1 d . . . . .
C11 C 0.2796(10) 0.8123(6) 0.4239(10) 0.040(4) Uani 1 1 d . . . . .
H11A H 0.1882 0.8682 0.4584 0.059 Uiso 1 1 calc GR . . . .
H11B H 0.2219 0.7715 0.3434 0.059 Uiso 1 1 calc GR . . . .
H11C H 0.3835 0.8822 0.4197 0.059 Uiso 1 1 calc GR . . . .
C1 C 0.8574(10) 0.8349(6) 0.5197(10) 0.047(5) Uani 1 1 d . . . . .
H1 H 0.9722 0.8362 0.5755 0.057 Uiso 1 1 calc R . . . .
C10 C 0.1953(10) 0.5669(6) 0.5061(10) 0.039(4) Uani 1 1 d . . . . .
H10A H 0.2499 0.4777 0.5476 0.058 Uiso 1 1 calc GR . . . .
H10B H 0.1301 0.5344 0.4250 0.058 Uiso 1 1 calc GR . . . .
H10C H 0.1078 0.6129 0.5499 0.058 Uiso 1 1 calc GR . . . .
C12 C 0.1493(10) 0.6201(6) 0.0662(10) 0.031(4) Uani 1 1 d . . . . .
H12A H 0.2058 0.5453 0.0196 0.046 Uiso 1 1 calc GR . . . .
H12B H 0.0239 0.6401 0.0226 0.046 Uiso 1 1 calc GR . . . .
H12C H 0.1436 0.5790 0.1437 0.046 Uiso 1 1 calc GR . . . .
C4 C 0.6332(9) 0.7391(6) -0.0386(10) 0.027(3) Uani 1 1 d . . . . .
H4 H 0.5592 0.8259 -0.0570 0.032 Uiso 1 1 calc R . . . .
C13 C 0.2049(10) 0.8737(5) -0.0189(10) 0.042(5) Uani 1 1 d . . . . .
H13A H 0.2800 0.9693 -0.0036 0.064 Uiso 1 1 calc GR . . . .
H13B H 0.0740 0.8969 -0.0266 0.064 Uiso 1 1 calc GR . . . .
H13C H 0.2230 0.8221 -0.0932 0.064 Uiso 1 1 calc GR . . . .
O5A O 0.4210(6) 0.8183(4) 0.7271(7) 0.039(3) Uani 1 1 d . . . . .
C5 C 0.4152(8) 0.9624(5) 0.7204(9) 0.030(4) Uani 1 1 d . . . . .
H5 H 0.4179 1.0044 0.6456 0.036 Uiso 1 1 calc R . . . .
O6B O 1.0996(6) 0.4259(4) 0.7368(7) 0.036(3) Uani 1 1 d . . . . .
O6A O 1.0314(6) 0.6750(4) 0.7493(7) 0.034(3) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu2 0.0317(4) 0.0212(3) 0.0356(14) -0.0071(5) 0.0174(7) -0.0096(3)
Cu1 0.0310(4) 0.0207(3) 0.0411(13) -0.0061(4) 0.0188(7) -0.0090(2)
O1A 0.0398(19) 0.0388(14) 0.029(6) -0.004(2) 0.018(3) -0.0109(13)
O4A 0.041(2) 0.0267(16) 0.041(8) -0.011(3) 0.024(4) -0.0120(16)
O1B 0.0398(19) 0.0388(14) 0.029(6) -0.004(2) 0.018(3) -0.0109(13)
O4B 0.031(2) 0.0308(17) 0.010(8) 0.003(3) 0.006(4) -0.0040(15)
O3B 0.037(2) 0.0186(14) 0.032(8) -0.002(2) 0.012(4) -0.0100(14)
C6 0.031(3) 0.029(2) 0.051(11) -0.011(4) 0.022(6) -0.004(2)
O2A 0.0373(18) 0.0220(11) 0.046(6) -0.0092(18) 0.022(3) -0.0111(11)
O2B 0.036(2) 0.0232(15) 0.041(7) -0.007(2) 0.020(4) -0.0097(14)
O3A 0.033(2) 0.0279(16) 0.031(8) -0.010(3) 0.016(4) -0.0138(15)
C2 0.047(4) 0.019(2) 0.061(11) -0.007(4) 0.034(6) -0.007(2)
N1 0.0373(18) 0.0220(11) 0.046(6) -0.0092(18) 0.022(3) -0.0111(11)
C3 0.028(3) 0.024(2) 0.043(11) -0.012(4) 0.016(5) -0.009(2)
N2 0.035(3) 0.0232(19) 0.037(10) -0.004(3) 0.016(5) -0.0027(18)
O5B 0.038(2) 0.0202(14) 0.041(8) -0.003(2) 0.019(4) -0.0044(15)
C11 0.047(4) 0.036(3) 0.043(13) 0.002(4) 0.028(7) -0.002(3)
C1 0.046(4) 0.033(3) 0.070(14) -0.024(5) 0.037(7) -0.018(3)
C10 0.039(4) 0.035(3) 0.046(12) -0.007(4) 0.023(6) -0.014(2)
C12 0.038(3) 0.026(2) 0.032(11) 0.001(4) 0.015(6) -0.008(2)
C4 0.026(3) 0.031(2) 0.020(11) -0.005(4) -0.001(5) -0.003(2)
C13 0.054(4) 0.023(2) 0.058(14) -0.003(4) 0.032(7) -0.002(2)
O5A 0.048(3) 0.0275(16) 0.048(8) -0.007(3) 0.025(4) -0.0032(17)
C5 0.033(3) 0.029(2) 0.032(11) 0.001(4) 0.015(6) -0.003(2)
O6B 0.041(3) 0.0274(17) 0.042(8) -0.003(3) 0.015(4) -0.0039(16)
O6A 0.037(2) 0.0271(16) 0.041(8) -0.003(3) 0.016(4) 0.0002(15)

_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
Cu2 O1A 1.960(7) . ?
Cu2 O4B 1.914(7) . ?
Cu2 O3B 1.950(3) . ?
Cu2 O2B 1.936(3) . ?
Cu2 O5A 2.409(4) . ?
Cu2 O6A 2.172(4) . ?
Cu1 O4A 2.282(7) . ?
Cu1 O1B 2.236(7) . ?
Cu1 O2A 1.937(3) . ?
Cu1 O3A 1.931(3) . ?
Cu1 O5B 1.986(4) . ?
Cu1 O6B 1.934(4) 2_766 ?
O1A C1 1.259(6) . ?
O4A C4 1.239(11) . ?
O1B C1 1.212(13) . ?
O4B C4 1.260(7) 1_556 ?
O3B C3 1.253(7) 2_666 ?
C6 O6B 1.243(5) . ?
C6 O6A 1.229(8) . ?
O2A C2 1.251(5) . ?
O2B C2 1.261(5) 2_776 ?
O3A C3 1.258(5) . ?
C2 O2B 1.261(5) 2_776 ?
N1 C11 1.444(11) . ?
N1 C10 1.491(5) . ?
C3 O3B 1.253(7) 2_666 ?
N2 C12 1.480(5) . ?
N2 C13 1.508(13) . ?
O5B C5 1.271(8) 2_676 ?
C4 O4B 1.260(7) 1_554 ?
O5A C5 1.238(6) . ?
C5 O5B 1.271(8) 2_676 ?
O6B Cu1 1.934(4) 2_766 ?

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
O1A Cu2 O5A 90.0(2) . . ?
O1A Cu2 O6A 94.5(2) . . ?
O4B Cu2 O1A 176.11(16) . . ?
O4B Cu2 O3B 92.7(2) . . ?
O4B Cu2 O2B 89.0(2) . . ?
O4B Cu2 O5A 86.1(2) . . ?
O4B Cu2 O6A 89.3(2) . . ?
O3B Cu2 O1A 87.2(2) . . ?
O3B Cu2 O5A 80.45(13) . . ?
O3B Cu2 O6A 95.22(14) . . ?
O2B Cu2 O1A 90.4(2) . . ?
O2B Cu2 O3B 170.53(18) . . ?
O2B Cu2 O5A 90.40(13) . . ?
O2B Cu2 O6A 94.10(15) . . ?
O6A Cu2 O5A 173.57(17) . . ?
O1B Cu1 O4A 174.44(17) . . ?
O2A Cu1 O4A 93.1(2) . . ?
O2A Cu1 O1B 87.7(2) . . ?
O2A Cu1 O5B 88.95(16) . . ?
O3A Cu1 O4A 89.1(2) . . ?
O3A Cu1 O1B 90.2(2) . . ?
O3A Cu1 O2A 177.8(3) . . ?
O3A Cu1 O5B 91.49(17) . . ?
O3A Cu1 O6B 93.87(17) . 2_766 ?
O5B Cu1 O4A 85.4(2) . . ?
O5B Cu1 O1B 89.1(2) . . ?
O6B Cu1 O4A 92.9(2) 2_766 . ?
O6B Cu1 O1B 92.7(2) 2_766 . ?
O6B Cu1 O2A 85.76(17) 2_766 . ?
O6B Cu1 O5B 174.35(18) 2_766 . ?
C1 O1A Cu2 118.4(7) . . ?
C4 O4A Cu1 112.1(4) . . ?
C1 O1B Cu1 133.5(3) . . ?
C4 O4B Cu2 126.8(6) 1_556 . ?
C3 O3B Cu2 123.4(5) 2_666 . ?
O6A C6 O6B 125.9(8) . . ?
C2 O2A Cu1 117.8(3) . . ?
C2 O2B Cu2 120.6(3) 2_776 . ?
C3 O3A Cu1 122.4(3) . . ?
O2A C2 O2B 121.1(4) . 2_776 ?
C11 N1 C10 112.6(7) . . ?
O3B C3 O3A 121.0(6) 2_666 . ?
C12 N2 C13 111.0(7) . . ?
C5 O5B Cu1 115.5(6) 2_676 . ?
O1B C1 O1A 127.3(10) . . ?
O4A C4 O4B 126.3(7) . 1_554 ?
C5 O5A Cu2 105.6(3) . . ?
O5A C5 O5B 123.9(8) . 2_676 ?
C6 O6B Cu1 128.6(6) . 2_766 ?
C6 O6A Cu2 144.1(3) . . ?

_shelx_res_file                  
;
    CuForm_8_3GPa_synchr.res created by SHELXL-2014/7

TITL CuForm_8_3GPa_synchr_a.res in P-1
REM Old TITL CuForm_8_3GPa_synchr in P-1
REM SHELXT solution in P-1
REM R1 0.144, Rweak 0.002, Alpha 0.056, Orientation as input
REM Formula found by SHELXT: C11 N2 O11 Cu2
CELL 0.49647 7.2432 8.5444 11.2169 92.441 102.055 91.298
ZERR 2 0.0013 0.0011 0.0019 0.013 0.015 0.013
LATT 1
SFAC C H Cu N O
DISP C 0.0008 0.0007 6.2498
DISP Cu 0.3132 0.6683 1903.5186
DISP N 0.002 0.0014 9.3391
DISP O 0.0043 0.0027 13.9729
UNIT 20 44 4 4 24
EADP O2A N1
EADP O1A O1B

L.S. 40
PLAN  5
SIZE 0.056 0.072 0.11
list 4
fmap 2 53
acta
OMIT -5 -6 6
OMIT 5 -5 2
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_8_3GPa_synchr.hkl">
REM </olex2.extras>

WGHT    0.055400
FVAR       0.60918
CU2   3    0.745038    0.754911    0.732910    11.00000    0.03171    0.02124 =
         0.03563   -0.00705    0.01741   -0.00962
CU1   3    0.741643    0.753200    0.232845    11.00000    0.03098    0.02066 =
         0.04108   -0.00605    0.01879   -0.00899
O1A   5    0.712767    0.799968    0.559991    11.00000    0.03976    0.03882 =
         0.02908   -0.00402    0.01783   -0.01092
O4A   5    0.597537    0.656744    0.042510    11.00000    0.04130    0.02673 =
         0.04094   -0.01140    0.02407   -0.01203
O1B   5    0.863835    0.867118    0.416454    11.00000    0.03976    0.03882 =
         0.02908   -0.00402    0.01783   -0.01092
O4B   5    0.760001    0.716654    0.901483    11.00000    0.03128    0.03080 =
         0.00989    0.00313    0.00572   -0.00403
O3B   5    0.623462    0.550716    0.678913    11.00000    0.03691    0.01865 =
         0.03193   -0.00245    0.01170   -0.00998
C6    1    1.134234    0.563879    0.776284    11.00000    0.03139    0.02910 =
         0.05094   -0.01102    0.02193   -0.00395
AFIX  43
H6    2    1.248223    0.584923    0.831204    11.00000   -1.20000
AFIX   0
O2A   5    0.949317    0.849329    0.175225    11.00000    0.03729    0.02203 =
         0.04637   -0.00917    0.02206   -0.01111
O2B   5    0.824118    0.970750    0.779369    11.00000    0.03559    0.02320 =
         0.04096   -0.00732    0.01968   -0.00973
O3A   5    0.539530    0.659397    0.296521    11.00000    0.03319    0.02795 =
         0.03131   -0.00960    0.01573   -0.01384
C2    1    1.009423    0.982023    0.219889    11.00000    0.04651    0.01943 =
         0.06141   -0.00748    0.03430   -0.00749
AFIX  43
H2    2    0.929971    1.046995    0.253133    11.00000   -1.20000
AFIX   0

N1    4    0.347578    0.684597    0.499720    11.00000    0.03729    0.02203 =
         0.04637   -0.00917    0.02206   -0.01111
AFIX  23
H1A   2    0.398248    0.722893    0.574747    11.00000   -1.20000
H1B   2    0.437934    0.637303    0.470226    11.00000   -1.20000
AFIX   0

C3    1    0.465653    0.527173    0.258109    11.00000    0.02808    0.02401 =
         0.04314   -0.01159    0.01552   -0.00907
AFIX  43
H3    2    0.477370    0.486671    0.181859    11.00000   -1.20000
AFIX   0

N2    4    0.264315    0.767966    0.085642    11.00000    0.03505    0.02324 =
         0.03657   -0.00363    0.01620   -0.00267
AFIX  23
H2A   2    0.385632    0.746369    0.092656    11.00000   -1.20000
H2B   2    0.251124    0.817070    0.154807    11.00000   -1.20000
AFIX   0

O5B   5    0.594307    0.943543    0.190319    11.00000    0.03769    0.02015 =
         0.04052   -0.00305    0.01868   -0.00441
C11   1    0.279590    0.812315    0.423949    11.00000    0.04714    0.03626 =
         0.04338    0.00244    0.02799   -0.00218
AFIX 137
H11A  2    0.188158    0.868207    0.458410    11.00000   -1.50000
H11B  2    0.221944    0.771509    0.343380    11.00000   -1.50000
H11C  2    0.383459    0.882157    0.419675    11.00000   -1.50000
AFIX   0

C1    1    0.857377    0.834946    0.519743    11.00000    0.04587    0.03346 =
         0.07039   -0.02369    0.03692   -0.01769
AFIX  43
H1    2    0.972174    0.836246    0.575547    11.00000   -1.20000
AFIX   0

C10   1    0.195283    0.566932    0.506112    11.00000    0.03925    0.03549 =
         0.04570   -0.00713    0.02315   -0.01422
AFIX 137
H10A  2    0.249915    0.477702    0.547622    11.00000   -1.50000
H10B  2    0.130067    0.534387    0.424979    11.00000   -1.50000
H10C  2    0.107780    0.612922    0.549853    11.00000   -1.50000
AFIX   0

C12   1    0.149279    0.620115    0.066181    11.00000    0.03837    0.02553 =
         0.03169    0.00061    0.01531   -0.00807
AFIX 137
H12A  2    0.205763    0.545338    0.019578    11.00000   -1.50000
H12B  2    0.023877    0.640122    0.022644    11.00000   -1.50000
H12C  2    0.143583    0.578989    0.143700    11.00000   -1.50000
AFIX   0

C4    1    0.633183    0.739120   -0.038591    11.00000    0.02597    0.03080 =
         0.01962   -0.00458   -0.00127   -0.00298
AFIX  43
H4    2    0.559202    0.825931   -0.057032    11.00000   -1.20000
AFIX   0

C13   1    0.204939    0.873679   -0.018936    11.00000    0.05426    0.02288 =
         0.05808   -0.00267    0.03180   -0.00206
AFIX 137
H13A  2    0.279957    0.969327   -0.003617    11.00000   -1.50000
H13B  2    0.074048    0.896922   -0.026601    11.00000   -1.50000
H13C  2    0.223011    0.822088   -0.093166    11.00000   -1.50000
AFIX   0

O5A   5    0.420975    0.818284    0.727118    11.00000    0.04778    0.02750 =
         0.04838   -0.00714    0.02460   -0.00321
C5    1    0.415175    0.962423    0.720413    11.00000    0.03269    0.02908 =
         0.03177    0.00080    0.01476   -0.00260
AFIX  43
H5    2    0.417924    1.004373    0.645624    11.00000   -1.20000
AFIX   0
O6B   5    1.099617    0.425932    0.736775    11.00000    0.04058    0.02742 =
         0.04165   -0.00296    0.01473   -0.00391
O6A   5    1.031401    0.674968    0.749312    11.00000    0.03654    0.02714 =
         0.04101   -0.00319    0.01566    0.00018
HKLF 4

REM  CuForm_8_3GPa_synchr_a.res in P-1
REM R1 =  0.0508 for    1297 Fo > 4sig(Fo)  and  0.1064 for all    2430 data
REM    227 parameters refined using      0 restraints

END

WGHT      0.0835      0.0000

REM Highest difference peak  0.702,  deepest hole -0.504,  1-sigma level  0.109
Q1    1   0.8330  0.7060  0.7688  11.00000  0.05    0.70
Q2    1   0.8540  0.7173  0.3043  11.00000  0.05    0.70
Q3    1   0.6350  0.7839  0.6796  11.00000  0.05    0.61
Q4    1   0.6348  0.7846  0.1807  11.00000  0.05    0.60
Q5    1   0.8235  0.6679  1.0231  11.00000  0.05    0.47
;
_shelx_res_checksum              20969

# start Validation Reply Form
_vrf_PLAT029_CuForm_8_3GPa_synchr 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.471 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT660_CuForm_8_3GPa_synchr 
;
PROBLEM: No Valid _diffrn_radiation_type Value Reported .     Please Do !  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_8_3GPa_synchr 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1281 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.704
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.3860 2046 3 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.6140 1910 3 nmt -0.4145 -0.7020 0.1904 0.7507 -0.5398 -0.3323 1.1361 0.3412
0.8187

_twin_special_details            
;
Component 2 rotated by 124.5592° 
around [0.19 -0.12 0.97] (reciprocal) or [0.59 -0.09 0.80] (direct)
;
####################################################################### 
# 
# 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_CuForm_3_4GPa
_database_code_depnum_ccdc_archive 'CCDC 2067548'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C12 H12 Cu4 O24), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_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'
Cu Cu 0.3201 1.2651 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.323(3)
_cell_length_b                   8.4733(14)
_cell_length_c                   11.1183(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.553(12)
_cell_angle_gamma                90
_cell_volume                     781.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    415
_cell_measurement_temperature    294.13(10)
_cell_measurement_pressure       3.40(0.03)
_cell_measurement_theta_max      24.8230
_cell_measurement_theta_min      3.4110
_shelx_estimated_absorpt_T_max   0.873
_shelx_estimated_absorpt_T_min   0.768
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.319
_diffrn_reflns_Laue_measured_fraction_max 0.298
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            710
_diffrn_reflns_point_group_measured_fraction_full 0.319
_diffrn_reflns_point_group_measured_fraction_max 0.298
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.932
_diffrn_reflns_theta_min         3.026
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.319
_diffrn_measured_fraction_theta_max 0.298
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -40.00   1.00   30.00    --  -25.00 134.00 -57.00   57
  2  φ    -90.00 -27.00   1.00   30.00 -82.00 -25.00 134.00    --    63
  3  ω     40.00  97.00   1.00   30.00    --   25.00-134.00  57.00   57
  4  φ     27.00  90.00   1.00   30.00  82.00  25.00-134.00    --    63
  5  φ    -40.00  40.00   1.00   30.00   0.00   0.00   0.00    --    80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                188
_reflns_number_total             229
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         229
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.094
_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)+(0.0629P)²+0.9060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N1) = Uanis(C4)
Uanis(C1) = Uanis(O1)
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.7500 0.7500 0.7500 0.0162(13) Uani 1 2 d S T P . .
O3 O 0.3624(12) 0.4710(8) 0.6716(5) 0.022(3) Uani 1 1 d . . . . .
O1 O 0.7579(11) 0.8680(7) 0.5995(4) 0.019(2) Uani 1 1 d . . . . .
C1 C 0.7500 0.7959(17) 0.5000 0.019(2) Uani 1 2 d S T P . .
H1 H 0.7500 0.6862 0.5000 0.023 Uiso 1 2 calc RS T P . .
O2 O 0.5398(12) 0.6658(9) 0.6862(5) 0.0244(19) Uani 1 1 d . U . . .
N1 N 0.2500 0.6913(15) 0.5000 0.028(3) Uani 1 2 d S T P . .
H1A H 0.3056 0.6292 0.5528 0.034 Uiso 0.5 1 calc R . . . .
H1B H 0.1944 0.6292 0.4472 0.034 Uiso 0.5 1 calc R . . . .
C4 C 0.363(2) 0.7833(11) 0.4360(8) 0.028(3) Uani 1 1 d . . . . .
H4A H 0.3051 0.8441 0.3739 0.043 Uiso 1 1 calc GR . . . .
H4B H 0.4367 0.7137 0.4003 0.043 Uiso 1 1 calc GR . . . .
H4C H 0.4219 0.8530 0.4915 0.043 Uiso 1 1 calc GR . . . .
C2 C 0.4902(17) 0.5329(12) 0.7175(8) 0.025(6) Uani 1 1 d . . . . .
H2 H 0.5509 0.4778 0.7775 0.030 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.019(4) 0.0166(19) 0.0127(8) 0.0022(6) 0.0007(13) -0.0028(10)
O3 0.025(11) 0.017(7) 0.024(3) 0.005(3) 0.005(5) -0.010(5)
O1 0.028(8) 0.015(5) 0.017(2) -0.003(3) 0.010(4) 0.002(4)
C1 0.028(8) 0.015(5) 0.017(2) -0.003(3) 0.010(4) 0.002(4)
O2 0.024(2) 0.024(2) 0.0245(19) 0.0012(11) 0.0014(11) -0.0001(11)
N1 0.011(12) 0.046(10) 0.029(4) 0.000 0.005(6) 0.000
C4 0.011(12) 0.046(10) 0.029(4) 0.000 0.005(6) 0.000
C2 0.03(2) 0.017(10) 0.026(5) 0.000(4) 0.005(8) 0.007(7)

_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 O3 2.296(7) 6_665 ?
Cu1 O3 2.296(7) 4_556 ?
Cu1 O1 1.955(5) . ?
Cu1 O1 1.955(5) 7_666 ?
Cu1 O2 1.969(9) . ?
Cu1 O2 1.969(9) 7_666 ?
O3 Cu1 2.296(7) 4_546 ?
O3 C2 1.257(15) . ?
O1 C1 1.260(9) . ?
C1 O1 1.260(9) 2_656 ?
C1 H1 0.9300 . ?
O2 C2 1.258(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C4 1.451(14) 2_556 ?
N1 C4 1.451(14) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2 0.9300 . ?

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
O3 Cu1 O3 180.0 4_556 6_665 ?
O1 Cu1 O3 87.2(2) . 4_556 ?
O1 Cu1 O3 92.8(2) . 6_665 ?
O1 Cu1 O3 87.2(2) 7_666 6_665 ?
O1 Cu1 O3 92.8(2) 7_666 4_556 ?
O1 Cu1 O1 180.0 . 7_666 ?
O1 Cu1 O2 88.0(3) . . ?
O1 Cu1 O2 88.0(3) 7_666 7_666 ?
O1 Cu1 O2 92.0(3) 7_666 . ?
O1 Cu1 O2 92.0(3) . 7_666 ?
O2 Cu1 O3 93.2(4) 7_666 6_665 ?
O2 Cu1 O3 86.8(4) . 6_665 ?
O2 Cu1 O3 93.2(4) . 4_556 ?
O2 Cu1 O3 86.8(4) 7_666 4_556 ?
O2 Cu1 O2 180.0 7_666 . ?
C2 O3 Cu1 122.9(7) . 4_546 ?
C1 O1 Cu1 120.1(7) . . ?
O1 C1 O1 122.1(13) 2_656 . ?
O1 C1 H1 119.0 2_656 . ?
O1 C1 H1 119.0 . . ?
C2 O2 Cu1 121.8(7) . . ?
H1A N1 H1B 107.5 . . ?
C4 N1 H1A 108.5 . . ?
C4 N1 H1A 108.5 2_556 . ?
C4 N1 H1B 108.5 2_556 . ?
C4 N1 H1B 108.5 . . ?
C4 N1 C4 115.0(14) . 2_556 ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C2 O2 123.2(11) . . ?
O3 C2 H2 118.4 . . ?
O2 C2 H2 118.4 . . ?

_shelx_res_file                  
;
    cuform_3_4gpa.res created by SHELXL-2014/7

TITL CuForm_3_4GPa_a.res in I2/a
REM Old TITL CuForm_3_4GPa_a.res in I2/a
REM SHELXT solution in I2/a
REM R1 0.080, Rweak 0.004, Alpha 0.060, Orientation as input
REM Formula found by SHELXT: C5 Cu O7
CELL 0.71073 8.3233 8.4733 11.1183 90 94.553 90
ZERR 4 0.0025 0.0014 0.0007 0 0.012 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 0.5-X,+Y,1-Z
EQIV $2 1-X,2-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
ISOR 0.001 0.002 O2
EADP N1 C4
EADP C1 O1

L.S. 40
PLAN  5
SIZE 0.1 0.08 0.05
RTAB NO N1 O3_$1
RTAB NO N1 O2_$1
RTAB CO C4 O1_$2
RTAB CO C4 O3_$3
RTAB HO H1a O3_$1
RTAB HO H1a O2_$1
RTAB HO H4a O1_$2
RTAB HO H4b O3_$3
RTAB NHO N1 H1a O3_$1
RTAB NHO N1 H1a O2_$1
RTAB CHO C4 H4a O1_$2
RTAB CHO C4 H4b O3_$3
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_3_4GPa.hkl">
REM </olex2.extras>

WGHT    0.062900    0.906000
FVAR       0.70315
CU1   3    0.750000    0.750000    0.750000    10.50000    0.01924    0.01655 =
         0.01268    0.00215    0.00065   -0.00284
O3    5    0.362364    0.470994    0.671586    11.00000    0.02483    0.01708 =
         0.02394    0.00518    0.00492   -0.00959
O1    5    0.757858    0.867951    0.599456    11.00000    0.02804    0.01483 =
         0.01653   -0.00257    0.00991    0.00245
C1    1    0.750000    0.795931    0.500000    10.50000    0.02804    0.01483 =
         0.01653   -0.00257    0.00991    0.00245
AFIX  43
H1    2    0.750000    0.686174    0.500000    10.50000   -1.20000
AFIX   0
O2    5    0.539832    0.665754    0.686184    11.00000    0.02434    0.02417 =
         0.02454    0.00122    0.00140   -0.00006

N1    4    0.250000    0.691279    0.500000    10.50000    0.01067    0.04602 =
         0.02923    0.00000    0.00530    0.00000
AFIX  23
H1A   2    0.305599    0.629188    0.552772    10.50000   -1.20000
H1B   2    0.194399    0.629192    0.447227    10.50000   -1.20000
AFIX   0
C4    1    0.362966    0.783322    0.436007    11.00000    0.01067    0.04602 =
         0.02923    0.00000    0.00530    0.00000
AFIX 137
H4A   2    0.305063    0.844140    0.373915    11.00000   -1.50000
H4B   2    0.436736    0.713700    0.400273    11.00000   -1.50000
H4C   2    0.421851    0.853031    0.491487    11.00000   -1.50000
AFIX   0

C2    1    0.490161    0.532918    0.717473    11.00000    0.03271    0.01662 =
         0.02564   -0.00013    0.00490    0.00693
AFIX  43
H2    2    0.550904    0.477817    0.777461    11.00000   -1.20000
AFIX   0
HKLF 4

REM  CuForm_3_4GPa_a.res in I2/a
REM R1 =  0.0434 for     188 Fo > 4sig(Fo)  and  0.0524 for all     229 data
REM     53 parameters refined using      6 restraints

END

WGHT      0.0630      0.8900

REM Highest difference peak  0.342,  deepest hole -0.331,  1-sigma level  0.093
Q1    1   0.4976  0.7299  0.7424  11.00000  0.05    0.34
Q2    1   0.4632  0.4363  0.6563  11.00000  0.05    0.30
Q3    1   0.5034  0.7633  0.4480  11.00000  0.05    0.28
Q4    1   0.4523  0.6336  0.6925  11.00000  0.05    0.28
Q5    1   0.2262  0.7622  0.4085  11.00000  0.05    0.27
;
_shelx_res_checksum              77448

# start Validation Reply Form
_vrf_PLAT029_CuForm_3_4GPa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.319 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_3_4GPa       
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.32 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_3_4GPa       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        272 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;
####################################################################### 
# 
# 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_CuForm_7_15GPa
_database_code_depnum_ccdc_archive 'CCDC 2067551'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H6 Cu2 O12, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H22 Cu2 N2 O12'
_chemical_formula_weight         489.37
_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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.2638(16)
_cell_length_b                   8.5726(15)
_cell_length_c                   11.2929(17)
_cell_angle_alpha                92.384(13)
_cell_angle_beta                 101.797(16)
_cell_angle_gamma                91.352(16)
_cell_volume                     687.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    766
_cell_measurement_temperature    293.72(19)
_cell_measurement_pressure       7.15(0.03)
_cell_measurement_theta_max      21.1490
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   0.857
_shelx_estimated_absorpt_T_min   0.742
_exptl_absorpt_coefficient_mu    3.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.264
_diffrn_reflns_Laue_measured_fraction_max 0.214
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3829
_diffrn_reflns_point_group_measured_fraction_full 0.264
_diffrn_reflns_point_group_measured_fraction_max 0.214
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.369
_diffrn_reflns_theta_min         1.844
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.264
_diffrn_measured_fraction_theta_max 0.214
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00 -26.00   1.00   20.00    --  -27.18 -39.00  90.00    1
  2  ω    -27.00  21.00   1.00   60.00    --  -27.18 -39.00  12.00   48
  3  ω     -3.00  27.00   1.00   60.00    --  -27.18 -26.00   7.00   30
  4  ω    -20.00   6.00   1.00   60.00    --  -27.18  26.00  -7.00   26
  5  ω    -55.00  -1.00   1.00   60.00    --  -27.18  39.00 -12.00   54
  6  φ    -40.00  20.00   1.00   60.00   0.00 -30.00   0.00    --    60
  7  φ    -20.00  40.00   1.00   60.00   0.00  30.00   0.00    --    60
  8  ω    -27.00  28.00   1.00   60.00    --   27.65  39.00 -12.00   55
  9  ω    -21.00  36.00   1.00   60.00    --   27.65  13.00  -3.00   57
 10  ω      5.00  31.00   1.00   60.00    --   27.65 -39.00  12.00   26
 11  ω    -28.00  55.00   1.00   20.00    --    0.23 -39.00  12.00   83
 12  ω    -52.00   7.00   1.00   20.00    --    0.23  39.00 -12.00   59
 13  φ    -20.00  40.00   1.00   20.00   0.00   0.00 -10.00    --    60
 14  φ    -40.00  20.00   1.00   20.00   0.00   0.00  10.00    --    60
 15  φ    -40.00  40.00   1.00   20.00   0.00   0.00   0.00    --    80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                440
_reflns_number_total             737
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         737
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0767
_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)+(0.1401P)²+10.2624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2386
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H10B-H1_$3
 2.05 with sigma of 0.001
 H12A-H6_$8
 2.05 with sigma of 0.001
 H11A-O3A \\sim O3A-H1B
 with sigma of 0.02
 H1A-H10C \\sim H10C-H1B
 with sigma of 0.02
 H2A-H13B \\sim H13B-H2B
 with sigma of 0.02
 H2A-H12C \\sim H12C-H2B
 with sigma of 0.02
 H1B-H11B \\sim H11B-H1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C5) \\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(Cu1) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2B) \\sim Ueq,
Uanis(Cu2) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O3A)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4B) \\sim Ueq,
Uanis(O1A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O1B) \\sim Ueq, Uanis(O5A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6A) = Uanis(C6) = Uanis(O6B)
Uanis(O5A) = Uanis(C5)
Uanis(C12) = Uanis(C13) = Uanis(N2)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C1(H1), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.7457(10) 0.7539(5) 0.7355(2) 0.0199(11) Uani 1 1 d . U . . .
Cu1 Cu 0.7431(10) 0.7523(6) 0.2353(2) 0.0220(11) Uani 1 1 d . U . . .
O1A O 0.712(5) 0.800(3) 0.5653(13) 0.027(4) Uani 1 1 d . U . . .
O4A O 0.614(5) 0.652(3) 0.0469(13) 0.019(4) Uani 1 1 d . U . . .
O1B O 0.855(5) 0.868(3) 0.4192(13) 0.027(4) Uani 1 1 d . U . . .
O4B O 0.766(5) 0.709(3) 0.9043(13) 0.023(4) Uani 1 1 d . U . . .
O3B O 0.638(5) 0.549(3) 0.6822(13) 0.024(4) Uani 1 1 d . U . . .
C6 C 1.135(6) 0.558(4) 0.7756(19) 0.031(3) Uani 1 1 d . U . . .
H6 H 1.2510 0.5693 0.8285 0.038 Uiso 1 1 calc DR . . . .
O2A O 0.957(5) 0.848(3) 0.1790(14) 0.026(4) Uani 1 1 d . U . . .
O2B O 0.814(5) 0.972(3) 0.7815(14) 0.031(4) Uani 1 1 d . U . . .
O3A O 0.520(5) 0.666(3) 0.2970(13) 0.024(4) Uani 1 1 d D U . . .
C2 C 1.004(7) 0.988(4) 0.2187(19) 0.021(6) Uani 1 1 d . U . . .
H2 H 0.9213 1.0554 0.2455 0.025 Uiso 1 1 calc R . . . .
N1 N 0.341(6) 0.686(4) 0.4974(16) 0.031(5) Uani 1 1 d . U . . .
H1A H 0.3856 0.7271 0.5716 0.037 Uiso 1 1 calc DR . . . .
H1B H 0.4350 0.6363 0.4742 0.037 Uiso 1 1 calc DR . . . .
C3 C 0.461(8) 0.525(4) 0.2607(19) 0.023(6) Uani 1 1 d . U . . .
H3 H 0.4923 0.4795 0.1917 0.027 Uiso 1 1 calc R . . . .
N2 N 0.271(6) 0.762(4) 0.0829(17) 0.032(4) Uani 1 1 d . U . . .
H2A H 0.3885 0.7347 0.0828 0.039 Uiso 1 1 calc DR . . . .
H2B H 0.2689 0.8084 0.1546 0.039 Uiso 1 1 calc DR . . . .
O5B O 0.579(6) 0.946(3) 0.1928(15) 0.032(4) Uani 1 1 d . U . . .
C11 C 0.295(6) 0.804(3) 0.424(2) 0.038(7) Uani 1 1 d . U . . .
H11A H 0.2566 0.7631 0.3416 0.057 Uiso 1 1 calc DGR . . . .
H11B H 0.4029 0.8734 0.4299 0.057 Uiso 1 1 calc DGR . . . .
H11C H 0.1943 0.8597 0.4468 0.057 Uiso 1 1 calc GR . . . .
C1 C 0.860(5) 0.830(3) 0.5232(19) 0.026(6) Uani 1 1 d . U . . .
H1 H 0.9774 0.8235 0.5743 0.032 Uiso 1 1 calc DR . . . .
C10 C 0.201(5) 0.571(3) 0.5065(19) 0.032(7) Uani 1 1 d . U . . .
H10A H 0.1534 0.5215 0.4282 0.049 Uiso 1 1 calc GR . . . .
H10B H 0.1008 0.6201 0.5358 0.049 Uiso 1 1 calc DGR . . . .
H10C H 0.2556 0.4945 0.5617 0.049 Uiso 1 1 calc DGR . . . .
C12 C 0.149(6) 0.626(4) 0.0632(18) 0.032(4) Uani 1 1 d . U . . .
H12A H 0.1533 0.5756 -0.0135 0.048 Uiso 1 1 calc DGR . . . .
H12B H 0.0221 0.6564 0.0633 0.048 Uiso 1 1 calc GR . . . .
H12C H 0.1880 0.5556 0.1266 0.048 Uiso 1 1 calc DGR . . . .
C4 C 0.627(8) 0.731(5) -0.040(2) 0.033(6) Uani 1 1 d . U . . .
H4 H 0.5391 0.8053 -0.0658 0.040 Uiso 1 1 calc R . . . .
C13 C 0.206(8) 0.873(4) -0.017(2) 0.032(4) Uani 1 1 d . U . . .
H13A H 0.2117 0.8234 -0.0936 0.048 Uiso 1 1 calc GR . . . .
H13B H 0.2870 0.9654 -0.0034 0.048 Uiso 1 1 calc DGR . . . .
H13C H 0.0794 0.9017 -0.0165 0.048 Uiso 1 1 calc GR . . . .
O5A O 0.429(6) 0.817(3) 0.7289(15) 0.034(4) Uani 1 1 d . U . . .
C5 C 0.399(9) 0.971(5) 0.719(2) 0.034(4) Uani 1 1 d . U . . .
H5 H 0.3627 1.0122 0.6429 0.041 Uiso 1 1 calc R . . . .
O6B O 1.082(6) 0.432(3) 0.7302(14) 0.031(3) Uani 1 1 d . . . . .
O6A O 1.039(6) 0.672(3) 0.7542(15) 0.031(3) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu2 0.0186(17) 0.0194(15) 0.0220(11) 0.0024(9) 0.0054(11) -0.0020(10)
Cu1 0.0212(17) 0.0230(15) 0.0228(11) 0.0038(9) 0.0064(10) -0.0009(11)
O1A 0.027(4) 0.027(4) 0.027(4) 0.0016(12) 0.0057(14) 0.0008(12)
O4A 0.019(4) 0.019(4) 0.019(4) 0.0012(12) 0.0039(14) 0.0005(12)
O1B 0.027(4) 0.027(4) 0.027(4) 0.0014(12) 0.0056(14) 0.0009(12)
O4B 0.023(4) 0.023(4) 0.023(4) 0.0013(12) 0.0048(14) 0.0005(12)
O3B 0.024(4) 0.024(4) 0.024(4) 0.0012(12) 0.0048(14) 0.0008(12)
C6 0.031(3) 0.031(3) 0.032(3) 0.0014(12) 0.0066(13) 0.0008(12)
O2A 0.026(4) 0.026(4) 0.027(4) 0.0014(12) 0.0054(15) 0.0005(12)
O2B 0.031(4) 0.031(4) 0.031(4) 0.0018(12) 0.0064(15) 0.0008(12)
O3A 0.024(4) 0.024(4) 0.025(4) 0.0015(12) 0.0052(14) 0.0004(12)
C2 0.021(6) 0.021(6) 0.021(6) 0.0012(12) 0.0043(16) 0.0006(12)
N1 0.031(5) 0.031(5) 0.031(5) 0.0014(12) 0.0064(16) 0.0010(12)
C3 0.023(6) 0.023(6) 0.023(6) 0.0012(12) 0.0047(17) 0.0007(12)
N2 0.032(4) 0.032(4) 0.032(4) 0.0016(10) 0.0068(12) 0.0011(10)
O5B 0.032(5) 0.032(5) 0.032(4) 0.0012(12) 0.0064(15) 0.0011(12)
C11 0.038(8) 0.038(8) 0.038(7) 0.002(2) 0.008(3) 0.002(2)
C1 0.026(6) 0.026(6) 0.026(6) 0.0012(12) 0.0055(17) 0.0009(12)
C10 0.033(7) 0.033(7) 0.032(7) 0.002(2) 0.007(3) 0.001(2)
C12 0.032(4) 0.032(4) 0.032(4) 0.0016(10) 0.0068(12) 0.0011(10)
C4 0.034(7) 0.034(7) 0.033(7) 0.0015(12) 0.0069(18) 0.0012(12)
C13 0.032(4) 0.032(4) 0.032(4) 0.0016(10) 0.0068(12) 0.0011(10)
O5A 0.034(4) 0.034(4) 0.034(4) 0.0016(9) 0.0071(12) 0.0011(8)
C5 0.034(4) 0.034(4) 0.034(4) 0.0016(9) 0.0071(12) 0.0011(8)
O6B 0.031(3) 0.031(3) 0.032(3) 0.0014(12) 0.0066(13) 0.0008(12)
O6A 0.031(3) 0.031(3) 0.032(3) 0.0014(12) 0.0066(13) 0.0008(12)

_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
Cu2 O1A 1.947(16) . ?
Cu2 O4B 1.938(14) . ?
Cu2 O3B 1.930(16) . ?
Cu2 O2B 1.94(2) . ?
Cu2 O5A 2.37(5) . ?
Cu2 O6A 2.23(5) . ?
Cu1 O4A 2.269(15) . ?
Cu1 O1B 2.247(15) . ?
Cu1 O2A 1.97(2) . ?
Cu1 O3A 2.03(2) . ?
Cu1 O5B 2.08(5) . ?
Cu1 O6B 2.05(5) 2_766 ?
O1A C1 1.29(4) . ?
O4A C4 1.23(3) . ?
O1B C1 1.22(2) . ?
O4B C4 1.30(6) 1_556 ?
O3B C3 1.24(3) 2_666 ?
C6 H6 0.9300 . ?
C6 O6B 1.19(3) . ?
C6 O6A 1.21(7) . ?
O2A C2 1.27(3) . ?
O2B C2 1.36(5) 2_776 ?
O3A C3 1.29(3) . ?
C2 O2B 1.36(5) 2_776 ?
C2 H2 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C11 1.34(4) . ?
N1 C10 1.41(3) . ?
C3 O3B 1.24(3) 2_666 ?
C3 H3 0.9300 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C12 1.43(3) . ?
N2 C13 1.51(6) . ?
O5B C5 1.18(3) 2_676 ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C1 H1 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C4 O4B 1.30(6) 1_554 ?
C4 H4 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O5A C5 1.35(6) . ?
C5 O5B 1.18(3) 2_676 ?
C5 H5 0.9300 . ?
O6B Cu1 2.05(5) 2_766 ?

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
O1A Cu2 O5A 89.1(14) . . ?
O1A Cu2 O6A 95.8(13) . . ?
O4B Cu2 O1A 177.2(16) . . ?
O4B Cu2 O2B 90.0(7) . . ?
O4B Cu2 O5A 88.2(13) . . ?
O4B Cu2 O6A 87.0(13) . . ?
O3B Cu2 O1A 87.4(7) . . ?
O3B Cu2 O4B 92.0(6) . . ?
O3B Cu2 O2B 170.9(17) . . ?
O3B Cu2 O5A 83.4(13) . . ?
O3B Cu2 O6A 92.5(14) . . ?
O2B Cu2 O1A 90.1(8) . . ?
O2B Cu2 O5A 87.8(14) . . ?
O2B Cu2 O6A 96.4(14) . . ?
O6A Cu2 O5A 173.5(7) . . ?
O1B Cu1 O4A 175.4(16) . . ?
O2A Cu1 O4A 92.1(7) . . ?
O2A Cu1 O1B 88.8(7) . . ?
O2A Cu1 O3A 176.8(12) . . ?
O2A Cu1 O5B 92.2(14) . . ?
O2A Cu1 O6B 83.7(14) . 2_766 ?
O3A Cu1 O4A 89.7(7) . . ?
O3A Cu1 O1B 89.2(8) . . ?
O3A Cu1 O5B 85.2(13) . . ?
O3A Cu1 O6B 98.9(12) . 2_766 ?
O5B Cu1 O4A 87.1(11) . . ?
O5B Cu1 O1B 88.3(11) . . ?
O6B Cu1 O4A 92.0(11) 2_766 . ?
O6B Cu1 O1B 92.6(12) 2_766 . ?
O6B Cu1 O5B 175.8(8) 2_766 . ?
C1 O1A Cu2 118(3) . . ?
C4 O4A Cu1 117.8(14) . . ?
C1 O1B Cu1 134.6(13) . . ?
C4 O4B Cu2 122(3) 1_556 . ?
C3 O3B Cu2 122.8(17) 2_666 . ?
O6B C6 H6 119.3 . . ?
O6B C6 O6A 121(4) . . ?
O6A C6 H6 119.3 . . ?
C2 O2A Cu1 116(3) . . ?
C2 O2B Cu2 114(3) 2_776 . ?
C3 O3A Cu1 117(2) . . ?
O2A C2 O2B 114(4) . 2_776 ?
O2A C2 H2 123.1 . . ?
O2B C2 H2 123.1 2_776 . ?
H1A N1 H1B 107.0 . . ?
C11 N1 H1A 107.5 . . ?
C11 N1 H1B 107.5 . . ?
C11 N1 C10 119(4) . . ?
C10 N1 H1A 107.5 . . ?
C10 N1 H1B 107.5 . . ?
O3B C3 O3A 120(3) 2_666 . ?
O3B C3 H3 120.0 2_666 . ?
O3A C3 H3 120.0 . . ?
H2A N2 H2B 108.3 . . ?
C12 N2 H2A 109.9 . . ?
C12 N2 H2B 109.9 . . ?
C12 N2 C13 109(3) . . ?
C13 N2 H2A 109.9 . . ?
C13 N2 H2B 109.9 . . ?
C5 O5B Cu1 107(4) 2_676 . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1A C1 H1 118.4 . . ?
O1B C1 O1A 123(4) . . ?
O1B C1 H1 118.4 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4A C4 O4B 120(6) . 1_554 ?
O4A C4 H4 120.1 . . ?
O4B C4 H4 120.1 1_554 . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 O5A Cu2 113(3) . . ?
O5B C5 O5A 119(4) 2_676 . ?
O5B C5 H5 120.3 2_676 . ?
O5A C5 H5 120.3 . . ?
C6 O6B Cu1 119(4) . 2_766 ?
C6 O6A Cu2 143(2) . . ?

_shelx_res_file                  
;
    cuform_7_15gpa.res created by SHELXL-2014/7

TITL CuForm_7_15GPa_a.res in P-1
REM Old TITL CuForm_7_15GPa_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.186, Rweak 0.007, Alpha 0.121, Orientation as input
REM Formula found by SHELXT: C12 N2 O9 Cu2
CELL 0.71073 7.2638 8.5726 11.2929 92.384 101.797 91.352
ZERR 2 0.0016 0.0015 0.0017 0.013 0.016 0.016
LATT 1
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 1-X,1-Y,1-Z
EQIV $2 2-X,1-Y,1-Z
EQIV $3 -1+X,+Y,+Z
EQIV $4 2-X,2-Y,1-Z
EQIV $5 +X,+Y,-1+Z
EQIV $6 1-X,2-Y,1-Z
EQIV $7 1-X,1-Y,-Z
EQIV $8 -1+X,+Y,-1+Z
DFIX 2.05 0.001 H10b H1_$3
DFIX 2.05 0.001 H12a H6_$8
SADI H11a O3A O3A H1b
SADI H1a H10c H10c H1b
SADI H2a H13b H13b H2b
SADI H2a H12c H12c H2b
SADI H1b H11b H11b H1a
ISOR 0.001 0.002 C10 N1 C11
ISOR 0.001 0.002 C12 N2 C13
ISOR 0.001 0.002 C5 O5B Cu1 C6 O2A C2 O2B Cu2 O3B C3 O3A O4A C4 O4B O1A C1 =
 O1B O5A
EADP O6A C6 O6B
EADP O5A C5
EADP C12 C13 N2

L.S. 40
PLAN  5
SIZE 0.1 0.08 0.05
RTAB OO O1B O4A
RTAB OO O2A O3A
RTAB OO O5B O6B_$2
RTAB OO O1A O4B
RTAB OO O3B O2B
RTAB OO O5A O6A
RTAB NO N1 O1A
RTAB NO N1 O3B
RTAB NO N1 O3B_$1
RTAB NO N1 O3A
RTAB NO N1 O5A
RTAB HON H1b O1A
RTAB HON H1b O3B
RTAB HON H1b O3B_$1
RTAB HON H1b O3A
RTAB HON H1a O1A
RTAB HON H1a O3B_$1
RTAB HON H1a O5A
RTAB NHO N1 H1b O1A
RTAB NHO N1 H1b O3B
RTAB NHO N1 H1b O3B_$1
RTAB NHO N1 H1b O3A
RTAB NHO N1 H1a O1A
RTAB NHO N1 H1a O3B_$1
RTAB NHO N1 H1a O5A
RTAB CO C11 O2A_$3
RTAB CO C11 O3A
RTAB CO C11 O1A
RTAB CO C11 O1B_$3
RTAB HOC H11a O2A_$3
RTAB HOC H11a O3A
RTAB HOC H11b O1A
RTAB HOC H11b O3A
RTAB HOC H11c O1B_$3
RTAB CHO C11 H11a O2A_$3
RTAB CHO C11 H11a O3A
RTAB CHO C11 H11b O1A
RTAB CHO C11 H11b O3A
RTAB CHO C11 H11c O1B_$3
RTAB CO C10 O3B
RTAB CO C10 O6A_$1
RTAB CO C10 O6B_$1
RTAB CO C10 O6A_$3
RTAB CO C10 O3A_$1
RTAB CO C10 O6B_$3
RTAB HOC H10a O3B
RTAB HOC H10a O6A_$1
RTAB HOC H10a O6B_$1
RTAB HOC H10b O6A_$3
RTAB HOC H10c O3A_$1
RTAB HOC H10c O6B_$3
RTAB CHO C10 H10a O3B
RTAB CHO C10 H10a O6A_$1
RTAB CHO C10 H10a O6B_$1
RTAB CHO C10 H10b O6A_$3
RTAB CHO C10 H10c O3A_$1
RTAB CHO C10 H10c O6B_$3
RTAB COF C6 O4A_$2
RTAB COF C2 O6A_$4
RTAB COF C4 O5A_$5
RTAB HOF H6 O4A_$2
RTAB HOF H2 O6A_$4
RTAB HOF H4 O5A_$5
RTAB CHOF C6 H6 O4A_$2
RTAB CHOF C2 H2 O6A_$4
RTAB CHOF C4 H4 O5A_$5
RTAB NO2 N2 O3A
RTAB NO2 N2 O4A
RTAB NO2 N2 O5B_$6
RTAB NO2 N2 O2A_$3
RTAB NO2 N2 O2B_$3
RTAB HO2 H2 O3A
RTAB HO2 H2 O4A
RTAB HO2 H2 O5B_$6
RTAB HO2 H2 O2A_$3
RTAB HO2 H2 O2B_$3
RTAB NHO2 N2 H2 O3A
RTAB NHO2 N2 H2 O4A
RTAB NHO2 N2 H2 O5B_$6
RTAB NHO2 N2 H2 O2A_$3
RTAB NHO2 N2 H2 O2B_$3
RTAB CO2 C12 O4A_$7
RTAB CO2 C12 O2A_$3
RTAB CO2 C12 O4B_$3
RTAB CO2 C12 O4B_$7
RTAB CO2 C12 O3B
RTAB CO2 C13 O6A_$8
RTAB CO2 C13 O5B_$5
RTAB CO2 C13 O2A_$3
BIND O5A Cu2
BOND $H
list 4
fmap 2
acta
OMIT 1 3 3
OMIT 0 2 9
OMIT -1 -2 5
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_7_15GPa.hkl">
REM </olex2.extras>

WGHT    0.140100   10.262400
FVAR       0.59813
CU2   3    0.745732    0.753897    0.735470    11.00000    0.01862    0.01943 =
         0.02202    0.00238    0.00542   -0.00203
CU1   3    0.743063    0.752328    0.235333    11.00000    0.02123    0.02296 =
         0.02277    0.00382    0.00645   -0.00094
O1A   5    0.712442    0.800365    0.565277    11.00000    0.02703    0.02705 =
         0.02707    0.00160    0.00573    0.00078
O4A   5    0.613664    0.651659    0.046916    11.00000    0.01891    0.01895 =
         0.01898    0.00121    0.00393    0.00051
O1B   5    0.854516    0.867570    0.419198    11.00000    0.02683    0.02689 =
         0.02673    0.00140    0.00561    0.00089
O4B   5    0.765975    0.709093    0.904326    11.00000    0.02258    0.02268 =
         0.02284    0.00131    0.00476    0.00052
O3B   5    0.637957    0.548621    0.682246    11.00000    0.02373    0.02371 =
         0.02376    0.00117    0.00484    0.00076
C6    1    1.134636    0.558236    0.775608    11.00000    0.03120    0.03138 =
         0.03164    0.00145    0.00657    0.00084
AFIX  43
H6    2    1.250977    0.569324    0.828485    11.00000   -1.20000
AFIX   0
O2A   5    0.956888    0.847860    0.178985    11.00000    0.02609    0.02590 =
         0.02656    0.00144    0.00543    0.00053
O2B   5    0.813602    0.971762    0.781549    11.00000    0.03077    0.03076 =
         0.03100    0.00181    0.00645    0.00076
O3A   5    0.519831    0.665820    0.296950    11.00000    0.02433    0.02433 =
         0.02478    0.00153    0.00524    0.00039
C2    1    1.003846    0.987558    0.218744    11.00000    0.02103    0.02110 =
         0.02106    0.00116    0.00432    0.00062
AFIX  43
H2    2    0.921285    1.055414    0.245461    11.00000   -1.20000
AFIX   0

N1    4    0.340840    0.685532    0.497429    11.00000    0.03083    0.03086 =
         0.03089    0.00139    0.00642    0.00103
AFIX  23
H1A   2    0.385621    0.727127    0.571559    11.00000   -1.20000
H1B   2    0.434971    0.636343    0.474177    11.00000   -1.20000
AFIX   0

C3    1    0.460714    0.525199    0.260664    11.00000    0.02278    0.02276 =
         0.02292    0.00115    0.00475    0.00065
AFIX  43
H3    2    0.492275    0.479458    0.191688    11.00000   -1.20000
AFIX   0

N2    4    0.271025    0.761915    0.082936    11.00000    0.03223    0.03234 =
         0.03218    0.00163    0.00676    0.00107
AFIX  23
H2A   2    0.388472    0.734706    0.082802    11.00000   -1.20000
H2B   2    0.268901    0.808354    0.154590    11.00000   -1.20000
AFIX   0

O5B   5    0.579264    0.946246    0.192792    11.00000    0.03225    0.03211 =
         0.03232    0.00124    0.00643    0.00108
C11   1    0.295428    0.803885    0.423659    11.00000    0.03834    0.03844 =
         0.03813    0.00169    0.00806    0.00152
AFIX 137
H11A  2    0.256650    0.763056    0.341632    11.00000   -1.50000
H11B  2    0.402892    0.873404    0.429872    11.00000   -1.50000
H11C  2    0.194301    0.859740    0.446774    11.00000   -1.50000
AFIX   0

C1    1    0.860283    0.830380    0.523181    11.00000    0.02633    0.02638 =
         0.02630    0.00116    0.00554    0.00092
AFIX  43
H1    2    0.977376    0.823467    0.574327    11.00000   -1.20000
AFIX   0

C10   1    0.201495    0.571259    0.506503    11.00000    0.03258    0.03268 =
         0.03216    0.00152    0.00699    0.00145
AFIX 137
H10A  2    0.153379    0.521542    0.428165    11.00000   -1.50000
H10B  2    0.100843    0.620111    0.535838    11.00000   -1.50000
H10C  2    0.255641    0.494525    0.561667    11.00000   -1.50000
AFIX   0

C12   1    0.148564    0.626239    0.063206    11.00000    0.03223    0.03234 =
         0.03218    0.00163    0.00676    0.00107
AFIX 137
H12A  2    0.153263    0.575616   -0.013512    11.00000   -1.50000
H12B  2    0.022136    0.656365    0.063290    11.00000   -1.50000
H12C  2    0.188031    0.555594    0.126586    11.00000   -1.50000
AFIX   0

C4    1    0.627409    0.730627   -0.040041    11.00000    0.03350    0.03357 =
         0.03336    0.00154    0.00689    0.00119
AFIX  43
H4    2    0.539078    0.805325   -0.065795    11.00000   -1.20000
AFIX   0

C13   1    0.206335    0.873308   -0.016777    11.00000    0.03223    0.03234 =
         0.03218    0.00163    0.00676    0.00107
AFIX 137
H13A  2    0.211683    0.823387   -0.093632    11.00000   -1.50000
H13B  2    0.286962    0.965433   -0.003403    11.00000   -1.50000
H13C  2    0.079365    0.901694   -0.016485    11.00000   -1.50000
AFIX   0

O5A   5    0.428689    0.816911    0.728946    11.00000    0.03434    0.03432 =
         0.03444    0.00156    0.00707    0.00111
C5    1    0.399386    0.971287    0.718855    11.00000    0.03434    0.03432 =
         0.03444    0.00156    0.00707    0.00111
AFIX  43
H5    2    0.362710    1.012185    0.642939    11.00000   -1.20000
AFIX   0
O6B   5    1.082333    0.432360    0.730224    11.00000    0.03120    0.03138 =
         0.03164    0.00145    0.00657    0.00084
O6A   5    1.039231    0.671942    0.754200    11.00000    0.03120    0.03138 =
         0.03164    0.00145    0.00657    0.00084
HKLF 4

REM  CuForm_7_15GPa_a.res in P-1
REM R1 =  0.0767 for     440 Fo > 4sig(Fo)  and  0.1306 for all     737 data
REM    209 parameters refined using    151 restraints

END

WGHT      0.1401     10.2627

REM Highest difference peak  0.671,  deepest hole -0.666,  1-sigma level  0.134
Q1    1   0.6765  0.8375  0.2601  11.00000  0.05    0.67
Q2    1   0.8871  0.6456  0.7782  11.00000  0.05    0.66
Q3    1   0.7398  0.8033  0.2741  11.00000  0.05    0.65
Q4    1   1.1393  0.3322  0.7222  11.00000  0.05    0.59
Q5    1   0.7309  0.7966  0.7775  11.00000  0.05    0.58
;
_shelx_res_checksum              48533

# start Validation Reply Form
_vrf_PLAT029_CuForm_7_15GPa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.264 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_7_15GPa      
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.53 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT112_CuForm_7_15GPa      
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         I         96 %Fit  
RESPONSE: No additional symmetry, see Figure S2 in the Supporting Information.
;
_vrf_PLAT911_CuForm_7_15GPa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1622 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;
####################################################################### 
# 
# 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_CuForm_2_23GPa
_database_code_depnum_ccdc_archive 'CCDC 2067547'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C12 H12 Cu4 O24), C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69
_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'
Cu Cu 0.3201 1.2651 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.5019(14)
_cell_length_b                   8.5043(10)
_cell_length_c                   11.2256(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.055(7)
_cell_angle_gamma                90
_cell_volume                     808.48(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    450
_cell_measurement_temperature    294.03(12)
_cell_measurement_pressure       2.23(0.03)
_cell_measurement_theta_max      24.6500
_cell_measurement_theta_min      3.3820
_shelx_estimated_absorpt_T_max   0.877
_shelx_estimated_absorpt_T_min   0.774
_exptl_absorpt_coefficient_mu    2.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.319
_diffrn_reflns_Laue_measured_fraction_max 0.305
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            771
_diffrn_reflns_point_group_measured_fraction_full 0.319
_diffrn_reflns_point_group_measured_fraction_max 0.305
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.647
_diffrn_reflns_theta_min         3.395
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.319
_diffrn_measured_fraction_theta_max 0.305
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -40.00   1.00   30.00    --  -25.00 134.00 -57.00   57
  2  φ    -90.00 -27.00   1.00   30.00 -82.00 -25.00 134.00    --    63
  3  ω     40.00  97.00   1.00   30.00    --   25.00-134.00  57.00   57
  4  φ     27.00  90.00   1.00   30.00  82.00  25.00-134.00    --    63
  5  φ    -40.00  40.00   1.00   30.00   0.00   0.00   0.00    --    80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                199
_reflns_number_total             237
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         237
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.089
_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)+(0.0348P)²+5.7524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0820
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N1) = Uanis(C4)
Uanis(C1) = Uanis(O1) = Uanis(O2) = Uanis(C2) = Uanis(O3)
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.7500 0.7500 0.7500 0.0154(8) Uani 1 2 d S T P . .
O1 O 0.7570(8) 0.8627(7) 0.5984(4) 0.0211(14) Uani 1 1 d . . . . .
O3 O 0.3669(8) 0.4744(7) 0.6744(4) 0.0211(14) Uani 1 1 d . . . . .
O2 O 0.5438(8) 0.6631(8) 0.6879(4) 0.0211(14) Uani 1 1 d . . . . .
C1 C 0.7500 0.7927(14) 0.5000 0.0211(14) Uani 1 2 d S T P . .
H1 H 0.7500 0.6833 0.5000 0.025 Uiso 1 2 calc RS T P . .
N1 N 0.2500 0.6898(12) 0.5000 0.028(2) Uani 1 2 d S T P . .
H1A H 0.3035 0.6280 0.5533 0.034 Uiso 0.5 1 calc R . . . .
H1B H 0.1965 0.6280 0.4467 0.034 Uiso 0.5 1 calc R . . . .
C4 C 0.3618(14) 0.7828(11) 0.4390(7) 0.028(2) Uani 1 1 d . U . . .
H4A H 0.3053 0.8525 0.3832 0.042 Uiso 1 1 calc GR . . . .
H4B H 0.4274 0.7142 0.3969 0.042 Uiso 1 1 calc GR . . . .
H4C H 0.4265 0.8432 0.4966 0.042 Uiso 1 1 calc GR . . . .
C2 C 0.4897(12) 0.5348(11) 0.7178(6) 0.0211(14) Uani 1 1 d . . . . .
H2 H 0.5475 0.4797 0.7785 0.025 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.014(2) 0.0195(15) 0.0121(6) 0.0010(6) -0.0004(8) -0.0019(8)
O1 0.024(4) 0.017(3) 0.0216(12) 0.0044(15) 0.0013(18) -0.009(2)
O3 0.024(4) 0.017(3) 0.0216(12) 0.0044(15) 0.0013(18) -0.009(2)
O2 0.024(4) 0.017(3) 0.0216(12) 0.0044(15) 0.0013(18) -0.009(2)
C1 0.024(4) 0.017(3) 0.0216(12) 0.0044(15) 0.0013(18) -0.009(2)
N1 0.028(3) 0.029(3) 0.029(2) 0.000 0.0038(19) 0.000
C4 0.028(3) 0.029(3) 0.029(2) 0.000 0.0038(19) 0.000
C2 0.024(4) 0.017(3) 0.0216(12) 0.0044(15) 0.0013(18) -0.009(2)

_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 O1 1.959(5) 7_666 ?
Cu1 O1 1.959(5) . ?
Cu1 O3 2.345(6) 6_665 ?
Cu1 O3 2.345(6) 4_556 ?
Cu1 O2 1.972(7) . ?
Cu1 O2 1.972(7) 7_666 ?
O1 C1 1.251(7) . ?
O3 Cu1 2.345(6) 4_546 ?
O3 C2 1.226(11) . ?
O2 C2 1.243(9) . ?
C1 O1 1.251(7) 2_656 ?
C1 H1 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C4 1.453(10) . ?
N1 C4 1.453(10) 2_556 ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 7_666 . ?
O1 Cu1 O3 87.8(2) 7_666 6_665 ?
O1 Cu1 O3 92.2(2) . 6_665 ?
O1 Cu1 O3 92.2(2) 7_666 4_556 ?
O1 Cu1 O3 87.8(2) . 4_556 ?
O1 Cu1 O2 91.7(2) 7_666 . ?
O1 Cu1 O2 88.3(2) 7_666 7_666 ?
O1 Cu1 O2 91.7(2) . 7_666 ?
O1 Cu1 O2 88.3(2) . . ?
O3 Cu1 O3 180.0 4_556 6_665 ?
O2 Cu1 O3 92.4(3) 7_666 6_665 ?
O2 Cu1 O3 87.6(3) 7_666 4_556 ?
O2 Cu1 O3 87.6(3) . 6_665 ?
O2 Cu1 O3 92.4(3) . 4_556 ?
O2 Cu1 O2 180.0 . 7_666 ?
C1 O1 Cu1 122.1(6) . . ?
C2 O3 Cu1 124.8(5) . 4_546 ?
C2 O2 Cu1 124.9(6) . . ?
O1 C1 O1 123.1(11) . 2_656 ?
O1 C1 H1 118.4 2_656 . ?
O1 C1 H1 118.4 . . ?
H1A N1 H1B 107.6 . . ?
C4 N1 H1A 108.7 . . ?
C4 N1 H1A 108.7 2_556 . ?
C4 N1 H1B 108.7 2_556 . ?
C4 N1 H1B 108.7 . . ?
C4 N1 C4 114.1(11) . 2_556 ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C2 O2 125.7(8) . . ?
O3 C2 H2 117.2 . . ?
O2 C2 H2 117.2 . . ?

_shelx_res_file                  
;
    cuform_2_23gpa.res created by SHELXL-2014/7

TITL CuForm_2_23GPa_a.res in I2/a
REM Old TITL CuForm_2_23GPa_a.res in I2/a
REM SHELXT solution in I2/a
REM R1 0.064, Rweak 0.003, Alpha 0.047, Orientation as input
REM Formula found by SHELXT: C5 Cu N O6
CELL 0.71073 8.5019 8.5043 11.2256 90 95.055 90
ZERR 4 0.0014 0.001 0.0004 0 0.007 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 0.5-X,+Y,1-Z
EQIV $2 1-X,2-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
ISOR 0.001 0.002 C4
EADP N1 C4
EADP C1 O1 O2 C2 O3

L.S. 44
PLAN  5
SIZE 0.1 0.08 0.05
RTAB NO N1 O3_$1
RTAB NO N1 O2_$1
RTAB CO C4 O1_$2
RTAB CO C4 O3_$3
RTAB HO H1b O3_$1
RTAB HO H1b O2_$1
RTAB HO H4a O1_$2
RTAB HO H4b O3_$3
RTAB NHO N1 H1b O3_$1
RTAB NHO N1 H1b O2_$1
RTAB CHO C4 H4a O1_$2
RTAB CHO C4 H4b O3_$3
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_2_23GPa.hkl">
REM </olex2.extras>

WGHT    0.034800    5.752400
FVAR       0.70443
CU1   3    0.750000    0.750000    0.750000    10.50000    0.01426    0.01947 =
         0.01208    0.00101   -0.00039   -0.00188
O1    5    0.757013    0.862721    0.598357    11.00000    0.02415    0.01746 =
         0.02163    0.00435    0.00134   -0.00937
O3    5    0.366866    0.474403    0.674416    11.00000    0.02415    0.01746 =
         0.02163    0.00435    0.00134   -0.00937
O2    5    0.543821    0.663143    0.687872    11.00000    0.02415    0.01746 =
         0.02163    0.00435    0.00134   -0.00937
C1    1    0.750000    0.792667    0.500000    10.50000    0.02415    0.01746 =
         0.02163    0.00435    0.00134   -0.00937
AFIX  43
H1    2    0.750001    0.683311    0.500000    10.50000   -1.20000
AFIX   0

N1    4    0.250000    0.689817    0.500000    10.50000    0.02777    0.02852 =
         0.02875    0.00000    0.00384    0.00000
AFIX  23
H1A   2    0.303459    0.628039    0.553254    10.50000   -1.20000
H1B   2    0.196543    0.628037    0.446746    10.50000   -1.20000
AFIX   0
C4    1    0.361797    0.782812    0.439000    11.00000    0.02777    0.02852 =
         0.02875    0.00000    0.00384    0.00000
AFIX 137
H4A   2    0.305326    0.852508    0.383168    11.00000   -1.50000
H4B   2    0.427426    0.714155    0.396940    11.00000   -1.50000
H4C   2    0.426483    0.843197    0.496602    11.00000   -1.50000
AFIX   0

C2    1    0.489729    0.534750    0.717849    11.00000    0.02415    0.01746 =
         0.02163    0.00435    0.00134   -0.00937
AFIX  43
H2    2    0.547470    0.479676    0.778492    11.00000   -1.20000
AFIX   0
HKLF 4

REM  CuForm_2_23GPa_a.res in I2/a
REM R1 =  0.0335 for     199 Fo > 4sig(Fo)  and  0.0436 for all     237 data
REM     35 parameters refined using      6 restraints

END

WGHT      0.0302      6.1981

REM Highest difference peak  0.229,  deepest hole -0.255,  1-sigma level  0.067
Q1    1   0.3104  0.7789  0.3839  11.00000  0.05    0.23
Q2    1   0.4227  0.7705  0.4901  11.00000  0.05    0.22
Q3    1   0.3616  0.8578  0.4528  11.00000  0.05    0.20
Q4    1   0.1624  0.8762  0.3443  11.00000  0.05    0.19
Q5    1   0.2821  0.4940  0.6205  11.00000  0.05    0.19
;
_shelx_res_checksum              61604

# start Validation Reply Form
_vrf_PLAT029_CuForm_2_23GPa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.319 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_2_23GPa      
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.77 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_2_23GPa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        268 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;
####################################################################### 
# 
# 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_CuForm_9_1GPa
_database_code_depnum_ccdc_archive 'CCDC 2067553'
loop_
_audit_author_name
_audit_author_address
'Michal Andrzejewski'
;University of Bern
Switzerland
;
_audit_update_record             
;
2021-03-02 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H6 Cu2 O12, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H22 Cu2 N2 O12'
_chemical_formula_weight         489.37
_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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.2332(8)
_cell_length_b                   8.5452(10)
_cell_length_c                   11.085(4)
_cell_angle_alpha                92.908(17)
_cell_angle_beta                 102.278(18)
_cell_angle_gamma                91.268(10)
_cell_volume                     668.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    301
_cell_measurement_temperature    293.9(2)
_cell_measurement_pressure       9.1(0.03)
_cell_measurement_theta_max      24.0590
_cell_measurement_theta_min      3.6700
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.736
_exptl_absorpt_coefficient_mu    3.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.177
_diffrn_reflns_Laue_measured_fraction_max 0.167
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1301
_diffrn_reflns_point_group_measured_fraction_full 0.177
_diffrn_reflns_point_group_measured_fraction_max 0.167
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.842
_diffrn_reflns_theta_min         2.388
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.177
_diffrn_measured_fraction_theta_max 0.167
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -40.00   1.00   30.00    --  -25.00 134.00 -57.00   57
  2  φ    -90.00 -27.00   1.00   30.00 -82.00 -25.00 134.00    --    63
  3  ω     40.00  97.00   1.00   30.00    --   25.00-134.00  57.00   57
  4  φ     27.00  90.00   1.00   30.00  82.00  25.00-134.00    --    63
  5  φ    -40.00  23.00   1.00   30.00   0.00   0.00   0.00    --    63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                300
_reflns_number_total             432
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.091
_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     137
_refine_ls_number_reflns         432
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0547
_refine_ls_restrained_S_all      0.974
_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)+(0.0948P)²+3.4671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1638
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H11B-O3A \\sim O3A-H1B
 with sigma of 0.02
 H1A-H10A \\sim H10A-H1B
 with sigma of 0.02
 H2A-H13A \\sim H13A-H2B
 with sigma of 0.02
 H2A-H12C \\sim H12C-H2B
 with sigma of 0.02
 H1B-H11C \\sim H11C-H1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(Cu1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(O2B) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O1B) \\sim Ueq,
Uanis(O3B) \\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(O4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C13) = Uanis(O5B)
Uanis(O1A) = Uanis(C6) = Uanis(O3A) = Uanis(O3B) = Uanis(C5) = Uanis(O5A)
Uanis(O6B) = Uanis(C6) = Uanis(O6A)
Uanis(C4) = Uanis(O4A) = Uanis(O4B)
Uanis(O2A) = Uanis(C2) = Uanis(O2B)
Uanis(O1B) = Uanis(C1) = Uanis(O1A)
Uanis(O3B) = Uanis(C3) = Uanis(O3A)
Uanis(C10) = Uanis(N1) = Uanis(C11)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C1(H1), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.7452(5) 0.7559(3) 0.7331(7) 0.0158(12) Uani 1 1 d . U . . .
Cu1 Cu 0.7397(5) 0.7522(3) 0.2305(8) 0.0141(12) Uani 1 1 d . U . . .
O1A O 0.700(3) 0.7987(18) 0.545(4) 0.0201(15) Uani 1 1 d . U . . .
O1B O 0.865(3) 0.8688(19) 0.418(4) 0.0201(15) Uani 1 1 d . U . . .
O4B O 0.765(3) 0.7171(17) 0.908(4) 0.016(3) Uani 1 1 d . U . . .
O3B O 0.624(3) 0.5500(17) 0.679(3) 0.0201(15) Uani 1 1 d . U . . .
C6 C 1.135(5) 0.571(3) 0.774(6) 0.0201(15) Uani 1 1 d . U . . .
H6 H 1.2505 0.5975 0.8276 0.024 Uiso 1 1 calc R . . . .
O2A O 0.950(3) 0.8481(19) 0.176(4) 0.017(2) Uani 1 1 d . . . . .
O2B O 0.826(3) 0.9705(17) 0.779(4) 0.017(2) Uani 1 1 d . U . . .
O3A O 0.537(3) 0.6598(19) 0.294(3) 0.0201(15) Uani 1 1 d D U . . .
C2 C 1.008(4) 0.985(3) 0.221(6) 0.017(2) Uani 1 1 d . U . . .
H2 H 0.9287 1.0504 0.2546 0.021 Uiso 1 1 calc R . . . .
N1 N 0.352(3) 0.688(2) 0.514(3) 0.019(3) Uani 1 1 d . U . . .
H1A H 0.3820 0.7301 0.5911 0.023 Uiso 1 1 calc DR . . . .
H1B H 0.4542 0.6455 0.4952 0.023 Uiso 1 1 calc DR . . . .
C3 C 0.465(4) 0.526(3) 0.254(5) 0.0201(15) Uani 1 1 d . . . . .
H3 H 0.4769 0.4837 0.1776 0.024 Uiso 1 1 calc R . . . .
N2 N 0.263(3) 0.767(2) 0.090(4) 0.016(5) Uani 1 1 d . U . . .
H2A H 0.3858 0.7472 0.0990 0.019 Uiso 1 1 calc DR . . . .
H2B H 0.2471 0.8170 0.1591 0.019 Uiso 1 1 calc DR . . . .
O5B O 0.593(3) 0.939(2) 0.185(4) 0.022(4) Uani 1 1 d . . . . .
C11 C 0.273(4) 0.811(3) 0.423(6) 0.019(3) Uani 1 1 d . U . . .
H11A H 0.1597 0.8517 0.4429 0.028 Uiso 1 1 calc GR . . . .
H11B H 0.2435 0.7633 0.3403 0.028 Uiso 1 1 calc DGR . . . .
H11C H 0.3651 0.8948 0.4278 0.028 Uiso 1 1 calc DGR . . . .
C1 C 0.856(5) 0.834(3) 0.516(7) 0.0201(15) Uani 1 1 d . . . . .
H1 H 0.9669 0.8312 0.5762 0.024 Uiso 1 1 calc R . . . .
C10 C 0.189(4) 0.566(2) 0.499(6) 0.019(3) Uani 1 1 d . U . . .
H10A H 0.2256 0.4836 0.5534 0.028 Uiso 1 1 calc DGR . . . .
H10B H 0.1583 0.5234 0.4147 0.028 Uiso 1 1 calc GR . . . .
H10C H 0.0796 0.6153 0.5180 0.028 Uiso 1 1 calc GR . . . .
C12 C 0.152(4) 0.616(3) 0.071(6) 0.031(7) Uani 1 1 d . U . . .
H12A H 0.1722 0.5601 -0.0024 0.047 Uiso 1 1 calc GR . . . .
H12B H 0.0197 0.6367 0.0611 0.047 Uiso 1 1 calc GR . . . .
H12C H 0.1913 0.5539 0.1408 0.047 Uiso 1 1 calc DGR . . . .
C4 C 0.625(4) 0.740(3) -0.053(6) 0.016(3) Uani 1 1 d . . . . .
H4 H 0.5423 0.8179 -0.0837 0.020 Uiso 1 1 calc R . . . .
C13 C 0.204(4) 0.868(3) -0.017(6) 0.022(4) Uani 1 1 d . U . . .
H13A H 0.2769 0.9645 -0.0016 0.032 Uiso 1 1 calc DGR . . . .
H13B H 0.0719 0.8891 -0.0261 0.032 Uiso 1 1 calc GR . . . .
H13C H 0.2242 0.8144 -0.0908 0.032 Uiso 1 1 calc GR . . . .
O5A O 0.419(3) 0.820(2) 0.734(4) 0.0201(15) Uani 1 1 d . . . . .
C5 C 0.411(4) 0.966(3) 0.719(6) 0.0201(15) Uani 1 1 d . U . . .
H5 H 0.4086 1.0051 0.6423 0.024 Uiso 1 1 calc R . . . .
O6B O 1.098(3) 0.427(2) 0.738(4) 0.0201(15) Uani 1 1 d . . . . .
O6A O 1.027(3) 0.6751(19) 0.743(4) 0.0201(15) Uani 1 1 d . . . . .
O4A O 0.591(3) 0.6545(18) 0.035(4) 0.016(3) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu2 0.0165(12) 0.0155(16) 0.0157(18) 0.0025(11) 0.0041(12) -0.0019(9)
Cu1 0.0139(12) 0.0141(17) 0.0142(18) 0.0015(11) 0.0024(12) -0.0001(9)
O1A 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O1B 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O4B 0.017(3) 0.016(3) 0.016(3) 0.0010(12) 0.0036(14) 0.0006(11)
O3B 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
C6 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O2A 0.018(2) 0.017(3) 0.017(3) 0.0011(9) 0.0036(10) 0.0004(8)
O2B 0.018(2) 0.017(3) 0.017(3) 0.0011(9) 0.0036(10) 0.0004(8)
O3A 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
C2 0.018(2) 0.017(3) 0.017(3) 0.0011(9) 0.0036(10) 0.0004(8)
N1 0.019(3) 0.019(3) 0.019(3) 0.0012(10) 0.0040(13) 0.0005(10)
C3 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
N2 0.016(5) 0.016(5) 0.016(5) 0.0009(12) 0.0035(16) 0.0001(12)
O5B 0.022(4) 0.021(4) 0.021(5) 0.001(2) 0.003(3) 0.001(2)
C11 0.019(3) 0.019(3) 0.019(3) 0.0012(10) 0.0040(13) 0.0005(10)
C1 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
C10 0.019(3) 0.019(3) 0.019(3) 0.0012(10) 0.0040(13) 0.0005(10)
C12 0.031(7) 0.031(7) 0.031(7) 0.002(2) 0.007(3) 0.000(2)
C4 0.017(3) 0.016(3) 0.016(3) 0.0010(12) 0.0036(14) 0.0006(11)
C13 0.022(4) 0.021(4) 0.021(5) 0.001(2) 0.003(3) 0.001(2)
O5A 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
C5 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O6B 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O6A 0.0201(15) 0.0201(16) 0.0200(16) 0.0012(5) 0.0044(6) 0.0005(5)
O4A 0.017(3) 0.016(3) 0.016(3) 0.0010(12) 0.0036(14) 0.0006(11)

_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
Cu2 O1A 2.10(4) . ?
Cu2 O4B 1.96(4) . ?
Cu2 O3B 1.95(2) . ?
Cu2 O2B 1.921(19) . ?
Cu2 O5A 2.432(15) . ?
Cu2 O6A 2.152(16) . ?
Cu1 O1B 2.26(4) . ?
Cu1 O2A 1.934(12) . ?
Cu1 O3A 1.926(13) . ?
Cu1 O5B 1.97(2) . ?
Cu1 O6B 1.955(18) 2_766 ?
Cu1 O4A 2.31(4) . ?
O1A C1 1.27(2) . ?
O1B C1 1.15(8) . ?
O4B C4 1.20(2) 1_556 ?
O3B C3 1.27(4) 2_666 ?
C6 H6 0.9300 . ?
C6 O6B 1.28(3) . ?
C6 O6A 1.21(4) . ?
O2A C2 1.28(4) . ?
O2B C2 1.25(2) 2_776 ?
O3A C3 1.26(4) . ?
C2 O2B 1.25(2) 2_776 ?
C2 H2 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C11 1.53(4) . ?
N1 C10 1.53(3) . ?
C3 O3B 1.27(4) 2_666 ?
C3 H3 0.9300 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C12 1.48(3) . ?
N2 C13 1.49(6) . ?
O5B C5 1.31(7) 2_676 ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C1 H1 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C4 O4B 1.20(2) 1_554 ?
C4 H4 0.9300 . ?
C4 O4A 1.30(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O5A C5 1.27(3) . ?
C5 O5B 1.31(7) 2_676 ?
C5 H5 0.9300 . ?
O6B Cu1 1.955(18) 2_766 ?

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
O1A Cu2 O5A 90.1(11) . . ?
O1A Cu2 O6A 94.1(12) . . ?
O4B Cu2 O1A 175.2(7) . . ?
O4B Cu2 O5A 85.2(11) . . ?
O4B Cu2 O6A 90.5(12) . . ?
O3B Cu2 O1A 86.0(13) . . ?
O3B Cu2 O4B 92.4(12) . . ?
O3B Cu2 O5A 81.2(7) . . ?
O3B Cu2 O6A 94.0(7) . . ?
O2B Cu2 O1A 91.3(12) . . ?
O2B Cu2 O4B 89.6(13) . . ?
O2B Cu2 O3B 171.2(8) . . ?
O2B Cu2 O5A 90.5(7) . . ?
O2B Cu2 O6A 94.5(7) . . ?
O6A Cu2 O5A 173.4(7) . . ?
O1B Cu1 O4A 174.0(6) . . ?
O2A Cu1 O1B 86.6(12) . . ?
O2A Cu1 O5B 89.1(7) . . ?
O2A Cu1 O6B 85.1(6) . 2_766 ?
O2A Cu1 O4A 94.2(13) . . ?
O3A Cu1 O1B 90.6(12) . . ?
O3A Cu1 O2A 177.1(16) . . ?
O3A Cu1 O5B 91.5(7) . . ?
O3A Cu1 O6B 94.5(6) . 2_766 ?
O3A Cu1 O4A 88.7(12) . . ?
O5B Cu1 O1B 90.1(14) . . ?
O5B Cu1 O4A 84.0(14) . . ?
O6B Cu1 O1B 92.3(13) 2_766 . ?
O6B Cu1 O5B 173.6(10) 2_766 . ?
O6B Cu1 O4A 93.7(13) 2_766 . ?
C1 O1A Cu2 110(4) . . ?
C1 O1B Cu1 131(3) . . ?
C4 O4B Cu2 116(3) 1_556 . ?
C3 O3B Cu2 122(3) 2_666 . ?
O6B C6 H6 118.5 . . ?
O6A C6 H6 118.5 . . ?
O6A C6 O6B 123(4) . . ?
C2 O2A Cu1 118(2) . . ?
C2 O2B Cu2 120.1(16) 2_776 . ?
C3 O3A Cu1 122(2) . . ?
O2A C2 H2 120.4 . . ?
O2B C2 O2A 119(2) 2_776 . ?
O2B C2 H2 120.4 2_776 . ?
H1A N1 H1B 109.0 . . ?
C11 N1 H1A 111.1 . . ?
C11 N1 H1B 111.1 . . ?
C11 N1 C10 103(2) . . ?
C10 N1 H1A 111.1 . . ?
C10 N1 H1B 111.1 . . ?
O3B C3 H3 120.4 2_666 . ?
O3A C3 O3B 119(4) . 2_666 ?
O3A C3 H3 120.4 . . ?
H2A N2 H2B 108.0 . . ?
C12 N2 H2A 109.4 . . ?
C12 N2 H2B 109.4 . . ?
C12 N2 C13 111(4) . . ?
C13 N2 H2A 109.4 . . ?
C13 N2 H2B 109.4 . . ?
C5 O5B Cu1 112(4) 2_676 . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1A C1 H1 118.8 . . ?
O1B C1 O1A 122(6) . . ?
O1B C1 H1 118.8 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4B C4 H4 120.8 1_554 . ?
O4B C4 O4A 118(3) 1_554 . ?
O4A C4 H4 120.8 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 O5A Cu2 105.2(11) . . ?
O5B C5 H5 120.6 2_676 . ?
O5A C5 O5B 119(5) . 2_676 ?
O5A C5 H5 120.6 . . ?
C6 O6B Cu1 129(3) . 2_766 ?
C6 O6A Cu2 145.3(15) . . ?
C4 O4A Cu1 113(3) . . ?

_shelx_res_file                  
;
    CuForm_9_1GPa.res created by SHELXL-2014/7

TITL CuForm_9_1GPa_a.res in P-1
REM Old TITL CuForm_9_1GPa_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.294, Rweak 0.025, Alpha 0.177, Orientation as input
REM Formula found by SHELXT: H12a N O4 Cu2
CELL 0.71073 7.2332 8.5452 11.0846 92.908 102.278 91.268
ZERR 2 0.0008 0.001 0.0042 0.017 0.018 0.01
LATT 1
SFAC C H Cu N O
UNIT 20 44 4 4 24
EQIV $1 1-X,1-Y,1-Z
EQIV $2 2-X,1-Y,1-Z
EQIV $3 -1+X,+Y,+Z
EQIV $4 2-X,2-Y,1-Z
EQIV $5 +X,+Y,-1+Z
EQIV $6 1-X,2-Y,1-Z
EQIV $7 1-X,1-Y,-Z
EQIV $8 -1+X,+Y,-1+Z
EQIV $9 1-X,2-Y,-Z
SADI H11b O3A O3A H1b
SADI H1a H10a H10a H1b
SADI H2a H13a H13a H2b
SADI H2a H12c H12c H2b
SADI H1b H11c H11c H1a
ISOR 0.001 0.002 C5 O3A Cu1 C2 O2B C13 O1B O3B Cu2 C6 O1A O4B
ISOR 0.001 0.002 C10 N1 C11
ISOR 0.001 0.002 C12 N2 C13
EADP C13 O5B
EADP O1A C6 O3A O3B C5 O5A
EADP O6B C6 O6A
EADP C4 O4A O4B
EADP O2A C2 O2B
EADP O1B C1 O1A
EADP O3B C3 O3A
EADP C10 N1 C11

L.S. 40
PLAN  5
SIZE 0.1 0.08 0.05
RTAB OO O1B O4A
RTAB OO O2A O3A
RTAB OO O5B O6B_$2
RTAB OO O1A O4B
RTAB OO O3B O2B
RTAB OO O5A O6A
RTAB NO N1 O1A
RTAB NO N1 O3B
RTAB NO N1 O3B_$1
RTAB NO N1 O3A
RTAB NO N1 O5A
RTAB HON H1b O1A
RTAB HON H1b O3B
RTAB HON H1b O3B_$1
RTAB HON H1b O3A
RTAB HON H1a O1A
RTAB HON H1a O3B_$1
RTAB HON H1a O5A
RTAB NHO N1 H1b O1A
RTAB NHO N1 H1b O3B
RTAB NHO N1 H1b O3B_$1
RTAB NHO N1 H1b O3A
RTAB NHO N1 H1a O1A
RTAB NHO N1 H1a O3B_$1
RTAB NHO N1 H1a O5A
RTAB CO C11 O2A_$3
RTAB CO C11 O3A
RTAB CO C11 O1A
RTAB CO C11 O1B_$3
RTAB HOC H11b O2A_$3
RTAB HOC H11b O3A
RTAB HOC H11c O1A
RTAB HOC H11c O3A
RTAB HOC H11a O1B_$3
RTAB CHO C11 H11b O2A_$3
RTAB CHO C11 H11b O3A
RTAB CHO C11 H11c O1A
RTAB CHO C11 H11c O3A
RTAB CHO C11 H11a O1B_$3
RTAB CO C10 O3B
RTAB CO C10 O6A_$1
RTAB CO C10 O6B_$1
RTAB CO C10 O6A_$3
RTAB CO C10 O3A_$1
RTAB CO C10 O6B_$3
RTAB HOC H10b O3B
RTAB HOC H10b O6A_$1
RTAB HOC H10b O6B_$1
RTAB HOC H10c O6A_$3
RTAB HOC H10a O3A_$1
RTAB HOC H10a O6B_$3
RTAB CHO C10 H10b O3B
RTAB CHO C10 H10b O6A_$1
RTAB CHO C10 H10b O6B_$1
RTAB CHO C10 H10c O6A_$3
RTAB CHO C10 H10a O3A_$1
RTAB CHO C10 H10a O6B_$3
RTAB COF C6 O4A_$2
RTAB COF C2 O6A_$4
RTAB COF C4 O5A_$5
RTAB HOF H6 O4A_$2
RTAB HOF H2 O6A_$4
RTAB HOF H4 O5A_$5
RTAB CHOF C6 H6 O4A_$2
RTAB CHOF C2 H2 O6A_$4
RTAB CHOF C4 H4 O5A_$5
RTAB NO2 N2 O3A
RTAB NO2 N2 O4A
RTAB NO2 N2 O5B
RTAB NO2 N2 O2A_$3
RTAB NO2 N2 O2B_$6
RTAB HO2 H2a O3A
RTAB HO2 H2a O4A
RTAB HO2 H2a O5B
RTAB HO2 H2b O2A_$3
RTAB HO2 H2b O2B_$6
RTAB HO2 H2b O3A
RTAB HO2 H2b O5B
RTAB NHO2 N2 H2a O3A
RTAB NHO2 N2 H2a O4A
RTAB NHO2 N2 H2a O5B
RTAB NHO2 N2 H2b O2A_$3
RTAB NHO2 N2 H2b O2B_$6
RTAB NHO2 N2 H2b O3A
RTAB NHO2 N2 H2b O5B
RTAB CO2 C12 O4A_$7
RTAB CO2 C12 O2A_$3
RTAB CO2 C12 O4B_$8
RTAB CO2 C12 O4B_$1
RTAB CO2 C12 O3B_$1
RTAB CO2 C13 O6A_$8
RTAB CO2 C13 O5B_$9
RTAB CO2 C13 O2A_$9
RTAB HO2 H12a O4A_$7
RTAB HO2 H12b O2A_$3
RTAB HO2 H12b O4B_$8
RTAB HO2 H12c O4B_$1
RTAB HO2 H12c O3B_$1
RTAB HO2 H13c O6A_$8
RTAB HO2 H13a O5B_$9
RTAB HO2 H13b O2A_$9
RTAB CHO2 C12 H12a O4A_$7
RTAB CHO2 C12 H12b O2A_$3
RTAB CHO2 C12 H12b O4B_$8
RTAB CHO2 C12 H12c O4B_$1
RTAB CHO2 C12 H12c O3B_$1
RTAB CHO2 C13 H13c O6A_$8
RTAB CHO2 C13 H13a O5B_$9
RTAB CHO2 C13 H13b O2A_$9
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\CuForm_9_1GPa.hkl">
REM </olex2.extras>

WGHT    0.094800    3.467100
FVAR       0.60026
CU2   3    0.745229    0.755920    0.733057    11.00000    0.01654    0.01550 =
         0.01567    0.00247    0.00407   -0.00195
CU1   3    0.739672    0.752233    0.230507    11.00000    0.01388    0.01407 =
         0.01421    0.00153    0.00241   -0.00009
O1A   5    0.699939    0.798680    0.544651    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
O1B   5    0.864625    0.868840    0.418279    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
O4B   5    0.764597    0.717126    0.907982    11.00000    0.01685    0.01612 =
         0.01633    0.00105    0.00362    0.00062
O3B   5    0.624417    0.549994    0.678954    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
C6    1    1.135090    0.571432    0.774246    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
AFIX  43
H6    2    1.250504    0.597524    0.827613    11.00000   -1.20000
AFIX   0
O2A   5    0.949743    0.848092    0.175596    11.00000    0.01756    0.01729 =
         0.01746    0.00111    0.00359    0.00038
O2B   5    0.825872    0.970521    0.778713    11.00000    0.01756    0.01729 =
         0.01746    0.00111    0.00359    0.00038
O3A   5    0.536607    0.659841    0.293556    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
C2    1    1.008357    0.984774    0.221450    11.00000    0.01756    0.01729 =
         0.01746    0.00111    0.00359    0.00038
AFIX  43
H2    2    0.928713    1.050401    0.254610    11.00000   -1.20000
AFIX   0

N1    4    0.352016    0.688122    0.514055    11.00000    0.01894    0.01877 =
         0.01885    0.00116    0.00395    0.00053
AFIX  23
H1A   2    0.381973    0.730062    0.591132    11.00000   -1.20000
H1B   2    0.454162    0.645550    0.495157    11.00000   -1.20000
AFIX   0

C3    1    0.464810    0.526131    0.254333    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
AFIX  43
H3    2    0.476939    0.483693    0.177579    11.00000   -1.20000
AFIX   0

N2    4    0.263319    0.766518    0.090015    11.00000    0.01583    0.01570 =
         0.01575    0.00092    0.00350    0.00012
AFIX  23
H2A   2    0.385756    0.747220    0.098960    11.00000   -1.20000
H2B   2    0.247146    0.816972    0.159058    11.00000   -1.20000
AFIX   0

O5B   5    0.592752    0.939045    0.184893    11.00000    0.02197    0.02063 =
         0.02142    0.00148    0.00331    0.00117
C11   1    0.272675    0.810936    0.422746    11.00000    0.01894    0.01877 =
         0.01885    0.00116    0.00395    0.00053
AFIX 137
H11A  2    0.159699    0.851749    0.442891    11.00000   -1.50000
H11B  2    0.243498    0.763338    0.340300    11.00000   -1.50000
H11C  2    0.365063    0.894754    0.427775    11.00000   -1.50000
AFIX   0

C1    1    0.855759    0.833769    0.516156    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
AFIX  43
H1    2    0.966914    0.831175    0.576229    11.00000   -1.20000
AFIX   0

C10   1    0.188604    0.566186    0.498584    11.00000    0.01894    0.01877 =
         0.01885    0.00116    0.00395    0.00053
AFIX 137
H10A  2    0.225640    0.483569    0.553367    11.00000   -1.50000
H10B  2    0.158301    0.523391    0.414700    11.00000   -1.50000
H10C  2    0.079609    0.615291    0.518003    11.00000   -1.50000
AFIX   0

C12   1    0.151791    0.616024    0.070665    11.00000    0.03137    0.03090 =
         0.03103    0.00204    0.00679    0.00032
AFIX 137
H12A  2    0.172206    0.560062   -0.002427    11.00000   -1.50000
H12B  2    0.019714    0.636742    0.061113    11.00000   -1.50000
H12C  2    0.191319    0.553931    0.140795    11.00000   -1.50000
AFIX   0

C4    1    0.624650    0.740408   -0.052659    11.00000    0.01685    0.01612 =
         0.01633    0.00105    0.00362    0.00062
AFIX  43
H4    2    0.542340    0.817895   -0.083732    11.00000   -1.20000
AFIX   0

C13   1    0.203743    0.867686   -0.016657    11.00000    0.02197    0.02063 =
         0.02142    0.00148    0.00331    0.00117
AFIX 137
H13A  2    0.276887    0.964526   -0.001591    11.00000   -1.50000
H13B  2    0.071858    0.889061   -0.026063    11.00000   -1.50000
H13C  2    0.224225    0.814441   -0.090821    11.00000   -1.50000
AFIX   0

O5A   5    0.419410    0.819970    0.733649    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
C5    1    0.411429    0.966071    0.719411    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
AFIX  43
H5    2    0.408592    1.005139    0.642266    11.00000   -1.20000
AFIX   0
O6B   5    1.097799    0.427482    0.737775    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
O6A   5    1.027309    0.675057    0.742567    11.00000    0.02008    0.02009 =
         0.02004    0.00119    0.00441    0.00051
O4A   5    0.590815    0.654521    0.034640    11.00000    0.01685    0.01612 =
         0.01633    0.00105    0.00362    0.00062
HKLF 4

REM  CuForm_9_1GPa_a.res in P-1
REM R1 =  0.0547 for     300 Fo > 4sig(Fo)  and  0.0866 for all     432 data
REM    137 parameters refined using    107 restraints

END

WGHT      0.0959      1.3166

REM Highest difference peak  0.342,  deepest hole -0.308,  1-sigma level  0.091
Q1    1   0.6853  0.6721  0.0356  11.00000  0.05    0.34
Q2    1   0.6876  0.6616  0.8025  11.00000  0.05    0.31
Q3    1   0.5938  0.9164  0.0643  11.00000  0.05    0.30
Q4    1   0.7200  0.6649  0.8344  11.00000  0.05    0.29
Q5    1   0.4932  0.6386  0.0425  11.00000  0.05    0.29
;
_shelx_res_checksum              42067

# start Validation Reply Form
_vrf_PLAT029_CuForm_9_1GPa       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.264 Why?  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurements limits access to a sample. For this reason lower
completness of data was collected.
;
_vrf_PLAT088_CuForm_9_1GPa       
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.53 Note  
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample. For this reason lower
completness of data was collected and the data to parameters ratio is below 
the IUCR suggestion for an ambient conditions measurement.
;
_vrf_PLAT911_CuForm_9_1GPa       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1622 Report
RESPONSE: The construction of a diamond anvil cell used for the
high-pressure measurement limits access to a sample and rotation of 
the cell does not allow to cover full completness.
;
_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
;


#===END
